CN109892690A - A kind of cigarette graphene-based complex microsphere and preparation method thereof - Google Patents
A kind of cigarette graphene-based complex microsphere and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of cigarette graphene-based complex microspheres and preparation method thereof and the application in cigarette, belong to cigarette additive technical field.Graphene oxide is restored using natural reducing agent, obtained redox graphene is reacted with Fruity type aldehyde compound and Dopamine hydrochloride, then Soxhlet extraction, the graphene-based composite material with molecular recognition function is obtained, cigarette finally is made with graphene-based complex microsphere in graphene-based composite material compounding made from various different aldehyde compounds.The microballoon can from complicated natural essence fragrance selective absorption isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde and melonal, object and capacity controllable are adsorbed, and active force is mainly non-covalent bonding force between the microballoon binding molecule, there is preferable heat conductivity, in use, it can quickly be desorbed.Additive is made in the microballoon to be added in filter tip in use, fruity can not only be provided, promotion cigarette flavor matter improves suction comfort, moreover it is possible to prevent structure heat from collapsing.
Description
Technical field
The invention belongs to cigarette additive technical fields, and in particular to a kind of cigarette graphene-based complex microsphere and its preparation
Method and the application in cigarette.
Background technique
Graphene (Graphene) is a kind of two dimension for forming hexangle type in honeycomb lattice with sp2 hybridized orbit by carbon atom
Carbon nanomaterial.Graphene has excellent optics, electricity, mechanical characteristic, in materialogy, micro-nano technology, the energy, biomedicine
It is with important application prospects with drug delivery etc., it is considered to be a kind of future revolutionary material.
Cigarette additive is the auxiliary agent for improving tobacco physicochemical property, including flavors and fragrances, humectant, combustion adjuvant, mould inhibitor
And adsorbent.Wherein, it is to cover the irritation of natural baccy and miscellaneous gas etc. using the purpose of flavors and fragrances, and improves or improve
Its fragrance.The flavors and fragrances that application is added in cigarette is divided into natural perfume material and synthetic perfume two major classes by separate sources, at present state
Interior essence spice for cigarette manufacturing enterprise mostly uses greatly conventional extracted form natural plant path, or shallowly processing foreign is deployed
Flavors and fragrances.The flavors and fragrances complicated component of extracted form natural plant, wherein being also also easy to produce comprising more actual application negative
The chemical component of face effect.And current effect of the tobacco aromaticss carrier without specific recognition adsorption function ingredient, meanwhile, in master
Flue gas is flowed by fashion incapability when promoting cigarette smoking quality, the function that improvement plug configuration heat collapses.Therefore how to overcome
The problem of the deficiencies in the prior art are current cigarette additive technical field urgent need to resolve.
Summary of the invention
It is an object of the present invention to solve the deficiency of the existing technology and provide a kind of graphene-based complex microsphere of cigarette and its
Preparation method and the application in cigarette, the cigarette can be from complicated natural essence fragrance selectively with graphene-based complex microsphere
Isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde and melonal are adsorbed, object is adsorbed and adsorption capacity is controllable, and the microballoon has heat well
Conductibility can realize fruity class function when cigarette is burnt and sucked, main flume passes through under higher flue-gas temperature and suction
The quick desorption of energy ingredient；Fruity type cigarette filter tip additive is made with graphene-based complex microsphere in the cigarette, is added to filter
In use, fruity note can not only be provided, promote cigarette flavor matter in mouth, moreover it is possible to prevent from collapsing, application easy to spread.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of cigarette preparation method of graphene-based complex microsphere, includes the following steps:
Step (1), selection specific surface area are 300 ~ 700 m2/ g, piece diameter are 7 ~ 15 μm, the graphite oxide of average 6 ~ 20 layers of the number of plies
Alkene；
Step (2), by step (1) choose graphene oxide using natural reducing agent carry out reduction reaction, obtain C/O be 4.5 ~
8 redox graphene；
Step (3), it is 0.5 ~ 1.0 mg/ that the redox graphene that step (2) obtains, which is added in PBS buffer solution to concentration,
The Fruity type aldehydes chemical combination that quality is 2 ~ 5 times of redox graphene quality is added to after being uniformly dispersed in mL, ultrasound thereto
Object, while Dopamine hydrochloride is added, it is stirred to react, is centrifuged, then solid formation washing is the first of 9 ~ 12% acetic acid with mass concentration
Alcoholic solution Soxhlet extraction obtains the graphene-based composite material with molecular recognition function to remove Fruity type aldehyde compound；
Wherein, the mass ratio of Dopamine hydrochloride and redox graphene is 1:0.6 ~ 1.2；
The Fruity type aldehyde compound is isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde or melonal；
Isopentyl aldehyde respectively, octanal, aldehyde C-9, capraldehyde, melonal are graphene-based composite material made from raw material, pressed by step (4)
Mass ratio 1:0.5 ~ 0.8:1 ~ 1.2:0.7 ~ 0.9:0.3 ~ 0.5 is mixed, and obtained mixture is then added to mass concentration
In glucose solution for 0.1 ~ 0.5 g/mL, ultrasound is to after being uniformly dispersed, electrostatic spray, and wet process is collected, and obtains cigarette graphite
Alkenyl complex microsphere；
The solid-liquid ratio of the glucose solution and mixture is 0.1 ~ 0.5 g/mL.
