CN110484367A - A kind of preparation method of nicotine essence particle - Google Patents
A kind of preparation method of nicotine essence particle Download PDFInfo
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- CN110484367A CN110484367A CN201910796598.2A CN201910796598A CN110484367A CN 110484367 A CN110484367 A CN 110484367A CN 201910796598 A CN201910796598 A CN 201910796598A CN 110484367 A CN110484367 A CN 110484367A
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- nicotine
- essence
- supercritical
- supercritical fluid
- suspension
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/241—Extraction of specific substances
- A24B15/243—Nicotine
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0403—Solvent extraction of solutions which are liquid with a supercritical fluid
- B01D11/0407—Solvent extraction of solutions which are liquid with a supercritical fluid the supercritical fluid acting as solvent for the solute
-
- 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
-
- 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
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
After the present invention provides a kind of preparation method of nicotine essence particle, nicotine essence and filming agent by solvent dissolution, adjusting pH value is 2~5, and the nicotiana alkaloids in nicotine essence is precipitated at this time, and filming agent is covered in the surface of nicotiana alkaloids, forms aaerosol solution；The aaerosol solution is injected in supercritical extraction reactor, is mixed with the supercritical fluid for equally injecting the supercritical extraction reactor, the nicotine essence particle of filming agent package nicotiana alkaloids is precipitated in the solvent extraction in suspension by supercritical fluid；The nicotine essence particle is the particle for having cyst wall, have the characteristics that small in size, surface area is big, uniform particle sizes, be tightly combined, the nicotine essence particle includes nicotiana alkaloids, and biological tobacco alkali content is greater than 60wt%, fragrance can slowly and be uniformly discharged during heating, to be capable of forming the sensory experience of mellow in taste in aspiration procedure, alleviate sensorial differences light after brought preceding weight in aspiration procedure.
Description
Technical field
The present invention relates to essence technical field more particularly to a kind of preparation methods of nicotine essence particle.
Background technique
Flavors and fragrances is added in cigarette, its role is to improve the physicochemical property of cigarette, mellow and full fragrance, modification cigarette perfume
Taste improves the style inhaled taste, establish product, affects smell, the sense of taste and the tactile of user to a certain extent, promotes product
It is acceptable.Flavouring essence for tobacco can be directly added into tobacco component, also may be added to filter tip, cigarette paper, packaging material.Mesh
Before, flavouring essence for tobacco source is broadly divided into 3 types, fragrance, non-tobacco natural perfume material respectively from tobacco itself and artificial
The fragrance of synthesis.The fragrance of tobacco itself refers to the extract extracted from tobacco；Non-tobacco natural perfume material refers to from except tobacco
The extract extracted in various plants or animal in addition, such as extracts from the flower of various plants, fruit, leaf, stem, root or skin
Essential oil or water, alcohol steep object such as medicinal extract for coming etc..
Flavouring essence for tobacco is a kind of special commodity, in use should be in view of the influence to cigarette product, again
In view of the health of smoker, no matter therefore in tobacco by which kind of approach should all be had using flavouring essence for tobacco certain odor type and
Fragrance characteristic can transmit graceful fragrance in smoking process and inhale taste, furthermore have corresponding adaptability and stability to tobacco,
And with matrix or ingredient phase harmony.
But the effective component in existing flavouring essence for tobacco is readily volatilized, flavor matter cannot during the smoking process
Uniform slow release forms stimulus to the sense organ light after weight before fragrance in aspiration procedure, to bring poor experience sense, and flavouring essence for tobacco
Vulnerable to the environmental factors such as light, oxygen, heat influence and it is rotten influence product quality, be not convenient to use and store.
Summary of the invention
It is an object of the invention to overcome the deficiencies of existing technologies, a kind of preparation method of nicotine essence particle is provided.
In order to achieve the above object, the present invention provides a kind of preparation method of nicotine essence particle, include the following steps:
Step a. mixes nicotine essence with filming agent, and solvent dissolution is added, and adjusts after pH value is 2~5 and obtains suspension；
Step b. by the suspension and supercritical fluid injection supercritical extraction reactor in, the supercritical fluid with it is described
Suspension mixes and by the solvent extraction in the suspension, and nicotine essence particle is precipitated.
