CN109700070A - A kind of particle and its preparation method and application that can reduce cigarette smoke temperature - Google Patents
A kind of particle and its preparation method and application that can reduce cigarette smoke temperature Download PDFInfo
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Abstract
The invention belongs to cigarette auxiliary materials technical fields, are related to a kind of particle and its preparation method and application that can reduce cigarette mainstream flue gas temperature.The particle is the active particle or non-active particles of non-active particles or outer coating layer.The non-active particles, being cladded with thicknesses of layers is 0-0.2mm, and outer layer film layer accounts for the 0-50% of entire granular mass；The active particle, being cladded with thicknesses of layers is 0.001-0.2mm, and outer layer film layer accounts for the 0.001-50% of entire granular mass.The non-active particles are to be less than 3.0mg/cm to nicotine absorption in flue gas aerosol3Particle；The non-active particles include inorganic particle or organic granular.Preparation method of the present invention simply, easily industrializes and industrialization, and the particle is easy to add in cigarette filter rod, and the particle surface is fine and close, does not leak, this particle is added in cigarette filter rod, the temperature of cigarette smoke can be greatly reduced.
Description
Technical field
The invention belongs to cigarette auxiliary materials technical field, it is related to a kind of particle that can reduce cigarette mainstream flue gas temperature and its system
Preparation Method and application.
Background technique
Cigarette is a kind of special consumer goods, and consumption pattern is that its flue gas is enjoyed by burning and sucking.Cigarette smoke refers to
The height concentration generated of combustion process of the pipe tobacco being ignited in cigarette by complexity and the aerosol system that constantly vary.
There are two types of forms for cigarette burning: one is burnings when suction, are known as burning and sucking；Another kind is the burning of suction gap, referred to as negative
It fires (also known as quiet combustion).
It is known as main flume (Main-stream Smoke, abbreviation MS) from the flue gas that the filter end of cigarette is sucked out when suction,
The flue gas that suction gap releases from fire end and is directly entered environment through cigarette paper diffusion is known as side-stream smoke
(Sidestream Smoke, abbreviation SS).During the smoking process, the heat that cigarette combustion cone generates can be by main flume band
To filter tip, and with cigarette smoking process, gradually risen by the flue-gas temperature of filter tip.The result of study of forefathers shows
Suction is close to when the preceding 2-3 mouthfuls of suctions terminated, and the flue-gas temperature of filter end reaches as high as 70 DEG C~80 DEG C, in depth suction mode
The flue-gas temperature maximum temperature of lower filter end has been even up to 100 DEG C or so.In general, flue-gas temperature is higher to bring flue gas
Stimulation and burning heat sensation reduce cigarette suction comfort.In order to control cigarette smoke temperature, Cigarette design developer is often led to
Lengthening filter stick is crossed, filtering rod is improved, increasing the means such as filter stick degree of ventilation reduces flue-gas temperature.But these technical method meetings
Cause cigarette smoke concentration to reduce, aspirates the problems such as smooth degree is insufficient, therefore there are biggish limitations on.
In recent years, new tobacco products achieves fast development, and buccal cigarette, electronic atomized cigarette, heats the cigarette that do not burn at chewing tobacco
The novel products such as straw-made articles appear widely in the market, and for these products compared with traditional cigarette, harmfulness has significant drop
It is low, therefore the approval of consumer is obtained, and certain market share is occupied on international tobacco market.It wherein heats non-ignitable
Burning tobacco product is in pumped mass and suction traditionally closest to the product of traditional cigarette, and development prospect is good.
Heating do not burn tobacco technology be by glow carbon-point or heating electronic component at 200~400 DEG C of temperature plus
Hot tobacco, makes tobacco not burn, but tobacco component remains to distillation and cracking, to also release flue gas.Relative to tradition
Burning tobacco product, heating do not burn cigarette due to there is no burning, release harmful components have compared with traditional cigarette
Significantly reduce, pumped mass close under conditions of, Product Safety significantly improves.Therefore, this technology has good
Development prospect and market potential.However, heating does not burn cigarette since tobacco material does not burn, release exhaust gas volumn compared with
Traditional cigarette is few, if reducing flue-gas temperature, product exhaust gas volumn meeting using the technological means for increasing filtering and ventilation dilution again
Further decline affects product suction impression.Therefore, reducing flue-gas temperature is to heat a key skill of the cigarette that do not burn
Art.
Chinese patent CN104203015A describes U.S. Philips Philip Morris and is used as heating not using polylactic acid membrane
The cooling material of burning cigarette.The material of above-mentioned reduction flue-gas temperature is mainly the glass transition by polylactic acid, i.e., from glass
Glass state absorbs heat to elastomeric state transformation, and from the flue-gas temperature for reducing smoking article.However problem is that glass occurs for polylactic acid
When glass transistion, it may appear that fusing or bond vitrified phenomenon, therefore the polymer of the cooling most stick end crowd of flue gas is contacted at first
Serious adhesion can occur immediately and collapse for material, block duct, prevent flue gas is from the smooth polymeric inner for flowing through fold, drop
Low cooling surface product, causes flue-gas temperature excessively high.
For the above technical need and prior art defect, the present inventor opens on the basis for summarizing the prior art
Issue a kind of technology for reducing cigarette and new tobacco products flue-gas temperature.
Summary of the invention
It is an object of that present invention to provide a kind of particles and its preparation method and application that can reduce cigarette smoke temperature.In order to
Reach above-mentioned purpose, the technical solution adopted by the present invention is that:
A kind of particle that can reduce cigarette smoke temperature.
