KR101731319B1 - Composition of tow for cigarette filter, Tow for cigarette filter and Manufacturing method thereof - Google Patents

Abstract

The present invention relates to a fiber bundle composition for a tobacco filter tow, comprising a fiber bundle composition for tobacco filter tow having an optimum composition and composition ratio capable of greatly improving the adsorption performance of tobacco smoke in a tobacco filter tow, The present invention relates to a tobacco filter tow and a method of manufacturing the same.

Description

TECHNICAL FIELD The present invention relates to a fiber bundle composition for a cigarette filter tow, a tow for a cigarette filter, and a method for manufacturing the filter cigarette filter.

The present invention relates to a fiber bundle composition for a tobacco filter tow, which comprises a fiber bundle composition for a tobacco filter tow having an optimum composition and composition ratio capable of greatly improving the adsorption performance of tobacco smoke of a tobacco filter tow, A tobacco filter tow and a method for manufacturing the same.

Tobacco smoke, as well as tar and nicotine, contains about 4,000 harmful ingredients. 40 of them are known to be carcinogens that cause cancer, and recently, they have been reported to contain dioxin substances known as highly toxic environmental hormones. The various illnesses and death rates caused by the smoking of these cigarette smoke are increasing year by year, and the damage is reaching serious level.

Accordingly, in order to reduce the amount of harmful components in the cigarette smoke inhaled into the human body, efforts have been made to develop various filters to remove toxic substances such as tar and nicotine as much as possible

Cellulosic fiber bundles are mainly used in tobacco filters. First, a cellulose fiber bundle is prepared by extruding a raw liquid obtained by dissolving cellulose, which is a raw material polymer, in acetone, which is a solvent, with a gear pump and discharging it from a nozzle into a radiation cylinder in a heating atmosphere to quickly pulverize the solvent to form a raw fiber bundle. In this case, the short fibers discharged from one discharge hole are combined with the other short fibers so that the single fiber fineness is 0.8 to 10 dtex and the total number is 100 to 1,500 It becomes a raw fiber bundle.

Next, the raw fiber bundles are supplied with an emulsion oil, and become a raw fiber bundle having an oil fraction of about 1 mass% and a water content of about 25 mass%. The number of the raw fiber bundles is 5 to 40, and the total fiber fineness is 10,000 to 50,000 dtex. The fiber tow is crimped in a crimper and then guided to a drying process for removing moisture and solvent. Here, from the application of the emulsion oil to the drying step, it is also carried out in a short time not exceeding one second.

Thereafter, water and solvent are removed from the fibrous tow through water in the drying process until the desired moisture content is obtained, and a bundle of cellulose fibers is obtained. The obtained cellulose fiber bundle is induced in the packing process and is introduced until the packing container is filled for several hours.

In the above-described manufacturing process, the time required from ejection to crimping is less than 2 seconds. In addition, the drying time is generally less than 10 minutes in consideration of the production efficiency, even in a drying process requiring a long time before the packaging process. In the production of a cellulose fiber bundle which is continuously subjected to each step, the solvent such as acetone is present at a rate of 200 to 300 mass% (large solid content) until the moment of discharge from the nozzle, (Acetate fiber bundles) of less than 0.10% by mass was not easy.

Japanese Unexamined Patent Application Publication No. 1-318001 discloses a method for removing a residual polysaccharide from a residual polysaccharide by treating a solid polysaccharide with humidified air to reduce the residual water affinity organic solvent, This method is difficult to apply to a production line producing cellulosic fiber bundles of several hundreds of thousands of meters in length without cutting, and by emulsifying the emulsified oil, a high moisture content raw fiber bundle is moistened There is a problem that it is difficult to further increase the water content by treating with air.

Japanese Patent Application Laid-Open No. 2006-144176 discloses a method of increasing the water content of a fiber tow by adding emulsion oil to a fiber tow obtained by bundling a plurality of raw fiber bundles in a method of producing a cellulose fiber bundle. There is a problem that it is difficult to stably obtain a bundle of cellulose fibers having a low content of solvent because the conditions are not limited.

Korean public patent 2009-0091926 (public date April 8, 2010)

The present invention for solving the above problems is to provide a method for producing a tobacco filter tow by using a specific thermoplastic cellulose ester capable of melt spinning Resin and a specific composition in an optimal composition ratio, and to provide a tobacco filter tow using the same and a method for producing the same.

The present invention relates to a fiber bundle composition for tobacco filter tow comprising a thermoplastic cellulose ester resin, a plasticizer, a radical formation inhibitor and a radical activity inhibitor.

In one preferred embodiment of the present invention, the fiber bundle composition for a tobacco filter tow comprises 15 to 45 parts by weight of the plasticizer, 0.01 to 2 parts by weight of the radical generation inhibitor and 100 parts by weight of the thermoplastic resin composition, 0.01 to 2.5 parts by weight of a radical activity inhibitor.