As a further improvement of the above technical scheme, it the nicotine essence particle and will be mixed with described in the solvent
Supercritical fluid separation, then injects the supercritical fluid in separating still, the supercritical fluid together with the solvent
It is separated with the solvent.
As a further improvement of the above technical scheme, the filming agent includes methylcellulose, ethyl cellulose, hydroxypropyl
One of base cellulose, carboxymethyl cellulose, cellulose acetate, cellulose acetate-phthalate or combination.
As a further improvement of the above technical scheme, in the step a, the weight of the nicotine essence and the filming agent
Amount is than being 1:(2~10).
As a further improvement of the above technical scheme, in the step a, the solvent includes alcohol or alcoholic solution.
As a further improvement of the above technical scheme, in the step b, the pressure of the supercritical extraction reactor is 20~
30MPa, temperature are 35~50 DEG C.
As a further improvement of the above technical scheme, in the step c, the pressure of the separating still is 15~25MPa,
Temperature is 15~25 DEG C.
As a further improvement of the above technical scheme, in the step b, the injection direction of the supercritical fluid and institute
The injection direction for stating suspension is opposite.
As a further improvement of the above technical scheme, the supercritical fluid from the bottom of the supercritical extraction reactor to
Upper injection；The suspension is injected from the kettle top of the supercritical extraction reactor, flow velocity 0.01-1L/min.
As a further improvement of the above technical scheme, in the step c, the supercritical fluid is laggard by solvent extraction
The flow velocity for entering the separating still is 0.5-3L/min.
Beneficial effects of the present invention:
After the present invention provides a kind of preparation method of nicotine essence particle, nicotine essence and filming agent by solvent dissolution,
Adjusting pH value is 2~5, and the nicotiana alkaloids in nicotine essence is precipitated at this time, and filming agent is covered in the surface of nicotiana alkaloids, from
And aaerosol solution is formed, which is injected in supercritical extraction reactor, is faced with the super of the supercritical extraction reactor is equally injected
The mixing of boundary's fluid, supercritical fluid is by the solvent extraction in suspension, to be precipitated what filming agent package nicotiana alkaloids was formed
Nicotine essence particle, collecting supercritical extraction reactor bottom particles is nicotine essence particle；The nicotine essence particle is to have cyst wall
Particle, there is ultra-small volume and huge specific surface area, diameter is distributed in the nicotine essence particle between 1~15 μm and accounts for total nicotine
The 70~90% of essence particle；Therefore, which has the characteristics that uniform particle sizes, is tightly combined, the nicotine essence
Particle includes nicotiana alkaloids, and the biological tobacco alkali content of nicotine essence particle is greater than 60wt%, during heating can
Slow release fragrance, and fragrance release is uniformly, so that the sensory experience of mellow in taste is capable of forming in aspiration procedure, it is steady fragrant
Sensorial differences light after brought preceding weight in aspiration procedure are alleviated in smart bring pessimal stimulation sense.
Specific embodiment
Term as used herein:
" by ... preparation " it is synonymous with "comprising".Term "comprising" used herein, " comprising ", " having ", " containing "
Or its any other deformation, it is intended that cover non-exclusionism includes.For example, composition, step, method comprising listed elements,
Product or device are not necessarily limited to those elements, but may include not expressly listed other elements or such composition, step
Suddenly, method, product or the intrinsic element of device.
Conjunction " by ... form " exclude any element that do not point out, step or component.If in claim,
This phrase will make claim closed, so that it is not included the material in addition to the material of those descriptions, but relative
Except customary impurities.When phrase " by ... form " be rather than immediately following theme in the clause that appears in claim main body after
When, only it is limited to element described in the clause；Other elements be not excluded the claim as a whole it
Outside.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1~5 ", described range should be interpreted as including range " 1~4 ", " 1~3 ", " 1~2 ", " 1~2 and 4~
5 ", " 1~3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range is intended to include its end
Value and all integers and score in the range.
In these embodiments, unless otherwise specified, described part and percentage is by mass.