Further, the particle is the active particle or non-active particles of non-active particles or outer coating layer.
Optionally, the non-active particles equally can outer coating layer, outer coating layer with a thickness of 0-0.2mm, outer overlay film
Layer accounts for the 0-50% of entire granular mass；Obviously, when the thickness of its outer coating layer or when accounting for entire granular mass and being 0, i.e. table
Show the not outer coating layer of non-active particles；The active particle, needs disactivation to handle, outer coating layer with a thickness of 0.001-
0.2mm accounts for the 0.001-50% of entire granular mass.
Optionally, the non-active particles are to be less than 3.0mg/cm to nicotine absorption in flue gas aerosol3Particle.
Optionally, the non-active particles include inorganic particle or organic granular.
Optionally, the inorganic particle include aluminum oxide, zirconium oxide, carbonic acid calcisphere, bead, silica, iron,
One or more of copper, aluminium, gold, platinum, magnesium silicate ball or calcium sulfate.
Optionally, the organic granular includes cellulose acetate, cellulose acetate propionate, acetylbutyrylcellulose, crystallite
Cellulose, cane sugar powder, dextrin, lactose, Icing Sugar, glucose, mannitol, starch, methylcellulose, ethyl cellulose, polylactic acid,
Polyethylene, polypropylene, poly butyric ester, poly-epsilon-caprolactone, polyglycolic acid, polyhydroxyalkanoates or the thermoplasticity based on starch
One or more of resin.
Optionally, the active particle is to adsorb more than nicotine in flue gas aerosol equal to 3.0mg/cm3Particle.
Optionally, the active particle include molecular sieve, active carbon, diatomite, zeolite, perlite, ceramics, sepiolite,
One or more of bleaching earth, ion exchange resin.
Optionally, the outer coating layer is the material that can be formed a film.
Optionally, the filmogen includes cellulose acetate, cellulose acetate propionate, acetylbutyrylcellulose, hydroxypropyl
Cellulose, hypromellose, methylcellulose, ethyl cellulose, polyvinylpyrrolidone, polyethylene contracting ethyl alcohol diethylamine
Acetate, styrol maleic acid copolymers, styrene-ethylene pyridine copolymer, cellulose acetate-phthalate, O-phthalic
Sour hydroxypropyl methyl cellulose, cellulose acetate/polyethylene glycol, methylcellulose/polyethylene glycol, carboxymethyl cellulose/poly- second
Glycol, hypromellose/polyethylene glycol, ethyl cellulose/polyethylene glycol, acrylic resin/polyethylene glycol or polylactic acid
One or more of.
Optionally, the grain shape includes spherical, spherical, pie, flake, band-like, needle-shaped, multilateral shape, band
Faceted shape is one or more of randomly shaped.
Optionally, the particle at least one dimension have 50 microns, 100 microns, 150 microns, 200 microns or
The average diameter of the upper limit of 250 microns of lower limit to 5000 microns, 2000 microns, 1000 microns, 900 microns or 700 microns.
A kind of preparation method of the above-mentioned particle that can reduce cigarette smoke temperature comprising the steps of:
(1) it carries out activity/inactive powder and binder solution that wet feed is made by mixing；
(2) wet feed that step (1) obtains is squeezed using wet-method extrusion granulating process using rotary extrusion granulator and is cut into directly
The cylinder bar of identical, the smooth densification of diameter, and cylinder bar obtained is subjected to round as a ball molding in spheronizator, it is made just
Beginning wet granular；
(3) by initial wet particle drying, moisture removal is removed, obtains activity/non-active particles.
Optionally, the adhesive in the step (1) includes hypromellose aqueous solution, pregelatinized starch aqueous solution
Or one or more of sodium carboxymethyl cellulose solution.
Optionally, the hypromellose aqueous solution or pregelatinized starch concentration of aqueous solution are 8-12%.
Optionally, the mass ratio of the adhesive in the step (1) and powder is 1.0-1.2 ︰ 1.
Optionally, the rotary extrusion granulator in the step (2) is fed with the speed of 23-25rpm, with 25-30rpm's
Speed squeezes out.
Optionally, the spheronizator in the step (2) works 1-2 minutes at 600-700rpm, then slows down in 450-
It works again under 500rpm 3-4 minutes.
A kind of preparation method of the particle of the above-mentioned outer coating layer that can reduce cigarette smoke temperature comprising the steps of:
(1) it under certain air themperature and atomizing pressure, by fluidized bed coating method, coats and is coated in particle surface
Liquid forms and consolidates composite phase-change coating film layer, obtains incipient wetness particle；
(2) heat drying removes the solvent of incipient wetness particle surface, obtains primary particles；
(3) it sieves, obtains coating particles.
Optionally, the coating solution in the step (1) is in water-soluble coating solution, ethyl alcohol coating solution or acetone coating solution
More than one.
Optionally, the water-soluble coating solution include hypromellose/Aqueous Solutions of Polyethylene Glycol, methylcellulose/
One of Aqueous Solutions of Polyethylene Glycol, carboxymethyl cellulose/Aqueous Solutions of Polyethylene Glycol or acrylic resin/Aqueous Solutions of Polyethylene Glycol
More than；The solvent is water；The molecular weight polyethylene glycol is 1000-20000.
Optionally, the mass concentration of the water-soluble coating solution is 3.5-6.5%；The polyethylene glycol accounts for coating solution quality
Ratio is 20-50%.
Optionally, the ethyl alcohol coating solution includes ethyl cellulose/polyethylene glycol ethanol solution；The solvent is 95% second
Alcohol；The molecular weight polyethylene glycol is 1000-20000.