As a preferred embodiment of the present invention, in the fiber bundle composition for tobacco filter tow of the present invention, the thermoplastic cellulose ester resin has a degree of substitution of cellulose hydroxyl groups of 1.8 to 3.0 and a weight average molecular weight of 30,000 to 60,000 can do.

In a preferred embodiment of the present invention, the thermoplastic cellulose ester resin is selected from the group consisting of cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, cellulose acetate phthalate, cellulose acetate caproate, cellulose acetate caprylate, cellulose acetate laurethate, cellulose Acetate palmitate, cellulose acetate stearate, and cellulose acetate oleate.

As a preferred embodiment of the present invention, in the fiber bundle composition for a tobacco filter tow of the present invention, the plasticizer is selected from polyethylene glycol, polypropylene glycol, polyglycolic acid, polybutyl adipate, glycerin, tri Butyl sebacate, triacetin, and triethyl citrate. ≪ Desc / Clms Page number 7 >

As a preferred embodiment of the present invention, in the fiber bundle composition for a tobacco filter tow of the present invention, the radical generation inhibitor may include a water insoluble compound including a phenol group.

In one preferred embodiment of the present invention, the radical generation inhibitor is tetrakis (methylene) (3,5-di-t-butyl-4-hydroxycinnamate) methane, pentaerythritol tetrakis (3,5-di-t-butyl-4-hydroxyphenyl) propionate methane, . ≪ / RTI >

As a preferred embodiment of the present invention, in the fiber bundle composition for a tobacco filter tow of the present invention, the radical activity inhibitor may include a water-insoluble compound containing phosphorus at the terminal.

In a preferred embodiment of the present invention, the radical activity inhibitor includes at least one selected from tris (2,4-di-t-butylphenyl) phosphite, tris-nonylphenyl phosphite and triphenyl phosphite .

Another object of the present invention is a tobacco filter tow using the fiber bundle composition for tobacco filter tow described above, wherein the tobacco filter tow of the present invention comprises a bundle of molten cellulose ester fibers formed from the fiber bundle composition .

In a preferred embodiment of the present invention, the tobacco filter tow of the present invention comprises a bundle of molten cellulose ester fibers in a number of crimps of 20 to 30 fibers / inch.

As a preferred embodiment of the present invention, in the tobacco filter tow of the present invention, the fiber bundle is formed by melt-spun cellulose ester fibers having a fineness of 0.8 to 10.0 deniers of short fibers and having a fineness of 25,000 to 45,000 denier And the like.

According to a preferred embodiment of the present invention, the tobacco filter tow of the present invention may have an aspiration resistance of 50% to 65% of tar and 40% to 50% of nicotine when measured according to the KS H ISO 6565 method .

Another object of the present invention is to provide a method for producing a tobacco filter tow using the fiber bundle composition for tobacco filter tow described above, comprising: mixing a tobacco filter tow composition to prepare a mixed resin; Adding the mixed resin to a kneader and blending the kneaded mixture under a condition of raising the internal temperature of the kneader from 150 ° C to 220 ° C to produce a molten cellulose ester chip; Drying the molten cellulose ester chip at 70 ° C to 90 ° C for 20 to 30 hours; Melting and spinning the dried molten cellulose ester chips through a spinneret to produce a molten cellulose ester fiber bundle; And a step of crimping the molten cellulose ester fiber bundle to produce a tow, thereby manufacturing the tobacco filter tow.

As a preferred embodiment of the present invention, in the production method of the present invention, the kneader is a kneader equipped with a twin-screw extruder, and the blending is performed at 20 to 30 kg / hr of a circle feeder and at a kneader motor speed of 220 to 300 rpm And the like.

As a preferred embodiment of the present invention, in the production method of the present invention, the melt spinning may be performed at a spinning speed of 2,000 mpm to 3,000 mpm and a spinning temperature of 250 to 290 ° C.

According to a preferred embodiment of the present invention, in the method of the present invention, the detachment is a deformed section detachment, and the deformed section detachment comprises a cross section section section, a polygonal section section section, a C section section section, a circular section section section, , A cross-section of the fleshy leaf, or a cross-section of the fleshy leaf.

As a preferred embodiment of the present invention, in the production method of the present invention, the melt-cellulose ester resin has a melting temperature of 160 ° C to 230 ° C, a load of 2.16 kg according to the ASTM D1238 method, A heat flow rate of 3 to 10 g / 10 min, a shear rate of 9 to 20 / s, and a melt viscosity of 1,150 to 1,700 Pa.sec (230 DEG C).

As a preferred embodiment of the present invention, in the manufacturing method of the present invention, the molten cellulose ester fiber bundle may be obtained by extruding molten cellulose ester fiber having a fineness of 0.8 to 10.0 denier of a short fiber with a fineness of 25,000 to 45,000 denier, And the like.

As a preferred embodiment of the present invention, in the production method of the present invention, the crimp may be characterized by crimping the melt-cellulose ester fiber bundle at 20 to 30 crimps / inch.