" mass parts " refer to the basic measurement unit for indicating the mass ratio relationship of multiple components, and 1 part can indicate arbitrary list
Position quality, can such as be expressed as 1g, may also indicate that 2.689g etc..If we say that the mass parts of component A are a parts, the matter of B component
Measuring part is b parts, then it represents that the quality of component A and the mass ratio a:b of B component.Alternatively, indicating that the quality of component A is aK, B group
The quality divided is bK (K is arbitrary number, indicates multiplying factor).It can not misread, unlike mass fraction, all components
The sum of mass parts be not limited to 100 parts of limitation.
"and/or" is used to indicate that one of illustrated situation or both may to occur, for example, A and/or B includes (A
And B) and (A or B).
The present invention provides a kind of preparation method of nicotine essence particle, includes the following steps:
Step a. mixes nicotine essence with filming agent, and solvent dissolution is added, and adjusts after pH value is 2~5 and obtains suspension；
Step b. by the suspension and supercritical fluid injection supercritical extraction reactor in, the supercritical fluid with it is described
Suspension mixes and by the solvent extraction in the suspension, and nicotine essence particle is precipitated.
Specifically, the nicotine essence refers to the solution containing nicotiana alkaloids, the nicotiana alkaloids include nicotine and
Other alkaloids, wherein nicotiana alkaloids accounts for the weight percent of nicotine essence up to 90% or more, and nicotine accounts for nicotiana alkaloids
Weight percent is 85~99%.
The nicotine essence can extract tobacco by ion-exchange, steam distillation, supercritical extraction etc.
Liquid extracts to obtain, and the tobacco leaching liquor includes after tobacco product to be added to flooding in the liquid being separated by solid-liquid separation
The waste water containing tobacco leachable that is generated in body, tobacco processing course and to the tobacco corner generated in tobacco processing course
At least one of the aqueous solution that material or tobacco waste obtain after being extracted.
It should be understood that adjusting pH value is 2~5, at this time nicotine essence after nicotine essence and filming agent are dissolved by solvent
In nicotiana alkaloids be precipitated, filming agent is covered in the surface of nicotiana alkaloids, forms aaerosol solution, which is injected
It in supercritical extraction reactor, is mixed with the supercritical fluid for equally injecting the supercritical extraction reactor, supercritical fluid will be in suspension
Solvent extraction, thus be precipitated filming agent package nicotiana alkaloids formed nicotine essence particle, collect supercritical extract bottom
Portion's particle is nicotine essence particle.
The nicotine essence particle is the particle for having cyst wall, has ultra-small volume and huge specific surface area, can change well
The kind apparent property of substance, and fine material can be stored；The diameter of the nicotine essence particle between 500nm~500 μm,
Middle diameter is distributed in the nicotine essence particle between 1~15 μm and accounts for the 70~90% of total nicotine essence particle.Therefore, the nicotine is fragrant
Precise and tiny grain has the characteristics that small in size, surface area is big, uniform particle sizes, is tightly combined and safe and non-toxic, the nicotine essence particle
Comprising nicotiana alkaloids, the biological tobacco alkali content of nicotine essence particle is greater than 60wt%, can slowly release during heating
Fragrance is put, and fragrance release is uniformly, to be capable of forming the sensory experience of mellow in taste in aspiration procedure, steady essence is brought
Pessimal stimulation sense, alleviate it is brought in aspiration procedure before light sensorial differences after weight.
It should be understood that the nicotine essence particle being prepared can be used as tobacco additive agent, feed addictive, health care
Food additives or drug additive etc..
Optionally, the preparation method of above-mentioned nicotine essence particle further include step c. by the nicotine essence particle with mix
There is the supercritical fluid of the solvent to separate, the supercritical fluid is then injected into separating still together with the solvent
In, the supercritical fluid is separated with the solvent.
Above-mentioned, supercritical fluid will inject in separating still together after solvent extraction, and supercritical fluid is formed in separating still
Gas is separated with the solvent of liquid, and so as to recycle to supercritical fluid and solvent, can be recycled again makes
With.
Make supercritical fluid and solvent carry out regeneration by the above method, there is environmentally protective, safe and efficient, work
The simple feature of skill.