The present invention is not particularly limited the number of the time of centrifugation, the time of ultrasound, washing.
It is further preferred that the natural reducing agent is vitamin C, half Guang ammonia of chitosan, gallic acid or L-
Acid.
The present invention for being not specifically limited using the reducing condition of above-mentioned reducing agent, according to the condition in existing method into
Row controls the C/O of redox graphene by the control reaction time during the reaction.
It is further preferred that the pH of the PBS buffer solution is 7.5 ~ 8.0.
It is further preferred that mixing time is 0.5 ~ 3 h in step (3).
The present invention additionally provides a kind of preparation methods of Fruity type cigarette filter tip additive, using above-mentioned cigarette graphene
Base complex microsphere, includes the following steps:
Cigarette is soaked in graphene-based complex microsphere containing one in isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal by step (A)
It is adsorbed in kind or several natural essence spice solutions, after saturation to be adsorbed, is taken out, low temperature drying；
Step (B), after spermaceti and lanocerin are mixed according to mass ratio for 1:0.2 ~ 0.3, to whole meltings under reduced pressure
Afterwards, microballoon after step (A) drying is immersed, takes out, stand after 7 ~ 15s, the time is no less than 5 min；
Step (C), plant amylum is added into deionized water, while emulsion adjuvant is added, will be through step after being stirred until homogeneous
(B) microballoon stood is immersed, and is taken out after 3 ~ 6s, is spontaneously dried to get Fruity type cigarette filter tip additive.
The present invention is for containing natural essence fragrance one or more of in isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal
It is not specifically limited, such as tangerine oil.
It is further preferred that the temperature of low temperature drying is 2 ~ 6 DEG C in step (A).
It is further preferred that plant amylum described in step (C) is pueraria starch, pawpaw starch and acorn starch
The combination of middle one or more.When for composition, mutually before the ratio present invention be not specially limited.
It is further preferred that the mass ratio of the plant amylum, deionized water and emulsion adjuvant is 1 ~ 3:10 ~ 20:
0.07~0.12；The emulsion adjuvant is polyethylene glycol 400, sucrose ester, fatty acid esters of sorbitan, glucan, Span-
20 or Span-40.
It is further preferred that the diameter of the Fruity type cigarette filter tip additive is 1.5 ~ 3.5 mm.
The present invention protects cigarette made from the preparation method of above-mentioned Fruity type cigarette filter tip additive with graphene-based simultaneously
Application of the complex microsphere in cigarette.
The present invention in order to control the adsorption capacity of isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal, select specific surface area for
300~700 m2/ g, piece diameter are 7 ~ 15 μm, the graphene oxide of average 6 ~ 20 layers of the number of plies.Later to graphene oxide carry out portion
Divide reduction, improves its heating conduction；It is polymerize later by monomer of Dopamine hydrochloride, preparing has answering for molecular recognition function
Condensation material, the composite material can increase the specific surface area and recognition site of imprinted material, and can be effectively reduced template point
The resistance to mass tranfer that son is adsorbed and is desorbed in the polymeric material.The present invention is according to isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, muskmelon
Aldehyde is that graphene-based composite material made from raw material carries out the compatibility of science, and microballoon is made, which can be more multiple from ingredient
Selective absorption isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde and melonal in miscellaneous natural essence fragrance adsorb object and capacity controllable,
And the microballoon has preferable heat conductivity, when main flume passes through under flue-gas temperature and suction effect, so that inhaling
Attached substance fast implements desorption.