The present invention also relates to a cigarette filter including a tow for a cigarette filter manufactured by the above-described manufacturing method.

The fiber bundle composition of the tobacco filter tow of the present invention is capable of melt-spinning unlike the conventional method, and it has an advantage in that the productivity can be increased through high-speed spinning and various additives can be added according to user's needs. A fiber bundle having various modified cross-sections can be produced through the sectioning, and the tobacco filter tow having excellent adsorption performance can be provided.

Hereinafter, the present invention will be described in detail.

The tobacco filter tow fiber bundle composition of the present invention comprises a thermoplastic cellulose ester resin, a plasticizer, a radical formation inhibitor and a radical activity inhibitor.

The composition comprises a cellulose ester resin and is a cellulose derivative in which a part or all of the hydroxyl groups of the cellulose are substituted by ester bonds, so that the strong hydrogen bonds of the cellulose hydroxyl are weakened so that the plasticizer can be mixed well therebetween. Further, as the plasticizer is mixed effectively, strong hydrogen bonding due to the hydroxyl group of the cellulose may be interfered and melt spinning may be possible.

In the present invention, the cellulose ester resin is preferably selected from the group consisting of cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, cellulose acetate phthalate, cellulose acetate caprate, cellulose acetate caprylate, cellulose acetate laurethate, Cellulose acetate stearate or cellulose acetate oleate, or the like. The cellulose ester resin of the present invention may have a weight average molecular weight of 30,000 to 60,000 and a degree of substitution of 1.8 to 3.0, preferably a weight average molecular weight of 35,000 to 47,000 and a degree of substitution of 2.0 to 2.8, More preferably a weight average molecular weight of 37,000 to 45,000 and a degree of substitution of 2.2 to 2.6. When the degree of substitution of the cellulose ester resin is less than 1.8, the fluidity of the molecules may be lowered when the cellulose ester resin is melted and the processability may be deteriorated. When the degree of substitution of the cellulose ester resin is less than 1.8, the degree of substitution of the cellulose ester resin may be decreased. Further substitution with a limiting substitution of a cellulose derivative is not feasible.

In addition, the fiber bundle composition for tobacco filter tow of the present invention may contain a plasticizer in addition to the above-mentioned cellulose ester resin. The plasticizer is not particularly limited as long as it is mixed with the cellulose ester to prevent strong hydrogen bonding due to the hydroxyl groups present in the cellulose ester and to allow melt spinning. More preferably, the plasticizer has a low molecular weight of 1,000 or less Can be used.

Examples of the plasticizer include phthalic acid esters such as dimethyl phthalate, diethyl phthalate, dihexyl phthalate, dioctyl phthalate, dimethoxyethyl phthalate, ethyl phthalyl ethyl glycolate and butyl phthalyl butyl glycolate; Aromatic polycarboxylic acid esters such as tetraoctyl pyromellitate and trioctyl trimellitate; Aromatic polycarboxylic acid esters such as dibutyl adipate, dioctyl adipate, dibutyl sebacate, dioctyl sebacate, diethyl azelate, dibutyl azelate and dioctyl azelate; Lower fatty acid esters of polyhydric alcohols such as glycerin triacetate, diglycerin tetraacetate and polyglycolic acid; Phosphoric acid esters such as triethyl phosphate, tributyl phosphate, tributoxyethyl phosphate and tricresyl phosphate; Aliphatic polyesters composed of glycols and dibasic acids such as polyethylene glycol, polypropylene glycol, polyethylene adipate, polybutylene adipate, polyethylene succinate, and polybutylene succinate; Aliphatic polyesters composed of oxycarboxylic acids such as polyglycolic acid; Aliphatic polyesters composed of lactones such as polycaprolactone, polypropiolactone, and polar valerolactone; Vinyl polymers such as polyvinylpyrrolidone; Tributyl sebacate; Triacetin; And triethyl citrate; , And the like. More preferably, at least one selected from polyethylene glycol, polypropylene glycol, polyglycolic acid, polybutyl adipate, glycerin, tributyl sebacate, triacetin and triethyl citrate having a weight average molecular weight of 1,000 or less can be used have.

The amount of the plasticizer to be used is preferably 15 to 45 parts by weight, preferably 25 to 40 parts by weight, more preferably 25 to 35 parts by weight, based on 100 parts by weight of the cellulose ester, Thermosetting of the cellulose ester may not be sufficiently carried out and thermal processing may not be possible. If it is used in excess of 45 parts by weight, there may be a problem of fuming during melt spinning, and mechanical properties of the fiber bundle may be deteriorated due to excessive plasticization , There may be a problem that breed-out of the plasticizer occurs on the surface of the fiber bundle melt-spun.