Specifically, the pH value after adjusting can be 2,3,4,5 etc., the cigarette under this pH value range, in nicotine essence
Careless alkaloid can sufficiently be precipitated, and the surface of nicotiana alkaloids is covered in convenient for filming agent, and inclusion effect is good.The pH value is higher than
5 cannot be such that nicotiana alkaloids is precipitated, and cause filming agent that cannot be covered in the surface of nicotiana alkaloids well.
Optionally, the filming agent includes methylcellulose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose, vinegar
One of acid cellulose, cellulose acetate-phthalate or combination.
It should be understood that selecting above-mentioned methylcellulose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose, acetic acid
One of cellulose, cellulose acetate-phthalate or combination are used as filming agent, have and are soluble in solvent, overlay film effect
Well, and will not be by supercritical fluid extraction the characteristics of, can coat nicotiana alkaloids well and form nicotine essence particle, inclusion
Rate is high.
Optionally, in the step a, the solvent includes alcohol or alcoholic solution.
Specifically, the alcohol includes methanol and one kind of ethyl alcohol or combine；
Specifically, one of methanol solution and ethanol solution that the alcoholic solution includes volume fraction no more than 50% or
A variety of combinations.
It should be understood that selecting one of methanol solution, ethanol solution or a variety of combinations as solvent, one side energy
Enough be well dissolved in filming agent and nicotine essence is formed together homogeneous phase solution, consequently facilitating filming agent can be covered in tobacco
The surface of alkaloid, and covered effect is good；On the other hand it is easy to avoid nicotine essence particle obtained by supercritical fluid extraction
Residual solvent.
Optionally, in the step a, the weight ratio of the nicotine essence and the filming agent is 1:(2~10), for example,
1:2,1:3,1:4,1:5,1:6,1:7,1:8,1:9,1:10 etc..
Optionally, in the step b, the supercritical fluid is supercritical CO2；Supercritical CO2With nontoxic, tasteless, no
Combustion and inexpensive feature.
Optionally, in the step b, the pressure of the supercritical extraction reactor is 20~30MPa, for example, 20MPa,
23MPa, 25MPa, 27MPa, 30MPa etc..
Optionally, the temperature of the supercritical extraction reactor is 35~50 DEG C, for example, 35 DEG C, 38 DEG C, 40 DEG C, 43 DEG C, 45
DEG C, 48 DEG C, 50 DEG C etc..
It should be understood that the pressure and temperature range of supercritical extraction reactor will affect the nicotine essence particle to be formed, work as temperature
When degree is with hypotony, the supercritical fluid of supercritical extraction reactor cannot keep flow morphology, thus can not be in suspension
Solvent is extracted, it is more difficult to nicotine essence particle be precipitated；When temperature and hypertonia, the extraction selectivity of supercritical fluid
It is low, only solvent cannot be extracted completely, cause the nicotine essence particle being precipitated impure.
Optionally, in the step c, the pressure of the separating still is 15~25MPa, for example, 15MPa, 18MPa,
20MPa, 22MPa, 25MPa etc..
Optionally, the temperature of the separating still is 15~25 DEG C, for example, 15 DEG C, 16 DEG C, 17 DEG C, 18 DEG C, 20 DEG C, 22
DEG C, 23 DEG C, 25 DEG C etc..
Optionally, in the step b, the injection direction phase of the injection direction of the supercritical fluid and the suspension
Instead.
It should be understood that enabling supercritical fluid and suspension by injecting supercritical fluid in opposite directions with suspension
Sufficiently, so that supercritical fluid can carry out counter-current extraction to the solvent in suspension, supercritical fluid consumption is few for contact,
Extraction yield is high.
As an embodiment, the supercritical fluid sprays upwards from the bottom of the supercritical extraction reactor；Institute
It states suspension to inject from the kettle top of the supercritical extraction reactor, flow velocity 0.01-1L/min, for example, 0.01L/min, 0.1L/
Min, 0.3L/min, 0.5L/min, 0.6L/min, 0.8L/min, 1.0L/min etc..
It should be understood that being lower than supercritical extraction reactor by the pressure of control separating still, and control enters separating still
Uninterrupted, so that supercritical fluid is made to form gas in separating still when entering separating still from supercritical extraction reactor, with
The solvent of liquid separates.