Cigarette of the present invention can be used alone with graphene-based complex microsphere, after adsorbing aldehyde compound, add as additive
It is added in filter tip, fragrance can not only be assigned, moreover it is possible to prevent heat from collapsing.
Fruity type cigarette filter tip additive produced by the present invention is three layers of spherical structure, and internal layer ball is cigarette with graphene-based
Complex microsphere, middle layer are temperature sensing material, and outer layer is plant amylum layer.With the mixture wrapping inner layer microballoon of spermaceti and lanocerin
The compound for being beneficial to prevent selective absorption is desorbed due to storing for a long time in air or denaturation.The temperature sensing material exists
It is solid-state under room temperature, will become liquid in aspiration procedure, which facilitates the desorption of above-mentioned Fruity type aldehyde compound.
Simultaneously, it is contemplated that filter tip can lead to the problem of collapse in use, the present invention first, by graphene oxide portion
Divide reduction, plays thermal conduction effect；Second, extra temperature sensing material liquid is buffered using outer layer plant amylum layer, prevents Yin Wen
It is collapsed caused by quick material swelling.The present invention also optimizes suction mouthfeel, fruity is provided first with endothecium structure, inside
When layer spherical structure preparation, threshold value and the hamony of various Fruity type compounds are fully taken into account to be deployed, in combination with outer
The layer further enhanced products style of plant amylum layer, acquired fragrance is naturally pure and fresh, graceful mellow.
The source chemicals used in preparation process of the present invention are environmentally protective, meet consumption concept under the new situation.
Compared with prior art, the present invention has the advantages that:
(1) cigarette of the present invention with graphene-based complex microsphere can from complicated natural essence fragrance selective absorption isopentyl aldehyde, pungent
Aldehyde, aldehyde C-9, capraldehyde and melonal, adsorb object and adsorption capacity is controllable, and the microballoon has good heat conductivity, is using
In the process, targeted functional ingredients can quickly be desorbed；
(2) for cigarette of the present invention with graphene-based complex microsphere in absorption, molten for propylene glycol, water-soluble or oily molten etc. essence is fragrant
Material is adsorbable, is not particularly limited；
(3) Fruity type cigarette filter tip additive is made with graphene-based complex microsphere in the cigarette, is added in filter tip and uses
When, fruity can not only be provided, cigarette flavor quality is promoted, improve suction comfort, moreover it is possible to prevent plug configuration from collapsing, be easy to push away
Wide application.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and it should not be regarded as limiting this hair
Bright range.In the examples where no specific technique or condition is specified, described technology or conditions according to the literature in the art
Or it is carried out according to product description.Production firm person is not specified in material therefor or equipment, is that can be obtained by purchase
Conventional products.
Embodiment 1
A kind of cigarette preparation method of graphene-based complex microsphere, includes the following steps:
Step (1), choosing specific surface area is about 450 m2/ g, piece diameter are 8 ~ 12 μm, the graphite oxide of average 7 ~ 12 layers of the number of plies
Alkene；
Step (2), the graphene oxide that step (1) is chosen carry out reduction reaction using natural reducing agent, and obtaining C/O is about 6
Redox graphene；
Step (3), it is 0.5 mg/mL that the redox graphene that step (2) obtains, which is added in PBS buffer solution to concentration,
To after being uniformly dispersed the Fruity type aldehyde compound that quality is 3 times of redox graphene quality is added, simultaneously in ultrasound thereto
Dopamine hydrochloride is added, is stirred to react, is centrifuged, solid formation washing, then with the methanol solution for containing mass concentration being 9% acetic acid
Soxhlet extraction is carried out to remove Fruity type aldehyde compound, obtains graphene-based composite material；
Wherein, the mass ratio of Dopamine hydrochloride and redox graphene is 1:0.6；
The Fruity type aldehyde compound is isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde or melonal；
Step (4), will respectively using isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal as graphene-based composite material made from raw material,
It is 1:0.5:1:0.7:0.3 mixing according to mass ratio, it is 0.1 g/mL that obtained mixture, which is then added to mass concentration,
Glucose solution in, ultrasound to after being uniformly dispersed, electrostatic spray, wet process collect, obtain cigarette with graphene-based complex microsphere；
The solid-liquid ratio of the glucose solution and mixture is 0.1 g/mL.