Optionally, the mass concentration of the ethyl alcohol coating solution is 3.5-6.5%；The polyethylene glycol accounts for coating solution mass ratio
Example is 20%-50%.
Optionally, the acetone coating solution includes cellulose diacetate/polyethylene glycol acetone soln or acetate butyrate fiber
One or more of element/polyethylene glycol acetone soln；The solvent is acetone；The molecular weight polyethylene glycol is 1000-
20000。
Optionally, the mass concentration of the acetone coating solution is 3.5-6.5%；The polyethylene glycol accounts for coating solution mass ratio
Example is 20%-50%.
Optionally, it is 0-50% that the coating film layer in the step (1), which accounts for the percentage of entire granular mass,.
Optionally, the fluidized bed inlet air temperature in the step (1) is 40-60 DEG C；Temperature of charge is 30-45 DEG C；Spray gun
Nozzle diameter is 1.0mm；Atomizing pressure 0.15-0.20MPa；Peristaltic pump flow velocity is 5-15r/min.
A kind of application of the above-mentioned particle that can reduce cigarette mainstream flue gas temperature in cigarette filter rod.
Technical solution of the present invention is further illustrated from another angle below:
The present invention is a kind of particle that can reduce cigarette smoke temperature, which is that non-active particles or active particle are overcoating
Film layer.
Grain shape includes spherical, spherical, pie, thin slice, band-like, needle-shaped, polygon (such as cube), randomly shaped
(such as rubble shape), band facet (such as crystal shape) or any mixing.
Particle can be at least one dimension with 50 microns, 100 microns, 150 microns, 200 microns, 250 microns
Lower limit is to 5000 microns, 2000 microns, 1000 microns, 900 microns, the average diameter of 700 microns of the upper limit.Wherein average diameter
To the upper limit and any subset therein can be covered for any lower limit.
Active particle, which can be, to be suitable for enhancing any material that flue gas flows through it.Refer to energy suitable for enhancing flow of flue gas
It is enough remove, reduce component in flue gas stream or into flue gas stream addO-on therapy any material.In general, active particle is to cigarette
Nicotine is adsorbed more than equal to 3.0mg/cm in gas aerosol3.It is on the contrary then be non-active particles.Active particle is widely used
In tobacco plug field, main function is the harmful substance generated during removing result of combustion of tobacco, such as tar, phenol.Add
Containing less harmful components in the hot cigarette that do not burn, active particle has stronger adsorption capacity to nicotine again, therefore is not suitable for straight
Connect the filter stick for heating the cigarette that do not burn.If active particle, which is used in, heats cigarette field of not burning, surface needs to carry out non-live
Change processing.Disactivation processing includes a variety of methods, such as surface corona processing, plasma modification, flame treatment, chemistry
Modification, radiation modification, photochemical modification, power chemical modification, coupling agent modified etc., one of method are carried out in particle surface
Coating.Such as film coating, spraying, impregnating.
Active particle includes molecular sieve, active carbon, diatomite, zeolite, perlite, ceramics, sepiolite, bleaching earth, ion
One or more of exchanger resin.
Non-active particles include organic or inorganic particle.Inorganic particle include aluminum oxide, zirconium oxide, carbonic acid calcisphere,
Bead, silica, iron, copper, aluminium, gold, platinum, magnesium silicate ball or calcium sulfate.Organic granular includes cellulose acetate, acetic acid third
Acid cellulose, acetylbutyrylcellulose, microcrystalline cellulose, cane sugar powder, dextrin, lactose, Icing Sugar, glucose, mannitol, starch,
Methylcellulose, ethyl cellulose, polylactic acid, polyethylene, polypropylene, poly butyric ester, poly-epsilon-caprolactone, polyglycolic acid,
At least one of polyhydroxyalkanoates, thermoplastic resin based on starch.
Particle outer layer film layer has flue gas cool-down, covers inner layer granule smell and inner layer granule is prevented to adsorb flue gas gas molten
Glue leads to the insufficient effect of exhaust gas volumn.The film layer of outer layer is made by fluidized bed coating.Due to containing filming performance in coating solution
Very good high molecular material, such as include cellulose acetate, cellulose acetate propionate, acetylbutyrylcellulose, hydroxypropylcellulose,
Hypromellose, methylcellulose, ethyl cellulose, polyvinylpyrrolidone, polyethylene contracting ethyl alcohol diethylamine acetate,
Styrol maleic acid copolymers, styrene-ethylene pyridine copolymer, cellulose acetate-phthalate, phthalic acid chamber third
Ylmethyl cellulose, cellulose acetate/polyethylene glycol, methylcellulose/polyethylene glycol, carboxymethyl cellulose/polyethylene glycol, hydroxyl
Third methylcellulose/polyethylene glycol, ethyl cellulose/polyethylene glycol, acrylic resin/one of polyethylene glycol or polylactic acid
More than.In coating process, film clothing repeatedly to form a film, then layer laminated film overlapping, in conjunction with and formed.Film layer has 0.001-0.2 micro-
The thickness of rice has very good compactness, moisture resistance, therefore 0.3-0.5 microns of flue gas aerosols of partial size can be prevented to penetrate into
The internal layer of particle prevents suction-operated of the inner layer material to flue gas aerosol.Also due to the compactness of coating film layer, and can hide
The smell that lid inner layer material distributes brings miscellaneous gas to avoid to flue gas, and influence consumer sucks sense.When flue gas aerosol passes through
Cool down after particle, if film material is phase-change material, increases heat absorption due to phase transformation or than hot melt, cause flue-gas temperature cold
But, the water in aerosol is condensed in particle surface, and due to the compactness of film layer, condensed water is impermeable to inside particle, because
This condensed water for being deposited on particle surface can also adsorb the phenol in aerosol, to improve the rejection of Pyrogentisinic Acid.