In order to guarantee the separating effect of supercritical fluid Yu the solvent, in the step c, the supercritical fluid will be molten
Agent extraction after enter the separating still flow velocity be 0.5-3L/min, for example, 0.5L/min, 0.8L/min, 1.0L/min,
1.2L/min, 1.5L/min, 2.0L/min, 2.2L/min, 2.5L/min, 2.8L/min, 3.0L/min etc..
It is above-mentioned, supercritical fluid enter supercritical extraction reactor flow velocity adapt to supercritical fluid by after solvent extraction together into
Enter the flow velocity of the separating still.
Embodiment of the present invention is described in detail below in conjunction with specific embodiment, but those skilled in the art
It will be understood that the following example is merely to illustrate the present invention, and it is not construed as limiting the scope of the invention.It is not specified in embodiment
Actual conditions person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer,
It is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
The nicotine essence 500g that biological tobacco alkali content is 90wt% is weighed, the carboxymethyl cellulose of 1.5kg is added, by two
Person's mixing puts into stirring sufficiently dissolution in the ethanol solution that volume fraction is 90% and continues to stir, make after all dissolutions
Suspension is obtained for 3 to pH value with the salt acid for adjusting pH of 2mol/L.
By the suspension and supercritical CO2Supercritical extraction reactor is pumped by high-pressure pump, wherein suspension is with 0.5L/
The speed of min is sprayed down from the kettle top portion of supercritical extraction reactor, supercritical CO2It is up sprayed from the bottom of supercritical extraction reactor
It penetrates；Temperature in supercritical extraction reactor is 35 DEG C, pressure 25MPa；The supercritical fluid is mixed and is incited somebody to action with the suspension
Solvent extraction in the suspension is precipitated and collects nicotine essence particle.
The supercritical fluid will be entered in separating still after solvent extraction with the speed of 1L/min, and the temperature of separating still is 15
DEG C, pressure 15MPa, supercritical fluid forms gas, separates with the solvent of liquid, recycles.
Collecting supercritical extraction reactor bottom particles is nicotine essence particle, and through micro- measurement, diameter is distributed as 4.5-12 μ
Nicotine essence particle between m accounts for the 90% of total nicotine essence particle, and the average grain diameter of nicotine essence particle is 7.5 μm, simultaneously
Use the average value of the biological tobacco alkali content in gas chromatography measurement nicotine essence particle for 75wt%.
Compared with the uncoated nicotiana alkaloids essence of equivalent, fragrance stationary phase extends 11 months.
Embodiment 2
The nicotine essence 500g that biological tobacco alkali content is 90wt% is weighed, the carboxymethyl cellulose of 5kg is added, by the two
Mixing puts into stirring sufficiently dissolution in the ethanol solution that volume fraction is 90% and continues to stir after all dissolutions, uses
The salt acid for adjusting pH of 2mol/L obtains suspension to pH value for 5.
By the suspension and supercritical CO2Supercritical extraction reactor is pumped into wherein by high-pressure pump, and suspension is with 0.5L/
The speed of min is sprayed down from the kettle top portion of supercritical extraction reactor, supercritical CO2It is up sprayed from the bottom of supercritical extraction reactor
It penetrates；Temperature in supercritical extraction reactor is 35 DEG C, pressure 25MPa；The supercritical fluid is mixed and is incited somebody to action with the suspension
Solvent extraction in the suspension is precipitated and collects nicotine essence particle.
The supercritical fluid will be entered in separating still after solvent extraction with the speed of 1L/min, and the temperature of separating still is 15
DEG C, pressure 15MPa；Supercritical fluid forms gas, separates with the solvent of liquid, recycles.
Collecting supercritical extraction reactor bottom particles is nicotine essence particle, and through micro- measurement, diameter is distributed in 1-13.2 μ
Nicotine essence particle between m accounts for the 87% of total nicotine essence particle, and the average grain diameter of nicotine essence particle is 7.8 μm, simultaneously
Use the average value of the biological tobacco alkali content of gas chromatography measurement nicotine essence particle for 72wt%.
Compared with the uncoated nicotiana alkaloids essence of equivalent, fragrance stationary phase extends 10 months.