Wherein, the natural reducing agent is the vitamin c solution of 7.5 wt%.
Embodiment 2
A kind of cigarette preparation method of graphene-based complex microsphere, includes the following steps:
Step (1), choosing specific surface area is about 500 m2/ g, piece diameter are 7 ~ 10 μm, the graphite oxide of average 11 ~ 15 layers of the number of plies
Alkene；
Step (2), the graphene oxide that step (1) is chosen carry out reduction reaction using natural reducing agent, and obtaining C/O is about 8
Redox graphene；
Step (3), the redox graphene that step (2) obtains is added in the PBS buffer solution that pH is 7.5 is to concentration
The Fruity type aldehydes that quality is 5 times of redox graphene quality is added to after being uniformly dispersed in 1.0 mg/mL, ultrasound thereto
Compound, while Dopamine hydrochloride is added, 2.5 h are stirred to react, are centrifuged, then solid formation washing is with containing mass concentration
The methanol solution of 12% acetic acid carries out Soxhlet extraction to remove Fruity type aldehyde compound, obtains the stone with molecular recognition function
Mertenyl composite material；
Wherein, the mass ratio of Dopamine hydrochloride and redox graphene is 1:1.2；
The Fruity type aldehyde compound is isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde or melonal；
Step (4), will respectively using isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal as graphene-based composite material made from raw material,
It is 1:0.8:1.2:0.9:0.5 mixing according to mass ratio, it is 0.5 g/ that obtained mixture, which is then added to mass concentration,
In the glucose solution of mL, ultrasound is to after being uniformly dispersed, electrostatic spray, and wet process is collected, and obtains cigarette with graphene-based complex microsphere；
The solid-liquid ratio of the glucose solution and mixture is 0.5 g/mL.
Wherein, the natural reducing agent is the acidic aqueous solution of chitosan.
Embodiment 3
A kind of cigarette preparation method of graphene-based complex microsphere, includes the following steps:
Step (1), choosing specific surface area is about 300 m2/ g, piece diameter are 12 ~ 15 μm, the graphite oxide of average 16 ~ 20 layers of the number of plies
Alkene；
Step (2), the graphene oxide that step (1) is chosen carry out reduction reaction using natural reducing agent, and obtaining C/O is about 5
Redox graphene；
Step (3), the redox graphene that step (2) obtains is added in the PBS buffer solution that pH is 8.0 is to concentration
The Fruity type aldehyde that quality is 2.5 times of redox graphene quality is added to after being uniformly dispersed in 0.6 mg/mL, ultrasound thereto
Class compound, while Dopamine hydrochloride is added, is stirred to react 0.5 h, is centrifuged, solid formation washing, then with containing mass concentration
Soxhlet extraction is carried out to remove Fruity type aldehyde compound for the methanol solution of 10% acetic acid, obtains graphene-based composite material；
Wherein, the mass ratio of Dopamine hydrochloride and redox graphene is 1:0.6；
The Fruity type aldehyde compound is isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde or melonal；
Step (4), will respectively using isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal as graphene-based composite material made from raw material,
It is 1:0.7:1.1:0.8:0.4 mixing according to mass ratio, it is 0.2 g/ that obtained mixture, which is then added to mass concentration,
In the glucose solution of mL, ultrasound is to after being uniformly dispersed, electrostatic spray, and wet process is collected, and obtains cigarette with graphene-based complex microsphere；
The solid-liquid ratio of the glucose solution and mixture is 0.4 g/mL.
Wherein, the natural reducing agent is the gallic acid of 5 wt% and the mixture solution of Victoria C (m/m=1:1).