A kind of preparation method of the activity that cigarette smoke temperature can be reduced or non-active particles comprising the steps of:
(1) it carries out activity/inactive powder and binder solution that wet feed is made by mixing；
(2) wet feed that step (1) obtains is squeezed using wet-method extrusion granulating process using rotary extrusion granulator and is cut into directly
The cylinder bar of identical, the smooth densification of diameter, and cylinder bar obtained is subjected to round as a ball molding in spheronizator, it is made just
Beginning wet granular；
(3) by initial wet particle drying, moisture removal is removed, obtains activity/non-active particles.
Adhesive in the step (1) includes hypromellose aqueous solution, pregelatinized starch aqueous solution or carboxylic first
One or more of base sodium cellulosate aqueous solution.
The hypromellose aqueous solution or pregelatinized starch concentration of aqueous solution are 8-12%.
The mass ratio of adhesive and powder in the step (1) is 1.0-1.2:1.
Rotary extrusion granulator in the step (2) is fed with the speed of 23-25rpm, is squeezed with the speed of 25-30rpm
Out.
Spheronizator in the step (2) works 1-2 minutes at 600-700rpm, then slows down at 450-500rpm
It works again 3-4 minutes.
A kind of active particle that can reduce cigarette smoke temperature is cladded with the preparation method of membrane-coating granules comprising the steps of:
(1) it under certain air themperature and atomizing pressure, by fluidized bed coating method, is coated on active particle surface
Coating solution forms and consolidates composite phase-change coating film layer, obtains incipient wetness particle；
(2) heat drying removes the solvent of incipient wetness particle surface, obtains primary particles；
(3) it sieves, obtains coating particles.
Coating solution in the step (1) is one of water-soluble coating solution, ethyl alcohol coating solution or acetone coating solution
More than.
The water solubility coating solution includes hypromellose/Aqueous Solutions of Polyethylene Glycol, methylcellulose/polyethylene glycol
One or more of aqueous solution, carboxymethyl cellulose/Aqueous Solutions of Polyethylene Glycol or acrylic resin/Aqueous Solutions of Polyethylene Glycol；Institute
Stating solvent is water；The molecular weight polyethylene glycol is 1000-20000.
The mass concentration of the water solubility coating solution is 3.5-6.5%；The polyethylene glycol accounts for coating solution mass ratio
20-40%.
The ethyl alcohol coating solution includes ethyl cellulose/polyethylene glycol ethanol solution；The solvent is 95% ethyl alcohol；It is described
Molecular weight polyethylene glycol is 1000-20000.
The mass concentration of the ethyl alcohol coating solution is 3.5-6.5%；The polyethylene glycol accounts for coating solution mass ratio
20%-45%.
The acetone coating solution includes cellulose diacetate/polyethylene glycol acetone soln or acetylbutyrylcellulose/poly- second
One or more of glycol acetone soln；The solvent is acetone；The molecular weight polyethylene glycol is 1000-20000.
The mass concentration of the acetone coating solution is 3.5-6.5%；The polyethylene glycol accounts for coating solution mass ratio
20%-50%.
The percentage that coating film layer in the step (1) accounts for entire granular mass is 0-50%.
Fluidized bed inlet air temperature in the step (1) is 40-60 DEG C；Temperature of charge is 30-45 DEG C；Spray tip diameter
For 1.0mm；Atomizing pressure 0.15-0.20MPa；Peristaltic pump flow velocity is 5-15r/min.
A kind of application of the above-mentioned particle that can reduce cigarette mainstream flue gas temperature in cigarette filter rod.
The invention has the following advantages:
(1) the characteristics of simple, easy industrialization and industrialization；
(2) particle made is easy to add in cigarette filter rod；
(3) particle surface is fine and close, does not leak, this particle is added in cigarette filter rod, cigarette smoke can be greatly reduced
Temperature.
Detailed description of the invention
Fig. 1 is that do not burn cigarette products structure and flue-gas temperature test schematic diagram are heated in IQOS control.
11-thermocouples detect position in figure；12-have the filter stick of PLA film；13-heat the tobacco material that do not burn；
14-electric heating body cavitys；15-electrically heated rods；16-ventilation guide holes；17-cell devices；18-smoking set elements.
Fig. 2 is do not burnt using the heating of the present invention cooling particle cigarette products structure and flue-gas temperature test signal
Figure.
21-thermocouples detect position in figure；22-the filter sticks with present invention cooling particle；23-heat the cigarette that do not burn
Grassland material；24-electric heating body cavitys；25-electrically heated rods；26-ventilation guide holes；27-cell devices；28-smoking set elements.
Specific embodiment
The invention will be further described with reference to embodiments.Percentage (%) in following examples, unless separately
It is described, is mass percent.