In addition, the fiber bundle composition for a tobacco filter tow of the present invention comprises a radical generation inhibitor and a radical activity inhibitor, wherein the radical generation inhibitor is a compound which, when thermoplasticizing the cellulose ester resin or pre-spinning the plasticized cellulose ester resin, It prevents the decomposition by heat, and inhibits the radical generation which is generated in the chain tip, so that it is possible to spin at high temperature, and it is possible to provide a bundle of molten spinning fibers having excellent physical properties. The radical generation inhibitor may be in the form of a liquid or solid phase easily mixed with a cellulose ester resin and a plasticizer, preferably a water-insoluble compound containing a phenol group, more preferably tetrakis methylene (3, (3,5-di-t-butyl-4-hydroxycinnamate) methane, pentaerythritol tetrakis (3- Di-t-butyl-4-hydroxyphenyl) propionate methane. Specific examples thereof include Anox 20 (Chemtura Co.), Iganox 1010 (Ciba Specialty Chemicals, Inc. and Songnox 1010 (Songwon International Co., Ltd.).

The radical generation inhibitor may be used in an amount of 0.01 to 2 parts by weight, preferably 0.05 to 0.8 part by weight, based on 100 parts by weight of the cellulose ester resin. If the amount is less than 0.01 part by weight, The ester resin is insufficient in the ability to prevent thermal decomposition and the cellulose ester resin may be thermally decomposed in the course of thermoplasticization or spinning. If the amount exceeds 2 parts by weight, there may be a problem in workability as a cause of an increase in pack pressure.

By using not only the radical generation inhibitor but also a radical activity inhibitor, the present invention can provide a molten radiator having a low defective rate and excellent physical properties. In the present invention, the radical formation inhibitor plays a role in preventing oxidation of the melt-spun fiber bundle in the atmosphere and inhibits the radical generation generated by breaking of the cellulose main chain. The radical activity inhibitor may be in the form of a liquid or solid phase which is easily mixed with a cellulose ester resin and a plasticizer, and preferably a water-insoluble compound containing an elemental phosphorus at the terminal may be used. More preferably, the tris (2,4 (Di-t-butylphenyl) phosphite, tris-nonylphenyl phosphite and triphenyl phosphite. Specific examples thereof include Alkanox 240 (Chemtura Co.), Igafos 168 (Ciba Specialty Chemicals, Inc.) and Songnox 1680 (Songwon Industrial Co., Ltd.).

The radical scavenging agent may be used in an amount of 0.01 to 2.5 parts by weight, preferably 0.03 to 0.6 part by weight, based on 100 parts by weight of the cellulose ester resin. If the amount is less than 0.01 part by weight, The cellulose ester resin melted in the thermoplastic or melt spinning process may be pyrolyzed. If the amount exceeds 2.5 parts by weight, there may be a problem in workability and moldability as a cause of an increase in pack pressure.

Hereinafter, a method of manufacturing a tobacco filter tow using the fiber bundle composition for tobacco filter tow according to the present invention will be described.

The tow of the tobacco filter of the present invention comprises the steps of: preparing a mixed resin by mixing a thermoplastic cellulose ester resin, a plasticizer, a radical formation inhibitor and a radical activity inhibitor; Adding the mixed resin to a kneader and blending the kneaded mixture under a condition of raising the internal temperature of the kneader from 150 ° C to 220 ° C to produce a molten cellulose ester chip; Drying the molten cellulose ester chip at 70 ° C to 90 ° C for 20 to 30 hours; Melting and spinning the dried molten cellulose ester chips through a spinneret to produce a molten cellulose ester fiber bundle; And crimping the molten cellulose ester fiber bundle to produce a tow.

The thermoplastic cellulose ester resin, the plasticizer, the radical formation inhibitor and the radical activity inhibitor in the step of producing the mixed resin have the same kind and composition ratio of the fiber bundle composition for tobacco filter tow described above.

In the step of preparing the melted cellulose ester chips, the blending is preferably performed at a temperature in the range of 160 ° C to 210 ° C, more preferably 165 ° C If the internal temperature of the kneader is less than 150 ° C, the resin may not sufficiently melt to cause a problem that the resin is not smoothly kneaded and is released into an unmelted state. ° C, the main chain of the cellulose ester may be thermally decomposed due to excessive heat, and the color of the chip may be browned and the physical properties may be lowered. Therefore, it is preferable to perform the blending in the above temperature range.

The blending is preferably carried out at 20 kg / h to 30 kg / hr of the circle feeder and at a motor speed of 220 rpm to 300 rpm of the kneader, preferably 22 kg / h to 28 kg / hr of the circle feeder, Performing the kneading at a speed of 240 rpm to 290 rpm results in smooth kneading of the resin, which is advantageous in view of stable workability and productivity.

The kneader may be a general kneader used in the art, preferably a kneader equipped with a twin-screw extruder.