Embodiment 3
The nicotine essence 500g that biological tobacco alkali content is 92wt% is weighed, the carboxymethyl cellulose of 1kg is added, by the two
Mixing puts into stirring sufficiently dissolution in the ethanol solution that volume fraction is 90% and continues to stir after all dissolutions, uses
The salt acid for adjusting pH of 2mol/L obtains suspension to pH value for 2.
By the suspension and supercritical CO2Supercritical extraction reactor is pumped into wherein by high-pressure pump, and suspension is with 0.5L/
The speed of min is sprayed down from the kettle top portion of supercritical extraction reactor, supercritical CO2It is up sprayed from the bottom of supercritical extraction reactor
It penetrates.Temperature in supercritical extraction reactor is 35 DEG C, pressure 25MPa；The supercritical fluid is mixed and is incited somebody to action with the suspension
Solvent extraction in the suspension is precipitated and collects nicotine essence particle.
The supercritical fluid will be entered in separating still after solvent extraction with the speed of 1L/min, and the temperature of separating still is 15
DEG C, pressure 15MPa, supercritical fluid forms gas, separates with the solvent of liquid, recycles.
Collecting supercritical extraction reactor bottom particles is nicotine essence particle, and through micro- measurement, diameter is distributed in 2.6-
Nicotine essence particle between 14.1 μm accounts for the 78% of total nicotine essence particle, and the average grain diameter of nicotine essence particle is 7.4 μm,
Use the average value of the biological tobacco alkali content of gas chromatography measurement nicotine essence particle for 79wt% simultaneously.
Compared with the uncoated nicotiana alkaloids essence of equivalent, fragrance stationary phase extends 10.5 months.
Embodiment 4
The nicotine essence 500g that biological tobacco alkali content is 92wt% is weighed, the carboxymethyl cellulose of 1.5kg is added, by two
Person's mixing puts into stirring sufficiently dissolution in the ethanol solution that volume fraction is 90% and continues to stir, make after all dissolutions
Suspension is obtained for 3 to pH value with the salt acid for adjusting pH of 2mol/L.
By the suspension and supercritical CO2Supercritical extraction reactor is pumped by high-pressure pump, wherein suspension is with 1L/min
Speed sprayed down from the kettle top portion of supercritical extraction reactor, supercritical CO2It is up sprayed from the bottom of supercritical extraction reactor；It is super
Temperature in critical extraction kettle is 45 DEG C, pressure 30MPa；The supercritical fluid mixes with the suspension and will be described outstanding
Solvent extraction in supernatant liquid is precipitated and collects nicotine essence particle.
The supercritical fluid will be entered in separating still after solvent extraction with the speed of 1L/min, and the temperature of separating still is 15
DEG C, pressure 15MPa, supercritical fluid forms gas, separates with the solvent of liquid, recycles.
Collecting supercritical extraction reactor bottom particles is nicotine essence particle, and through micro- measurement, diameter is distributed in 1.5-15 μ
Nicotine essence particle between m accounts for the 82% of total nicotine essence particle, and the average grain diameter of nicotine essence particle is 6.8 μm, simultaneously
Use the average value of the biological tobacco alkali content of gas chromatography measurement nicotine essence particle for 77wt%.
Compared with the uncoated nicotiana alkaloids essence of equivalent, fragrance stationary phase extends 12 months.
Embodiment 5
The nicotine essence 500g that biological tobacco alkali content is 92wt% is weighed, the carboxymethyl cellulose of 1.5kg is added, by two
Person's mixing puts into stirring sufficiently dissolution in the ethanol solution that volume fraction is 90% and continues to stir, make after all dissolutions
Suspension is obtained for 3 to pH value with the salt acid for adjusting pH of 2mol/L.
By the suspension and supercritical CO2Supercritical extraction reactor is pumped by high-pressure pump, wherein suspension is with 0.01L/
The speed of min is sprayed down from the kettle top portion of supercritical extraction reactor, supercritical CO2,It is up sprayed from the bottom of supercritical extraction reactor
It penetrates；Temperature in supercritical extraction reactor is 50 DEG C, pressure 20MPa；The supercritical fluid is mixed and is incited somebody to action with the suspension
Solvent extraction in the suspension is precipitated and collects nicotine essence particle.