Embodiment 1
Use wet grinding at average grain diameter for 48 microns of powder industrial cellulose diacetate.Weigh 1 kilogram it is above-mentioned
1.18 kilogram of 7.8% hypromellose (HPMC) aqueous solution is added, in laboratory wet mixing machine in the powdered sample of grinding
On mixing is sufficiently stirred, be made wet feed.By the software wet feed of above-mentioned preparation at E-50 wet-method extrusion machine (distribution grid aperture 1.0mm)
Upper progress wet process squeezes granulation, obtains cylinder bar.The feed revolving speed of extruder is 23rpm, extruded velocity 26rpm.It will
Cylinder bar carries out round as a ball molding on S-250 spheronizator, obtains spherical wet granular.Round as a ball condition are as follows: spheronizator first exists
It works under 600rpm 1.5 minutes, then works at 500 rpm again 3 minutes.By above-mentioned spherical wet granular in 105-120 DEG C of temperature
Lower dry 5-6 hours, remove moisture removal, obtain dry active particle (and as in following table 1 flue-gas temperature test comparison ball
Shape particle).The active particle of drying is coated using fluidized bed bottom spirt row film layer, the dosage of coating solution is controlled, makes coating membrane
Layer accounts for the 13% of last spheric granules quality.After coating, under 60 DEG C of inlet air temperature, dry spheric granules 15 minutes,
Taking out after the drying of spheric granules surface moisture, 14 mesh and 20 meshes (0.83-1.18mm) are crossed, the drop of particle size needed for obtaining
Warm spheric granules.By test, the bulk density of spheric granules is 0.50g/mL.Coating solution concentration used is 5.25%.It is main at
It is divided into hypromellose and Macrogol 6000, solvent is water.It is 23.3% that wherein polyethylene glycol, which accounts for the ratio of principal component,.
Fluidized bed coating operating condition are as follows: inlet air temperature: 60 DEG C, temperature of charge: 37.5-38.5 DEG C, spray tip diameter 1.0mm, mist
Change pressure 0.17MPa, peristaltic pump flow velocity is 10r/min.
The complex technique prepared using cavity filter stick heats original PLA film section in the cigarette filter rod that do not burn in IQOS,
The cooling spheric granules or comparison spheric granules of the above-mentioned preparation of 250mg are added, GB/T19609-2004 is provided according to national standards
Cigarette smoking model carry out simulation smoking, using Canadian depth suction mode (HCI), smoking parameters are as follows: pumping volume
55mL/L, suction frequencies 30s, puff duration 2s.The heater that measurement process uses is IQOS heater.Test process
In, the temperature (referring to attached drawing 2) when electric thermo-couple temperature detector detects cigarette smoking at cigarette filter rod centre distance mouth end 5mm,
The test that the suction and flue-gas temperature for the cigarette (IQOS) that do not burn are heated in control is (see attached drawing 1) consistent with the above.Test result
It is shown in Table 1.
1 main flume temperature test result of table
The test data of table 1 shows the main flume temperature ratio of the cigarette using cooling spheric granules filter stick of the invention
Control cigarette sample temperature is low, and reduce amplitude reduces with being incremented by for puff number, wherein first and second mouthful of suction temperature
It is very big to spend the range of decrease, reaches 15 DEG C or more.Remaining mouthful of number temperature drop is minimum also to reach 4.7 DEG C.Compared with comparing spheric granules,
The cooling effect of its flue gas is also significantly improved, and illustrates that particle has cooling effect to flue gas.
Embodiment 2
1 kilogram of industrial microcrystalline cellulose (production of Anhui mountains and rivers company, 45 microns of powder average particle size) is weighed, is added 1.22
Kilogram 9.1% pregelatinized starch aqueous solution, is sufficiently stirred mixing on laboratory wet mixing machine, and wet feed is made.By above-mentioned system
Standby software wet feed carries out wet process on E-50 wet-method extrusion machine (distribution grid aperture 1.0mm) and squeezes granulation, obtains cylinder strip
Object.The feed revolving speed of extruder is 24rpm, extruded velocity 27rpm.Cylinder bar is rolled on S-250 spheronizator
Circle molding, obtains spherical wet granular.Round as a ball condition are as follows: spheronizator first works 2 minutes at 650rpm, then again at 450 rpm
Work 3 minutes.Spherical wet granular obtained above is 5-6 hours dry at a temperature of 105-120 DEG C, moisture removal is removed, is done
Dry active particle.The real ball of internal layer rigidity of drying is coated using fluidized bed bottom spirt row film layer, controls the dosage of coating solution,
Coating film layer is set to account for the 13% of last spheric granules quality.After coating, under 60 DEG C of inlet air temperature, dry spheric granules
15 minutes, spheric granules surface moisture is dried.It takes out, crosses 18 mesh and 24 meshes (0.7-0.88mm), partial size needed for obtaining is big
Small cooling spheric granules.Bulk density by testing spheric granules is 0.86g/mL.Coating solution concentration is 5.25%.It is main at
It is divided into hypromellose and Macrogol 6000, solvent is water.It is 23.3% that wherein polyethylene glycol, which accounts for the ratio of principal component,.
Fluidized bed coating operating condition are as follows: inlet air temperature: 60 DEG C, temperature of charge: 37.5-38.5 DEG C, spray tip diameter 1.0mm, mist
Change pressure 0.17MPa, peristaltic pump flow velocity is 10r/min.
The complex technique prepared using cavity filter stick heats original PLA film section in the cigarette filter rod that do not burn in IQOS,
The cooling spheric granules for adding the above-mentioned preparation of 400mg, according to country than cigarette smoking mould as defined in standard GB/T19609-2004
Type carries out simulation smoking, using Canadian depth suction mode (HCI), smoking parameters are as follows: pumping volume 55mL/L, suction frequency
Rate 30s, puff duration 2s.The heater that measurement process uses is IQOS heater.Electric thermo-couple temperature is examined in test process
The volume that do not burn is heated in temperature (referring to attached drawing 2) when surveying device detection cigarette smoking at cigarette filter rod centre distance mouth end 5mm, control
The suction of cigarette (IQOS) and the test of flue-gas temperature are (see attached drawing 1) consistent with the above.Test result is shown in Table 2.