When the melt flow index is measured according to the ASTM D1238 method, the melt cellulose ester resin thus produced has a melt flow rate of 3 to 10 g / 10 min and a shear rate 9 to 20 / s, a melt viscosity of 1,150 to 1,700 Pa.sec, and preferably a melt temperature of 180 to 220 deg. C, a load of 2.16 kg, a heat flow rate of 5 to 9 g / 10 min, a shear rate of 10 to 18 / s, and a melt viscosity of 1,250 to 1,650 Pa.sec.

The drying of the molten cellulose ester chips is carried out at 70 ° C to 100 ° C for 20 to 30 hours, preferably at 75 ° C to 85 ° C for 20 to 26 hours, more preferably at 78 ° C to 85 ° C If the drying temperature is less than 70 ° C., the drying time may become too long, resulting in a decrease in commerciality. In addition, if the drying temperature exceeds 100 ° C., Heat may impart fluidity to the polymer chain, and thermal deformation and thermal decomposition may occur in the chip.

In the step of producing the melt-cellulose ester fiber bundle, it is preferable that the melt spinning is performed at a spinning speed of 2,000 to 3,000 mpm and a spinning temperature of 250 to 290 ° C, preferably at a spinning speed of 2,200 to 2,900 mpm and a spinning temperature More preferably at a spinning rate of 2,300 to 2,800 mpm, and at a spinning temperature of 265 to 285 ° C. If the spinning speed is less than 2,000 mpm, the productivity may be reduced and the production cost may increase. If the spinning speed is higher than 3,000 mpm, the tensile force applied to the molten cellulose fiber is too high to cause a yarn break or a blow- So that it is preferable to perform melt spinning under the above-mentioned spinning speed. If the spinning temperature is lower than 250 ° C, the melt viscosity of the melted cellulose resin is too high to be suitable for the spinning operation, so there may be a problem in the threading in the nozzle. If the spinning temperature exceeds 290 ° C, There is a problem that the resin is thermally decomposed to discolor the color or deteriorate the physical properties.

And, the detachment used for the melt spinning can be a conventional detachment used in the art, and preferably a detachment section detachment can be used. In addition, the above-mentioned shaped cross-section can be used as a cross-shaped cross-section having various forms such as a cross-section cross-section, a polygonal cross-section, a C-cross-section, a circular cross-section, a cross-section cross-section,

The melt-cellulose ester fiber bundle produced by melt-spinning is a melt-cellulose ester fiber having a fineness of 0.8 to 10.0 denier, preferably a melt-cellulose ester fiber having a fineness of 1.5 to 8.0 denier and a fineness of 20,000 to 50,000 It can be manufactured to have a denier of preferably 25,000 to 45,000 denier, more preferably 30,000 to 40,000 denier. If the fineness of the fiber bundle is less than 20,000 denier, the bundle of fibers is too thin, so that there is a problem that the twist is not sufficiently provided in the process of manufacturing the filter, so that the process can not be passed smoothly. If the fineness exceeds 50,000 denier, There may be a problem that smooth passage of the nozzles is not achieved in the above process, and therefore it is preferable to have the fineness .

It is preferable to crimp the bundle of molten cellulose ester fibers so that the number of crimps is 10 to 40 crimps per inch, preferably 20 to 30 crimps per inch. At this time, If the number of crimps is less than 40 pieces / inch, the volume of the tow is increased more than necessary, and thus the cigarette filter manufacturing It is preferable that the crimping be performed so as to have the crimp number within the above range since the nozzle may not pass smoothly during the process.

According to the KS H ISO 6565 method, the tobacco filter tow of the present invention manufactured by this method can have an aspiration resistance of 50% to 65% of tar and 40% to 50% of nicotine when measured, The adsorption removal rate for the material is very good.

Hereinafter, the present invention will be described more specifically by way of examples. However, the following examples should not be construed as limiting the scope of the present invention, but should be construed to facilitate understanding of the present invention.

[ Example ]

Example  1: Preparation of melted cellulose acetate resin

30 parts by weight of polyethylene glycol (polyethylene glycol) having a weight average molecular weight of 600 as a plasticizer was mixed with 100 parts by weight of cellulose acetate having a degree of substitution of cellulose hydroxyl group of 2.4 and a weight average molecular weight of 40,000 (manufactured by Eastman) Respectively.

Next, 100 parts by weight of the mixture was mixed with tetrakis methylene (3,5-di-t-butyl-4-hydroxyhydrocinnamate) methane (Anox 20 (Chemtura Corporation) And 0.1 parts by weight of tris (2,4-di-t-butylphenyl) phosphate (Alcanox 240, Camtura Corporation) as a radical activity inhibitor were added thereto and the mixture was stirred for 2 minutes using a supermixer Mixture 2 was prepared.

Next, the mixture 2 was dried in a hot-air drier at 80 DEG C for 24 hours, fixed with a circulator feeder at 25 kg / hr and a kneader motor speed of 270 rpm using a kneader equipped with a twin-screw extruder, kneaded in a kneader die (DIE) The melted cellulose acetate resin was prepared by blending 5 minutes at a starting temperature of 170 占 폚 for 5 minutes while applying a temperature to a final terminal temperature of 200 占 폚 for 5 minutes.