The supercritical fluid will be entered in separating still after solvent extraction with the speed of 0.5L/min, and the temperature of separating still is
15 DEG C, pressure 15MPa, supercritical fluid forms gas, separates with the solvent of liquid, recycles.
Collecting supercritical extraction reactor bottom particles is nicotine essence particle, and through micro- measurement, diameter is distributed in 1.8-13 μ
Nicotine essence particle between m accounts for the 84% of total nicotine essence particle, and the average grain diameter of nicotine essence particle is 6.3 μm, simultaneously
Use the average value of the biological tobacco alkali content of gas chromatography measurement nicotine essence particle for 78wt%.
Compared with the uncoated nicotiana alkaloids essence of equivalent, fragrance stationary phase extends 11 months.
Embodiment 6
The nicotine essence 500g that biological tobacco alkali content is 95wt% is weighed, the ethyl cellulose of 1.5kg is added, by the two
Mixing puts into stirring sufficiently dissolution in the ethanol solution that volume fraction is 90% and continues to stir after all dissolutions, uses
The salt acid for adjusting pH of 2mol/L obtains suspension to pH value for 3.
By the suspension and supercritical CO2Supercritical extraction reactor is pumped by high-pressure pump, wherein suspension is with 0.1L/
The speed of min is sprayed down from the kettle top portion of supercritical extraction reactor, supercritical CO2It is up sprayed from the bottom of supercritical extraction reactor
It penetrates；Temperature in supercritical extraction reactor is 35 DEG C, pressure 20MPa；The supercritical fluid is mixed and is incited somebody to action with the suspension
Solvent extraction in the suspension is precipitated and collects nicotine essence particle.
The supercritical fluid will be entered in separating still after solvent extraction with the speed of 0.5L/min, and the temperature of separating still is
15 DEG C, pressure 15MPa, supercritical fluid forms gas, separates with the solvent of liquid, recycles.
Collecting supercritical extraction reactor bottom particles is nicotine essence particle, and through micro- measurement, diameter is distributed as 2.3-14 μ
Nicotine essence particle between m accounts for the 73% of total nicotine essence particle, and the average grain diameter of nicotine essence particle is 7.2 μm, simultaneously
Use the average value of the biological tobacco alkali content of gas chromatography measurement nicotine essence particle for 76wt%.
Compared with the uncoated nicotiana alkaloids essence of equivalent, fragrance stationary phase extends 10 months.
Embodiment 7
The nicotine essence 500g that biological tobacco alkali content is 95wt% is weighed, the ethyl cellulose of 1.5kg is added, by the two
Mixing puts into stirring sufficiently dissolution in the ethanol solution that volume fraction is 90% and continues to stir after all dissolutions, uses
The salt acid for adjusting pH of 2mol/L obtains suspension to pH value for 3.
By the suspension and supercritical CO2Supercritical extraction reactor is pumped by high-pressure pump, wherein suspension is with 1L/min
Speed sprayed down from the kettle top portion of supercritical extraction reactor, supercritical CO2It is up sprayed from the bottom of supercritical extraction reactor.It is super
Temperature in critical extraction kettle is 35 DEG C, pressure 30MPa；The supercritical fluid mixes with the suspension and will be described outstanding
Solvent extraction in supernatant liquid is precipitated and collects nicotine essence particle.
The supercritical fluid will be entered in separating still after solvent extraction with the speed of 3L/min, and the temperature of separating still is 15
DEG C, pressure 20MPa, supercritical fluid forms gas, separates with the solvent of liquid, recycles.
Collecting supercritical extraction reactor bottom particles is nicotine essence particle, and through micro- measurement, diameter is distributed in 3.6-15 μ
Nicotine essence particle between m accounts for the 84% of total nicotine essence particle, and the average grain diameter of nicotine essence particle is 6.9 μm, simultaneously
Use the average value of the biological tobacco alkali content of gas chromatography measurement nicotine essence particle for 78wt%.