2 main flume temperature test result of table
The test data of table 2 shows the main flume temperature ratio of the cigarette using cooling spheric granules filter stick of the invention
Control cigarette sample temperature is low, and reduce amplitude reduces with being incremented by for puff number, wherein first and second mouthful of suction temperature
It is very big to spend the range of decrease, reaches 18.6 DEG C or more.Remaining mouthful of number temperature drop is minimum also to reach 6.3 DEG C.
Embodiment 3
1 kilogram of industrial microcrystalline cellulose powder sample (production of Anhui mountains and rivers company, 45 microns of powder average particle size) is weighed,
1.22 kilogram of 9.1% pregelatinized starch aqueous solution is added, mixing is sufficiently stirred on laboratory wet mixing machine, wet feed is made.
The software wet feed of above-mentioned preparation is carried out to wet process on E-50 wet-method extrusion machine (distribution grid aperture 1.0mm) and squeezes granulation, is obtained
Cylinder bar.The feed revolving speed of extruder is 24rpm, extruded velocity 27rpm.By cylinder bar in S-250 spheronizator
It is upper to carry out round as a ball molding, obtain spherical wet granular.Round as a ball condition are as follows: spheronizator first works 2 minutes at 650rpm, then exists again
It works under 450rpm 3 minutes.Spherical wet granular obtained above is 5-6 hours dry at a temperature of 105-120 DEG C, it goes to remove water
Point, obtain dry active particle.The active particle of drying is subjected to film layer coating using bottom spray fluidized bed, controls coating solution
Dosage makes coating film layer account for the 9% of last spheric granules quality.It is dry spherical under 50 DEG C of inlet air temperature after coating
Particle 15 minutes, spheric granules surface moisture is dried.It takes out, crosses 18 mesh and 24 meshes (0.7-0.88mm), grain needed for obtaining
The cooling spheric granules of diameter size, spheric granules bulk density are 0.88g/mL.Coating solution concentration is 5.25%.Principal component is hydroxyl
Third methylcellulose and polyethylene glycol 1500, solvent are water.It is 23.3% that wherein polyethylene glycol, which accounts for the ratio of principal component,.Fluidized bed
Coating operations condition are as follows: inlet air temperature: 50 DEG C, temperature of charge: 37.5-38.5 DEG C, spray tip diameter 1.0mm, atomizing pressure
0.15MPa, peristaltic pump flow velocity are 10r/min.
The complex technique prepared using cavity filter stick is not burnt original PLA film in cigarette filter rod (IQOS) in heating
Section adds the cooling spheric granules of the above-mentioned preparation of 400mg, according to country than cigarette smoking as defined in standard GB/T19609-2004
Model carries out simulation smoking, using Canadian depth suction mode (HCI), smoking parameters are as follows: pumping volume 55mL/L, suction
Frequency 30s, puff duration 2s.The heater that measurement process uses is IQOS heater.Electric thermo-couple temperature in test process
Temperature (referring to attached drawing 2) when detector detects cigarette smoking at cigarette filter rod centre distance mouth end 5mm, control heating are not burnt
The suction of cigarette (IQOS) and the test of flue-gas temperature are (see attached drawing 1) consistent with the above.Test result is shown in Table 3.
3 main flume temperature test result of table
The test data of table 3 shows the main flume temperature ratio of the cigarette using cooling spheric granules filter stick of the invention
Control cigarette sample temperature is low, and reduce amplitude reduces with being incremented by for puff number, wherein first and second mouthful of suction temperature
It is very big to spend the range of decrease, reaches 29.1 DEG C or more.Remaining mouthful of number temperature drop is minimum also to reach 5.9 DEG C.
Embodiment 4
Use wet grinding at average grain diameter for 48 microns of powder industrial cellulose diacetate.Weigh 1 kilogram it is above-mentioned
1.18 kilogram of 7.8% hypromellose (HPMC) aqueous solution is added, in laboratory wet mixing machine in the powdered sample of grinding
On mixing is sufficiently stirred, be made wet feed.By the software wet feed of above-mentioned preparation at E-50 wet-method extrusion machine (distribution grid aperture 1.0mm)
Upper progress wet process squeezes granulation, obtains cylinder bar.The feed revolving speed of extruder is 23rpm, extruded velocity 26rpm.It will
Cylinder bar carries out round as a ball molding on S-250 spheronizator, obtains spherical wet granular.Round as a ball condition are as follows: spheronizator first exists
It works under 600rpm 1.5 minutes, then works at 500 rpm again 3 minutes.By spherical wet granular obtained above in 105-120
It is 5-6 hours dry at a temperature of DEG C, moisture removal is removed, dry active particle is obtained.The active particle of drying is used into bottom jet flow
Bed carries out film layer coating, controls the dosage of coating solution, coating film layer is made to account for the 13% of last spheric granules quality.Coating finishes
Afterwards, under 40 DEG C of inlet air temperature, dry spheric granules 15 minutes, spheric granules surface moisture is dried.Take out, cross 14 mesh and
20 meshes (0.83-1.18mm), the cooling spheric granules of particle size needed for obtaining, spheric granules bulk density are 0.52g/
mL.Coating solution concentration is 5.0%.Principal component is cellulose diacetate and Macrogol 6000, and solvent is acetone.Wherein poly- second two
The ratio that alcohol accounts for principal component is 30%.Fluidized bed operating condition are as follows: inlet air temperature: 40 DEG C, temperature of charge: 32.5 DEG C, spray gun spray
Outspoken diameter 1.0mm, atomizing pressure 0.17MPa, peristaltic pump flow velocity are 10r/min.