Example  2

A melted cellulose acetate resin was prepared in the same manner as in Example 1, except that 20 parts by weight of the polyethylene glycol was used for 100 parts by weight of cellulose acetate.

Example  3

A melted cellulose acetate resin was prepared in the same manner as in Example 1, except that the polyethylene glycol was used in an amount of 40 parts by weight based on 100 parts by weight of cellulose acetate.

Example  4

Except that cellulose acetate having a degree of substitution of cellulose hydroxyl group of 2.1 and a weight average molecular weight of 37,000 was used instead of cellulose acetate (substitution degree 2.4, Mw = 40,000) in the same manner as in Example 1, except that the molten cellulose acetate resin Cellulose acetate resin was prepared.

Comparative Example  One

A melted cellulose acetate resin was prepared in the same manner as in Example 1, except that the polyethylene glycol having a weight average molecular weight of 1,200 was used to prepare a melted cellulose acetate resin.

Comparative Example  2

A melted cellulose acetate resin was prepared in the same manner as in Example 1, except that the polyethylene glycol was used in an amount of 5 parts by weight based on 100 parts by weight of cellulose acetate.

Comparative Example  3

A melted cellulose acetate resin was prepared in the same manner as in Example 1, except that the polyethylene glycol was used in an amount of 50 parts by weight based on 100 parts by weight of cellulose acetate.

Comparative Example  4

Except that cellulose acetate having a degree of substitution of cellulose hydroxyl group of 1.4 and a weight average molecular weight of 42,000 was used instead of cellulose acetate (substitution degree 2.4, Mw = 40,000) in the same manner as in Example 1, except that the molten cellulose acetate resin Cellulose acetate resin was prepared.

Experimental Example  1: Measurement of physical properties of melted cellulose ester resin

The properties of the melt-cellulose ester resins prepared in the above Examples and Comparative Examples were measured, and the results are shown in Table 1 below.

The heat flux, shear rate and viscosity were measured according to ASTM D1238, and the melt temperature was set at 230 ° C and the load was measured using 2.16 kg.

division Viscosity
(Pa.sec, 230 < 0 > C) Heat flowability
(g / 10 min, 230 < 0 > C) Shear rate
(s ^-1 , 230 ° C) Example 1 1297.9 8.91 15.09 Example 2 1485.4 7.64 12.16 Example 3 1165.7 9.48 18.41 Example 4 1201.3 8.77 14.38 Comparative Example 1 985.4 2.49 8.63 Comparative Example 2 Not measurable Comparative Example 3 133.1 81.55 147.23 Comparative Example 4 Not measurable

In the case of Comparative Example 2 using 5 parts by weight of plasticizer and Comparative Example 4 using 1.4 having a degree of substitution of less than 1.8, measurement of heat flow, shear rate and melt viscosity at 230 캜 was impossible.

Comparative Example 1 using a plasticizer having a weight average molecular weight of more than 1,000 showed poor viscosity and heat flowability as compared with Example 1 and Comparative Example 3 using a plasticizer in an amount exceeding 45 parts by weight , The viscosity, heat flow rate and shear rate were significantly decreased.

However, unlike Comparative Examples 1 to 4, the melt-cellulose ester resins of Examples 1 to 4 had a heat flow rate of 3 to 10 g / 10 min, a shear rate of 9 to 20 / s, It was confirmed that it had an appropriate physical property of 1,700 Pa.sec.

Manufacturing example  One

The melt cellulose acetate resin prepared in Example 1 was spin-cast on a melt emitter equipped with a 48-hole hollow helix, under conditions of a spinning speed of 2,500 mpm and a spinning temperature of 275 ° C to obtain a melt cellulose ester fiber A fiber bundle composed of 35,000 denier of total fineness was produced.

Next, the fiber bundle was crimped at 25 yarns / inch to prepare a tow for a cellulose-based cigarette filter.

2 ~ Manufacturing example  4

A tobacco filter tow was prepared in the same manner as in Preparation Example 1 except that the molten cellulose ester resin prepared in Example 2 and Example 4 was used in place of the molten cellulose ester resin in Example 1, Respectively, and Production Examples 2 to 4 were respectively carried out.

Manufacturing example  5 ~ Manufacturing example  6

A tobacco filter tow was produced by using the molten cellulose ester resin of Example 1 in the same manner as in Preparation Example 1 except that a bundle of fibers having a total fineness of 28,000 denier was prepared and the bundle of fibers was crimped at a rate of 25 pieces per inch To prepare a tow for a cellulose-based tobacco filter.

Then, a fiber bundle having a total fineness of 44,000 deniers was prepared, and then a fiber bundle was crimped at 25 yarns / inch to prepare a tow for a cellulose-based tobacco filter.