Embodiment 4
A kind of cigarette preparation method of graphene-based complex microsphere, includes the following steps:
Step (1), choosing specific surface area is about 700 m2/ g, piece diameter are 7 ~ 9 μm, the graphene oxide of average 6 ~ 10 layers of the number of plies；
Step (2), the graphene oxide that step (1) is chosen carry out reduction reaction using natural reducing agent, and obtaining C/O is about
4.5 redox graphene；
Step (3), the redox graphene that step (2) obtains is added in the PBS buffer solution that pH is 7.8 is to concentration
The Fruity type aldehydes that quality is 2 times of redox graphene quality is added to after being uniformly dispersed in 0.7 mg/mL, ultrasound thereto
Compound, while Dopamine hydrochloride is added, 3 h are stirred to react, are centrifuged, then solid formation washing is with containing mass concentration
The methanol solution of 11% acetic acid carries out Soxhlet extraction to remove Fruity type aldehyde compound, obtains graphene-based composite material；
Wherein, the mass ratio of Dopamine hydrochloride and redox graphene is 1:0.7；
The Fruity type aldehyde compound is isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde or melonal；
Step (4), will respectively using isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal as graphene-based composite material made from raw material,
It is 1:0.66:1.05:0.75:0.42 mixing according to mass ratio, obtained mixture, which is then added to mass concentration, is
In the glucose solution of 0.25 g/mL, ultrasound is to after being uniformly dispersed, electrostatic spray, and wet process is collected, and obtains cigarette with graphene-based multiple
Close microballoon；
The solid-liquid ratio of the glucose solution and mixture is 0.15 g/mL.
Wherein, the natural reducing agent is the L-cysteine of 7 wt% and the mixture solution of Victoria C, the two mass ratio
For 1:2.
Embodiment 5
A kind of preparation method of Fruity type cigarette filter tip additive, using cigarette described in embodiment 1 with graphene-based compound micro-
Ball includes the following steps:
Cigarette is soaked in graphene-based complex microsphere containing one in isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal by step (A)
It is adsorbed in kind or several natural essence spice solutions, after saturation to be adsorbed, is taken out, 2 DEG C of freeze-day with constant temperature；
Step (B), will under reduced pressure after all meltings after mixing spermaceti and lanocerin for 1:0.2 according to mass ratio
Microballoon is immersed after step (A) is dry, is taken out after 7s, time of repose is no less than 5 min；
Step (C), pueraria starch is added into deionized water, while emulsion adjuvant polyethylene glycol 400 is added, and is stirred until homogeneous
Afterwards, the microballoon stood through step (B) is immersed, is taken out after 3s, spontaneously dried and added to get Fruity type cigarette filter tip
Agent controls about 1.5 mm of its diameter；
The mass ratio of the plant amylum, deionized water and emulsion adjuvant is 1:10:0.10；
Embodiment 6
A kind of preparation method of Fruity type cigarette filter tip additive, using cigarette as described in example 2 with graphene-based compound micro-
Ball includes the following steps:
Cigarette is soaked in graphene-based complex microsphere containing one in isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal by step (A)
It is adsorbed in kind or several natural essence spice solutions, after saturation to be adsorbed, is taken out, it is dry at 6 DEG C；
Step (B), will under reduced pressure after all meltings after mixing spermaceti and lanocerin for 1:0.3 according to mass ratio
Microballoon is immersed after step (A) is dry, is taken out after 10 s, time of repose is no less than 5 min；
Step (C), pawpaw starch is added into deionized water, while sucrose ester is added as emulsion adjuvant, is stirred until homogeneous
Afterwards, the microballoon stood through step (B) is immersed, is taken out after 6 s, spontaneously dried and added to get Fruity type cigarette filter tip
Agent controls a diameter of about 3.5 mm；
The mass ratio of the plant amylum, deionized water and emulsion adjuvant is 3:20:0.1；
Embodiment 7
A kind of preparation method of Fruity type cigarette filter tip additive, using cigarette described in embodiment 3 with graphene-based compound micro-
Ball includes the following steps:
Cigarette is soaked in graphene-based complex microsphere containing one in isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal by step (A)
It is adsorbed in kind or several natural essence spice solutions, after saturation to be adsorbed, is taken out, it is dry at 3 DEG C；
Step (B), after spermaceti and lanocerin are mixed according to mass ratio for 1:0.25, under reduced pressure after all meltings,
Microballoon after step (A) drying is immersed, is taken out after 7s, time of repose is no less than 5 min；
Step (C), by plant amylum --- the mixture that pawpaw starch and acorn starch mass ratio are 1:1 is added to deionized water