The complex technique prepared using cavity filter stick, heating, original PLA in cigarette (IQOS) filter stick that do not burn is thin
Film section is added the cooling spheric granules of the above-mentioned preparation of 250mg, is taken out according to country than cigarette as defined in standard GB/T19609-2004
It inhales model and carries out simulation smoking, using Canadian depth suction mode (HCI), smoking parameters are as follows: pumping volume 55mL/L takes out
Inhale frequency 30s, puff duration 2s.The heater that measurement process uses is IQOS heater.Thermocouple temperature in test process
Temperature (referring to attached drawing 2) when spending detector detection cigarette smoking at cigarette filter rod centre distance mouth end 5mm, control heating are non-ignitable
The test for burning the suction and flue-gas temperature of cigarette (IQOS) is (see attached drawing 1) consistent with the above.Test result is shown in Table 4.
4 main flume temperature test result of table
The test data of table 4 shows the main flume temperature ratio of the cigarette using cooling spheric granules filter stick of the invention
Control cigarette sample temperature is low, and reduce amplitude reduces with being incremented by for puff number, wherein first and second mouthful of suction temperature
It is very big to spend the range of decrease, reaches 14.2 DEG C or more.Remaining mouthful of number temperature drop is minimum also to reach 4.9 DEG C.
Embodiment 5
The complex technique prepared using cavity filter stick heats original PLA film in the cigarette filter rod that do not burn in IQOS
Section, add the spheric granules of different preparation methods, according to national standards cigarette smoking model as defined in GB/T19609-2004 into
Row simulation smoking, using Canadian depth suction mode (HCI).Classification substance is intercepted using cambridge filter, passes through HPLC- fluorescence
Carry out the quantitative test of Pyrogentisinic Acid.Influence of the spheric granules coating film layer to total mainstream aerosol phenol content has been investigated, and
Compared with generating product containing the reference aerosol for gathering PLA cooling unit and being studied.It the results are shown in Table 5.It tests and ties from table 5
Fruit is, it is evident that the spheric granules with coating film layer, Pyrogentisinic Acid have higher filter efficiency.
Influence of 5 coating film layer of table to phenol content in main flume
This hair can be understood and applied the above description of the embodiments is intended to facilitate those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to implementations here
Example, those skilled in the art's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be
Within protection scope of the present invention.
Claims (30)
1. a kind of particle that can reduce cigarette smoke temperature.
2. the particle according to claim 1 that cigarette smoke temperature can be reduced, it is characterised in that: the particle is nonactive
The active particle or non-active particles of particle or outer coating layer.
3. the particle according to claim 2 that cigarette smoke temperature can be reduced, it is characterised in that: the non-active particles,
Its overcoating thicknesses of layers is 0-0.2mm, and outer layer film layer accounts for the 0-50% of entire granular mass；The active particle, outer overlay film
For layer with a thickness of 0.001-0.2mm, outer layer film layer accounts for the 0.001-50% of entire granular mass.
4. the particle according to claim 2 that cigarette smoke temperature can be reduced, it is characterised in that: the non-active particles are
3.0mg/cm is less than to nicotine absorption in flue gas aerosol3Particle.
5. the particle according to claim 2 that cigarette smoke temperature can be reduced, it is characterised in that: the non-active particles packet
Include inorganic particle or organic granular.
6. the particle according to claim 5 that cigarette smoke temperature can be reduced, it is characterised in that: the inorganic particle includes
In aluminum oxide, zirconium oxide, carbonic acid calcisphere, bead, silica, iron, copper, aluminium, gold, platinum, magnesium silicate ball or calcium sulfate
More than one.
7. the particle according to claim 5 that cigarette smoke temperature can be reduced, it is characterised in that: the organic granular includes
Cellulose acetate, cellulose acetate propionate, acetylbutyrylcellulose, microcrystalline cellulose, cane sugar powder, dextrin, lactose, Icing Sugar, Portugal
Grape sugar, mannitol, starch, methylcellulose, ethyl cellulose, polylactic acid, polyethylene, polypropylene, poly butyric ester, poly- ε-
One or more of caprolactone, polyglycolic acid, polyhydroxyalkanoates or thermoplastic resin based on starch.
8. the particle according to claim 2 that cigarette smoke temperature can be reduced, it is characterised in that: the active particle is pair
Nicotine is adsorbed more than equal to 3.0mg/cm in flue gas aerosol3Particle.
9. the particle according to claim 2 that cigarette smoke temperature can be reduced, it is characterised in that: the active particle includes
One or more of molecular sieve, active carbon, diatomite, zeolite, perlite, ceramics, sepiolite, bleaching earth, ion exchange resin.
10. the particle according to claim 2 that cigarette smoke temperature can be reduced, it is characterised in that: the outer coating layer is
The material that can be formed a film.
11. the particle according to claim 10 that cigarette smoke temperature can be reduced, it is characterised in that: the filmogen packet
Include cellulose acetate, cellulose acetate propionate, acetylbutyrylcellulose, hydroxypropylcellulose, hypromellose, Methyl cellulose
Element, ethyl cellulose, polyvinylpyrrolidone, polyethylene contracting ethyl alcohol diethylamine acetate, styrol maleic acid copolymers, benzene second
Alkene-vinylpyridine copolymer, cellulose acetate-phthalate, Hydroxypropyl Methylcellulose Phathalate, cellulose acetate/
Polyethylene glycol, methylcellulose/polyethylene glycol, carboxymethyl cellulose/polyethylene glycol, hypromellose/polyethylene glycol, second
Base cellulose/polyethylene glycol, acrylic resin/one or more of polyethylene glycol or polylactic acid.