Manufacturing example  7 ~ Manufacturing example  8

A tow for a cigarette filter was prepared using the molten cellulose ester resin of Example 1 in the same manner as in Preparation Example 1, and a fiber bundle was crimped at 15 pcs / inch to prepare a tow for a cellulose-based cigarette filter, 7.

Production Example 8 was carried out by producing a tow for a cellulose-based cigarette filter by applying a fiber bundle to 35 crimps / inch.

Comparative Manufacturing Example  1 ~ Comparative Manufacturing Example  4

Except that the molten cellulose ester resin prepared in Comparative Example 1 to Comparative Example 4 was used in place of the molten cellulose ester resin in Example 1 to prepare a tobacco filter tow in the same manner as in Preparation Example 1, The tows were manufactured and Comparative Production Examples 1 to 4 were respectively carried out.

Comparative Manufacturing Example  5 ~ Comparative Manufacturing Example  6

A tobacco filter tow was produced by using the molten cellulose ester resin of Example 1 in the same manner as in Preparation Example 1 except that a bundle of fibers having a total fineness of 17,000 denier was prepared and then the bundle of fibers was crimped at 25 yarns / To prepare a tow for a cellulose-based tobacco filter, and Comparative Production Example 5 was carried out.

Then, a fiber bundle having a total fineness of 52,000 deniers was prepared, and then a fiber bundle was crimped at 25 yarns / inch to prepare a tow for a cellulose-based cigarette filter, and Comparative Production Example 6 was carried out.

Comparative Manufacturing Example  7 ~ Comparative Manufacturing Example  8

A tow for a cigarette filter was produced using the molten cellulose ester resin of Example 1 in the same manner as in Preparation Example 1, and a fiber bundle was crimped at 8 / inch to prepare a tow for a cellulose-based cigarette filter, Example 7 was carried out.

Then, a fiber bundle was crimped at 45 / inch to produce a tow for a cellulose-based cigarette filter, and Comparative Production Example 8 was conducted as shown in Table 2 below.

division Melted cellulose
Resin type Melted cellulose
Fineness of fiber
( de ) Fiber bundle
Total fineness
( de ) Crimp number
(Dogs / inches) Manufacturing example  One Example 1 3.2 35,000 25 Manufacturing example  2 Example 2 3.1 35,000 25 Manufacturing example  3 Example 3 3.2 35,000 25 Manufacturing example  4 Example 4 3.3 35,000 25 Manufacturing example  5 Example 1 3.3 28,000 25 Manufacturing example  6 Example 1 3.2 44,000 25 Manufacturing example  7 Example 1 3.4 35,000 15 Manufacturing example  8 Example 1 3.2 35,000 35 Comparative Manufacturing Example  One Comparative Example 1 3.2 35,000 25 Comparative Manufacturing Example  2 Comparative Example 2 Inoperable Comparative Manufacturing Example  3 Comparative Example 3 3.3 35,000 25 Comparative Manufacturing Example  4 Comparative Example 4 Inoperable Comparative Manufacturing Example  5 Example 1 Inoperable Comparative Manufacturing Example  6 Example 1 Inoperable Comparative Manufacturing Example  7 Example 1 3.2 35,000 8 Comparative Manufacturing Example  8 Example 1 3.2 35,000 45

Experimental Example  2: Adsorption performance test of tobacco filter tow

The tobacco filter tow prepared in Preparation Examples 1 to 8 and Comparative Production Examples 1 to 8 was subjected to a KS H ISO 6565 method to prepare a 17 mm round tobacco filter and the resistance of the tobacco smoke to tar and nicotine suction in smoking) were measured. The results are shown in Table 3 below.

division Tar suction resistance (%) Nicotine aspiration resistance (%) Toe manufacturing workability Manufacturing example  One 62.8% 49.1% ◎ Manufacturing example  2 57.6% 46.2% ○ Manufacturing example  3 58.3% 45.4% ○ Manufacturing example  4 60.2% 48.1% ○ Manufacturing example  5 52.5% 41.9% ◎ Manufacturing example  6 59.2% 47.3% ○ Manufacturing example  7 50.3% 40.3% ○ Manufacturing example  8 58.7% 47.1% ◎ Comparative Manufacturing Example  One 48.2% 37.8% △ Comparative Manufacturing Example  2 Inoperable × Comparative Manufacturing Example  3 46.8% 36.3% △ Comparative Manufacturing Example  4 Inoperable × Comparative Manufacturing Example  5 Inoperable × Comparative Manufacturing Example  6 Inoperable × Comparative Manufacturing Example  7 40.7% 29.5% △ Comparative Manufacturing Example  8 Inoperable × Toe manufacturing workability - ⊚: very good / ∘: good / △: poor / x: not possible

From the results of the experiment shown in Table 3, it was confirmed that the tobacco filter tow prepared in Production Examples 1 to 8 had an excellent suction resistance with a tar suction resistance of 50% or more and a nichton suction resistance of 40% or more.