In, while emulsion adjuvant glucan is added, after being stirred until homogeneous, the microballoon stood through step (B) is immersed, is taken after 5s
Out, it spontaneously dries to get Fruity type cigarette filter tip additive, controls a diameter of about 3.0 mm；
The mass ratio of the plant amylum, deionized water and emulsion adjuvant is 2:15:0.08；
Embodiment 8
A kind of preparation method of Fruity type cigarette filter tip additive, using cigarette as described in example 4 with graphene-based compound micro-
Ball includes the following steps:
Cigarette is soaked in graphene-based complex microsphere containing one in isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal by step (A)
It is adsorbed in kind or several natural essence spice solutions, after saturation to be adsorbed, is taken out, it is dry at 4 DEG C；
Step (B), after spermaceti and lanocerin are mixed according to mass ratio for 1:0.25, under reduced pressure after all meltings,
Microballoon after step (A) drying is immersed, takes out, stands after 15s, time of repose is no less than 5 min；
The mixture that plant amylum-pueraria starch, pawpaw starch and acorn starch mass ratio are 1:1:1 is added step (C)
Into deionized water, while emulsion adjuvant fatty acid esters of sorbitan is added, after being stirred until homogeneous, will be stood through step (B)
Microballoon be immersed, taken out after 4s, spontaneously dry the control a diameter of about 2.5 to get Fruity type cigarette filter tip additive
mm；
The mass ratio of the plant amylum, deionized water and emulsion adjuvant is 2:15:0.08；
Comparative example 1
The difference of comparative example 1 and embodiment 8 is that remaining is all identical using common graphene oxide.In preparation process, five kinds
Then Fruity type cigarette is added in the filter tip of identical trade mark cigarette by the equal adsorption saturation of aldehyde compound with filter tip with additive.
As a result compared with Example 8, found when suction, quality discrepancy is larger, is unfavorable for the control of product quality.
Comparative example 2
The difference of comparative example 2 and embodiment 8 is not restore graphene oxide, is added directly into PBS buffer solution, remaining all phase
Together.Obtained Fruity type cigarette filter tip is identical as the Adding Way of comparative example 1 with additive Adding Way.As a result, it has been found that taking out
When suction, the improvement collapsed to heat is unobvious, and 8 product of embodiment can significantly improve heat and collapse situation.
Comparative example 3
Comparative example 3 and the difference of embodiment 8 are: using isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal as graphite made from raw material
Alkenyl composite material directlys adopt pelletizer granulation, remaining is all identical using water as binder.As a result, it has been found that 3 cigarette of comparative example is used
Graphene-based complex microsphere holding time original is lower than 8 product of embodiment, fragile to be broken into powder.
Comparative example 4
Comparative example 4 has investigated the ratio of spermaceti and lanocerin on the basis of embodiment 8, carries out single factor experiment, obtained
Fruity type cigarette filter tip is identical as the Adding Way of comparative example 1 with additive Adding Way.As a result, it has been found that spermaceti adding proportion mistake
If few, obvious miscellaneous gas can be generated；If spermaceti adding proportion is excessive, then fruity gas can die down.
Comparative example 5
Comparative example 5 has investigated the type of starch on the basis of embodiment 8, carries out single factor experiment, obtained Fruity type cigarette
It is identical as the Adding Way of comparative example 1 with filter tip additive Adding Way.As a result, it has been found that using cornstarch, tapioca,
Sensory evaluating smoking's effect of potato starch is inferior to embodiment 8.
Performance detection
The graphene-based complex microsphere of 4 cigarette of embodiment 1- embodiment is adsorbed into lauryl aldehyde, myristic aldehyde, the hendecanal, peach aldehyde and coconut palm
Sub- aldehyde is to Fruity type aldehyde compound adsorption saturation, in cigarette filter tip shaping process with every/additive amount to conventional vinegar
In fine filter stick, and certain brand specification tobacco leaf formulation is used, Cigarette is made.Likewise, by embodiment 5-8 and comparative example 1-5
Filter stick for cigarettes additive, using identical product advise tobacco leaf formulation, roll into Cigarette.To be rolled up made of common vinegar fibre filter stick
For cigarette as control, the sense organ suction and heat for investigating cigarette sample collapse situation.Table 1 is that the heat of smoking cigarette collapses situation.Table 2 is
Cigarette sensory evaluating smoking evaluation, carries out according to GB5606.4-2005.