Compared with the uncoated nicotiana alkaloids essence of equivalent, fragrance stationary phase extends 11.5 months.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
In addition, it will be appreciated by those of skill in the art that although some embodiments in this include institute in other embodiments
Including certain features rather than other feature, but the combination of the feature of different embodiment means in the scope of the present invention
Within and form different embodiments.For example, in claims above, embodiment claimed it is any it
One can in any combination mode come using.The information disclosed in the background technology section is intended only to deepen to the present invention
General background technology understanding, and be not construed as recognizing or imply that information composition has been this field skill in any form
The prior art well known to art personnel.
Claims (10)
1. a kind of preparation method of nicotine essence particle, which comprises the steps of:
Step a. mixes nicotine essence with filming agent, and solvent dissolution is added, and adjusts after pH value is 2~5 and obtains suspension；
Step b. injects the suspension and supercritical fluid in supercritical extraction reactor, the supercritical fluid and the suspension
Liquid mixes and by the solvent extraction in the suspension, and nicotine essence particle is precipitated.
2. the preparation method of nicotine essence particle according to claim 1, which is characterized in that further include that step c. will be described
Nicotine essence particle is separated with the supercritical fluid for being mixed with the solvent, then by the supercritical fluid with it is described molten
Agent is injected in separating still together, and the supercritical fluid is separated with the solvent.
3. the preparation method of nicotine essence particle according to claim 1, which is characterized in that the filming agent includes methyl
Cellulose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose, cellulose acetate, in cellulose acetate-phthalate
A kind of or combination.
4. the preparation method of nicotine essence particle according to claim 1, which is characterized in that in the step a, the cigarette
The weight ratio of alkali essence and the filming agent is 1:(2~10).
5. the preparation method of nicotine essence particle according to claim 1, which is characterized in that described molten in the step a
Agent includes alcohol or alcoholic solution.
6. the preparation method of nicotine essence particle according to claim 1, which is characterized in that described super in the step b
The pressure of critical extraction kettle is 20~30MPa, and temperature is 35~50 DEG C.
7. the preparation method of nicotine essence particle according to claim 2, which is characterized in that in the step c, described point
Pressure from kettle is 15~25MPa, and temperature is 15~25 DEG C.
8. the preparation method of nicotine essence particle according to claim 1, which is characterized in that described super in the step b
The injection direction of critical fluids is opposite with the injection direction of the suspension.
9. the preparation method of nicotine essence particle according to claim 8, which is characterized in that the supercritical fluid is from institute
It sprays upwards the bottom for stating supercritical extraction reactor；The suspension is injected from the kettle top of the supercritical extraction reactor, and flow velocity is
0.01-1L/min。
10. the preparation method of nicotine essence particle according to claim 2, which is characterized in that described in the step c
The flow velocity for entering the separating still after solvent extraction is 0.5-3L/min by supercritical fluid.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104450186A (en) * | 2014-10-29 | 2015-03-25 | 山东中烟工业有限责任公司 | Method for preparing tobacco herbal fragrant substance for cigarette solution of electronic cigarette |
| CN109007954A (en) * | 2018-09-11 | 2018-12-18 | 鹰潭华宝香精有限公司 | A kind of method of supercritical fluid preparation tobacco extractive microcapsule |
| CN110141605A (en) * | 2019-04-19 | 2019-08-20 | 南京康齐生物科技有限公司 | A kind of preparation method of snowpoppy total alkaloid nanoparticle |
-
2019
- 2019-08-27 CN CN201910796598.2A patent/CN110484367A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104450186A (en) * | 2014-10-29 | 2015-03-25 | 山东中烟工业有限责任公司 | Method for preparing tobacco herbal fragrant substance for cigarette solution of electronic cigarette |
| CN109007954A (en) * | 2018-09-11 | 2018-12-18 | 鹰潭华宝香精有限公司 | A kind of method of supercritical fluid preparation tobacco extractive microcapsule |
| CN110141605A (en) * | 2019-04-19 | 2019-08-20 | 南京康齐生物科技有限公司 | A kind of preparation method of snowpoppy total alkaloid nanoparticle |
Non-Patent Citations (2)
| Title |
|---|
| 巩效伟等: "β-环糊精微胶囊的制备及其在电子烟烟液中的应用", 《烟草科技》 * |
| 杨君等: "烟用香精微胶囊技术及其应用前景", 《中国食品工业》 * |
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Application publication date: 20191122 |