In contrast, it was confirmed that Comparative Production Example 1, Comparative Production Example 3 and Comparative Production Example 7 had a tar attraction resistance of less than 49% and a low nicotine attraction resistance of less than 38%.

In Comparative Production Example 2, Comparative Production Examples 4 to 6, and Comparative Production Example 8, the properties of the molten cellulose ester resin used in the manufacture of the tow were not good, the total fineness of the fiber bundle was too high, We could not manufacture dragons.

Through the above Examples and Experimental Examples, it was confirmed that a tobacco filter tow having excellent suction resistance against tar and nicotine can be produced using the fiber bundle composition for tobacco filter tow according to the present invention.

Claims (18)

delete From 15 to 45 parts by weight of a plasticizer, from 0.01 to 2 parts by weight of a radical formation inhibitor and from 0.01 to 2.5 parts by weight of a radical activity inhibitor, based on 100 parts by weight of the thermoplastic cellulose ester resin,
The thermoplastic cellulose ester resin preferably has a cellulose hydroxyl group substitution degree of 1.8 to 3, a weight average molecular weight of 30,000 to 60,000,
Wherein the plasticizer comprises at least one selected from polyethylene glycol having a weight average molecular weight of 1,000 or less, polypropylene glycol, polyglycolic acid, polybutyl adipate, glycerin, tributyl sebacate, triacetin and triethyl citrate,
Wherein the radical generation inhibitor comprises a water insoluble compound comprising a phenolic group and wherein the radical activity inhibitor comprises a water insoluble compound containing phosphorus at the terminal.
The thermoplastic resin composition according to claim 2, wherein the thermoplastic cellulose ester resin
Selected from cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, cellulose acetate phthalate, cellulose acetate caprate, cellulose acetate caprylate, cellulose acetate laurethate, cellulose acetate palmitate, cellulose acetate stearate and cellulose acetate oleate Wherein the fiber bundle composition comprises at least one fiber bundle.
delete delete The method of claim 2, wherein the radical generation inhibitor is selected from the group consisting of tetrakis methylene (3,5-di-t-butyl-4-hydroxycinnamate) methane, pentaerythritol tetrakis (3- (3,5- Butyl-4-hydroxyphenyl) propionate and tetrakis methylene (3,5-di-t-butyl-4-hydroxyphenyl) propionate methane. A fiber bundle composition for filter tow.
3. The cigarette according to claim 2, wherein the radical activity inhibitor comprises at least one selected from tris (2,4-di-t-butylphenyl) phosphite and tris-nonylphenyl phosphite and triphenyl phosphite A fiber bundle composition for filter tow.
Mixing the fiber bundle composition for a tobacco filter tow of any one of claims 2, 3, 6, and 7 to prepare a mixed resin;
Adding the mixed resin to a kneader and blending the kneaded mixture under a condition of raising the internal temperature of the kneader from 150 ° C to 220 ° C to produce a molten cellulose ester chip;
Drying the molten cellulose ester chip at 70 ° C to 90 ° C for 20 to 30 hours;
Melting and spinning the dried molten cellulose ester chips through a spinneret to produce a molten cellulose ester fiber bundle; And
And crimping the molten cellulose ester fiber bundle to produce a tow,
Wherein the mixed resin has a melt flow rate of from 3 to 10 g / 10 min, a shear rate of from 9 to 20 / s, a melt viscosity of from 1 to 10 g / 10 min, a melt viscosity of from 160 to 230 캜, Is 1,150 to 1,700 Pa.sec,
Wherein the molten cellulose ester fiber bundle comprises a fused cellulose ester fiber having a fineness of 0.8 to 10.0 denier in a fineness of 25,000 to 45,000 denier,
Wherein the crimp crimps the molten cellulose ester fiber bundle at 20 to 30 crimps per inch.
The kneader of claim 8, wherein the kneader is a kneader equipped with a twin-screw extruder,
Wherein the blending is performed at 20 to 30 kg / hr of a circle feeder and at 220 to 300 rpm of a kneader motor speed.
The method of claim 8, wherein the melt spinning is performed at a spinning speed of 2,000 to 3,000 mpm and a spinning temperature of 250 to 290 ° C.
The method of claim 8, wherein the detachment is a deformed section detachment, wherein the deformed section detachment is characterized by a cross section section section, a polygonal section section section, a C section section section, a circular section section section, a four section section section section, Of the tobacco filter.
delete delete delete A bundle of molten cellulose ester fibers having a number of crimps of 20 to 30 yarns / inch formed from a fiber bundle composition for a tobacco filter of any one of claims 2, 3, 6, and 7,
Wherein the fiber bundle comprises molten cellulose ester fibers having a fineness of 0.8 to 10.0 denier in a total fineness of 25,000 to 45,000 denier.
delete delete The tobacco filter tow according to claim 15, characterized in that the suction resistance is between 50% and 65% of tar and between 40% and 50% of nicotine when measured according to the KS H ISO 6565 method.