The variation of 1 cigarette smoking process plug configuration of table
2 cigarette sample sensory evaluation of table comparison
The basic principles, main features and advantages of the present invention have been shown and described above.The technical staff of the industry
It should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe the present invention
Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these variation and
Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent
Object defines.
Claims (10)
1. a kind of cigarette preparation method of graphene-based complex microsphere, which comprises the steps of:
Step (1), selection specific surface area are 300 ~ 700 m2/ g, piece diameter are 7 ~ 15 μm, the graphite oxide of average 6 ~ 20 layers of the number of plies
Alkene；
Step (2), by step (1) choose graphene oxide using natural reducing agent carry out reduction reaction, obtain C/O be 4.5 ~
8 redox graphene；
Step (3), it is 0.5 ~ 1.0 mg/ that the redox graphene that step (2) obtains, which is added in PBS buffer solution to concentration,
The Fruity type aldehydes chemical combination that quality is 2 ~ 5 times of redox graphene quality is added to after being uniformly dispersed in mL, ultrasound thereto
Object, while Dopamine hydrochloride is added, it is stirred to react, is centrifuged, then solid formation washing is the first of 9 ~ 12% acetic acid with mass concentration
Alcoholic solution Soxhlet extraction obtains the graphene-based composite material with molecular recognition function to remove Fruity type aldehyde compound；
Wherein, the mass ratio of Dopamine hydrochloride and redox graphene is 1:0.6 ~ 1.2；
The Fruity type aldehyde compound is isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde or melonal；
Isopentyl aldehyde respectively, octanal, aldehyde C-9, capraldehyde, melonal are graphene-based composite material made from raw material, pressed by step (4)
Mass ratio 1:0.5 ~ 0.8:1 ~ 1.2:0.7 ~ 0.9:0.3 ~ 0.5 is mixed, and obtained mixture is then added to mass concentration
In glucose solution for 0.1 ~ 0.5 g/mL, ultrasound is to after being uniformly dispersed, electrostatic spray, and wet process is collected, and obtains cigarette graphite
Alkenyl complex microsphere；
The solid-liquid ratio of the glucose solution and mixture is 0.1 ~ 0.5 g/mL.
2. the cigarette according to claim 1 preparation method of graphene-based complex microsphere, which is characterized in that described is natural
Reducing agent is vitamin C, chitosan, gallic acid or L-cysteine.
3. the cigarette according to claim 1 preparation method of graphene-based complex microsphere, which is characterized in that the PBS
The pH of buffer is 7.5 ~ 8.0.
4. the cigarette according to claim 1 preparation method of graphene-based complex microsphere, which is characterized in that in step (3),
Mixing time is 0.5 ~ 3 h.
5. a kind of preparation method of Fruity type cigarette filter tip additive, using cigarette described in claim 1 with graphene-based multiple
Close microballoon, which comprises the steps of:
Cigarette is soaked in graphene-based complex microsphere containing one in isopentyl aldehyde, octanal, aldehyde C-9, capraldehyde, melonal by step (A)
It is adsorbed in kind or several natural essence spice solutions, after saturation to be adsorbed, is taken out, low temperature drying；
Step (B), after spermaceti and lanocerin are mixed according to mass ratio for 1:0.2 ~ 0.3, to whole meltings under reduced pressure
Afterwards, microballoon after step (A) drying is immersed, takes out, stand after 7 ~ 15s, the time is no less than 5 min；
Step (C), plant amylum is added into deionized water, while emulsion adjuvant is added, will be through step after being stirred until homogeneous
(B) microballoon stood is immersed, and is taken out after 3 ~ 6s, is spontaneously dried to get Fruity type cigarette filter tip additive.
6. the preparation method of Fruity type cigarette filter tip additive according to claim 5, which is characterized in that step (A)
In, the temperature of low temperature drying is 2 ~ 6 DEG C.
7. the preparation method of Fruity type cigarette filter tip additive according to claim 5, which is characterized in that step (C)
In, the plant amylum is combination one or more of in pueraria starch, pawpaw starch and acorn starch.
8. the preparation method of Fruity type cigarette filter tip additive according to claim 5, which is characterized in that step (C)
In, the mass ratio of the plant amylum, deionized water and emulsion adjuvant is 1 ~ 3:10 ~ 20:0.07 ~ 0.12；The emulsification
Auxiliary agent is polyethylene glycol 400, sucrose ester, fatty acid esters of sorbitan, glucan, Span-20 or Span-40.