12. the particle according to claim 1 that cigarette smoke temperature can be reduced, it is characterised in that: the grain shape packet
Include spherical, spherical, pie, flake, band-like, needle-shaped, multilateral shape, band faceted shape or it is one of randomly shaped with
On.
13. the particle according to claim 1 that cigarette smoke temperature can be reduced, it is characterised in that: the particle is at least
In one dimension with 50 microns, 100 microns, 150 microns, 200 microns or 250 microns lower limit to 5000 microns, it is 2000 micro-
Rice, 1000 microns, the average diameter of the upper limits of 900 microns or 700 microns.
14. the preparation method of any particle that can reduce cigarette smoke temperature, feature in a kind of claim 1-13
It is to comprise the steps of:
(1) it carries out activity/inactive powder and binder solution that wet feed is made by mixing；
(2) wet feed that step (1) obtains is squeezed using wet-method extrusion granulating process using rotary extrusion granulator and is cut into diameter phase
The cylinder bar of same, smooth densification, and cylinder bar obtained is subjected to round as a ball molding in spheronizator, initial wet is made
Particle；
(3) by initial wet particle drying, moisture removal is removed, obtains activity/non-active particles.
15. preparation method according to claim 14, it is characterised in that: the adhesive in the step (1) includes hydroxypropyl
One or more of methylated cellulose aqueous solution, pregelatinized starch aqueous solution or sodium carboxymethylcellulose.
16. preparation method according to claim 15, it is characterised in that: the hypromellose aqueous solution or pre- glue
Change amidin concentration is 8-12%.
17. preparation method according to claim 14, it is characterised in that: adhesive and powder in the step (1)
Mass ratio is 1.0-1.2 ︰ 1.
18. preparation method according to claim 14, it is characterised in that: the rotary extrusion granulator in the step (2)
It is fed with the speed of 23-25rpm, is squeezed out with the speed of 25-30rpm.
19. preparation method according to claim 14, it is characterised in that: the spheronizator in the step (2) is in 600-
It works under 700rpm 1-2 minutes, then slows down and work again at 450-500rpm 3-4 minutes.
20. the preparation side of the particle of any outer coating layer that can reduce cigarette smoke temperature in a kind of claim 1-13
Method, it is characterised in that comprise the steps of:
(1) by fluidized bed coating method, coating solution is coated in particle surface, is formed and consolidates composite phase-change coating film layer, obtained
Incipient wetness particle；
(2) heat drying removes the solvent of incipient wetness particle surface, obtains primary particles；
(3) it sieves, obtains coating particles.
21. preparation method according to claim 20, it is characterised in that: the coating solution in the step (1) is water-soluble
One or more of property coating solution, ethyl alcohol coating solution or acetone coating solution.
22. preparation method according to claim 21, it is characterised in that: the water solubility coating solution includes hydroxypropyl fibre
Tie up element/Aqueous Solutions of Polyethylene Glycol, methylcellulose/Aqueous Solutions of Polyethylene Glycol, carboxymethyl cellulose/Aqueous Solutions of Polyethylene Glycol or third
One or more of olefin(e) acid resin/Aqueous Solutions of Polyethylene Glycol；The solvent is water；The molecular weight polyethylene glycol is 1000-
20000。
23. preparation method according to claim 22, it is characterised in that: it is described water solubility coating solution mass concentration be
3.5-6.5%；It is 20-50% that the polyethylene glycol, which accounts for coating solution mass ratio,.
24. preparation method according to claim 21, it is characterised in that: the ethyl alcohol coating solution include ethyl cellulose/
Polyethylene glycol ethanol solution；The solvent is 95% ethyl alcohol；The molecular weight polyethylene glycol is 1000-20000.
25. preparation method according to claim 24, it is characterised in that: the mass concentration of the ethyl alcohol coating solution is 3.5-
6.5%；It is 20%-50% that the polyethylene glycol, which accounts for coating solution mass ratio,.
26. preparation method according to claim 21, it is characterised in that: the acetone coating solution includes diacetate fiber
One or more of element/polyethylene glycol acetone soln or acetylbutyrylcellulose/polyethylene glycol acetone soln；The solvent is third
Ketone；The molecular weight polyethylene glycol is 1000-20000.
27. preparation method according to claim 26, it is characterised in that: the mass concentration of the acetone coating solution is 3.5-
6.5%；It is 20%-50% that the polyethylene glycol, which accounts for coating solution mass ratio,.
28. preparation method according to claim 20, it is characterised in that: the coating film layer in the step (1) accounts for entirely
The percentage of granular mass is 0-50%.
29. preparation method according to claim 20, it is characterised in that: the fluidized bed inlet air temperature in the step (1)
It is 40-60 DEG C；Temperature of charge is 30-45 DEG C；Spray tip diameter is 1.0mm；Atomizing pressure 0.15-0.20MPa；Peristaltic pump
Flow velocity is 5-15r/min.
30. any particle that can reduce cigarette mainstream flue gas temperature is in cigarette filter rod in a kind of claim 1-13
Using.
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| CN201910157268.9A CN109700070B (en) | 2019-03-01 | 2019-03-01 | Particle capable of reducing cigarette smoke temperature and preparation method and application thereof |
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