9. the preparation method of Fruity type cigarette filter tip additive described in -8 according to claim 1, which is characterized in that described
The diameter control of cigarette filter tip additive is 1.5 ~ 3.5 mm.
10. the application of Fruity type cigarette filter tip additive described in claim 5-8 any one, which is characterized in that by institute
The cigarette stated is added in filter stick tow with graphene-based complex microsphere.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2776820A1 (en) * | 2009-10-09 | 2011-04-14 | Philip Morris Products S.A. | Tobacco-free pouched product containing flavor beads providing immediate and long lasting flavor release |
| CN103121672A (en) * | 2013-03-20 | 2013-05-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene oxide microsphere and graphene microsphere and preparation methods thereof |
| CN103752236A (en) * | 2014-01-09 | 2014-04-30 | 陕西科技大学 | Preparation method of double-layer wrapped essence micro-capsule |
| CN103801269A (en) * | 2012-11-14 | 2014-05-21 | 江南大学 | Preparation of surface imprinting graphene composite material |
| CN104401969A (en) * | 2015-01-08 | 2015-03-11 | 北京化工大学 | Method for preparing graphene microsphere through normal-pressure drying |
| CN104861934A (en) * | 2015-05-26 | 2015-08-26 | 西南科技大学 | Preparation method of phase change microcapsule with graphene-modified wall material |
| CN104910568A (en) * | 2015-01-28 | 2015-09-16 | 云南中烟工业有限责任公司 | Graphene-polymer composite aerogel filter perfume rod and preparation method thereof |
| CN105126751A (en) * | 2015-06-26 | 2015-12-09 | 中国航空工业集团公司北京航空材料研究院 | Graphene porous material for adsorbing flue gas |
| CN107713008A (en) * | 2017-10-09 | 2018-02-23 | 青岛海之林生物科技开发有限公司 | A kind of the inanimacy cigarette for wrapping up water-soluble essence quick-fried pearl wall material and preparation method |
| CN104098860B (en) * | 2014-07-30 | 2018-04-20 | 四川大学 | The preparation method of Kynoar/poly-dopamine coated graphite alkene nanocomposite |
-
2019
- 2019-04-17 CN CN201910310562.9A patent/CN109892690B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2776820A1 (en) * | 2009-10-09 | 2011-04-14 | Philip Morris Products S.A. | Tobacco-free pouched product containing flavor beads providing immediate and long lasting flavor release |
| CN103801269A (en) * | 2012-11-14 | 2014-05-21 | 江南大学 | Preparation of surface imprinting graphene composite material |
| CN103801269B (en) * | 2012-11-14 | 2015-12-09 | 江南大学 | A kind of preparation of surface imprinted graphene composite material |
| CN103121672A (en) * | 2013-03-20 | 2013-05-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene oxide microsphere and graphene microsphere and preparation methods thereof |
| CN103752236A (en) * | 2014-01-09 | 2014-04-30 | 陕西科技大学 | Preparation method of double-layer wrapped essence micro-capsule |
| CN104098860B (en) * | 2014-07-30 | 2018-04-20 | 四川大学 | The preparation method of Kynoar/poly-dopamine coated graphite alkene nanocomposite |
| CN104401969A (en) * | 2015-01-08 | 2015-03-11 | 北京化工大学 | Method for preparing graphene microsphere through normal-pressure drying |
| CN104910568A (en) * | 2015-01-28 | 2015-09-16 | 云南中烟工业有限责任公司 | Graphene-polymer composite aerogel filter perfume rod and preparation method thereof |
| CN104861934A (en) * | 2015-05-26 | 2015-08-26 | 西南科技大学 | Preparation method of phase change microcapsule with graphene-modified wall material |
| CN105126751A (en) * | 2015-06-26 | 2015-12-09 | 中国航空工业集团公司北京航空材料研究院 | Graphene porous material for adsorbing flue gas |
| CN107713008A (en) * | 2017-10-09 | 2018-02-23 | 青岛海之林生物科技开发有限公司 | A kind of the inanimacy cigarette for wrapping up water-soluble essence quick-fried pearl wall material and preparation method |
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