KR101765291B1 - Cigarette filter having lyocell tow and manufacturing method thereof - Google Patents

Abstract

A cigarette filter according to an embodiment of the present invention includes a lyocell tow including a plurality of lyocell fibers and is made of TBPH (Tetra Butyl Phophonium Hydroxide), water (H ₂ O), and PG propylene glycol), the plurality of lyocell fibers are cross-linked to each other at at least one junction.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a cigarette filter including a lyocell tow and a method of manufacturing the same.

A cigarette filter comprising a lyocell tow and a method of manufacturing the same are provided

Generally, in order to produce cigarettes, various kinds of leaf tobacco are first blended and processed so as to have desired flavor and taste. Next, the processed leaf tobacco is folded to prepare cut tobacco leaf, and the cigarette tobacco is rolled with cigarette paper to produce a filter-free cigarette. Next, the filter is attached to the filter-free cigarette if necessary.

The cigarette may be made of flax, wood pulp, etc., and it is required that the burning property and flavor of the cigarette are maintained when burned. The cigarette filter may include activated charcoal, flavor, etc., and may be composed of mono filters or multiple filters and is surrounded by cigarette filter wrapping paper. The tobacco filter is connected to the cigarette buttocks by tipping paper, and the tip paper may contain fine holes.

Conventional cigarette filters use cellulose acetate tow which is acetylated by extracting cellulose from wood pulp. In recent years, development of substitute materials for eco-friendly materials has been proceeding in order to protect natural environment and reduce cost. For example, unlike cellulose acetate, the development of tow using lyocell fiber in which cellulose itself is fibrous is under development.

When a cigarette filter is manufactured from a bundle of fiber strands, the hardness of the cigarette filter is low when the plasticizer or the curing agent is not used together, and the filter can be put on the drum in the filter manufacturing process or the cigarette manufacturing process. Therefore, it is necessary to improve the hardness of a certain level of the cigarette filter. For example, a method of increasing the hardness of a filter includes a method using a hardener and a method using a plasticizer. A method of using a hardener is a method of applying hardness to a filter by bonding a fiber strand using a binder-like material, and hardening the filter. A method of using a plasticizer is a method in which a fiber itself is partially dissolved or plasticized using a specific material to form a joint between fibers, and then plasticized. For example, in the case of cellulose acetate, TA (triacetin) is used as a plasticizer.

Recently, a plasticizer suitable for lyocell fibers has been researched and developed to improve the hardness of a cigarette filter to be manufactured.

One embodiment of the present invention is to improve the hardness of a tobacco filter through a plasticizer suitable for a tow comprising lyocell.

And can be used to achieve other tasks not specifically mentioned other than the above tasks.

A cigarette filter according to an embodiment of the present invention includes a lyocell tow including a plurality of lyocell fibers and is made of TBPH (Tetra Butyl Phophonium Hydroxide), water (H ₂ O), and PG propylene glycol), the plurality of lyocell fibers are cross-linked to each other at at least one junction.

TBPH may be from 46% by mass to 55% by mass, water may be from 14% by mass to 20% by mass, and PG may be from 25% by mass to 39% by mass based on the whole plasticizer component.

The hydrogen ion concentration index of the plasticizer component may be from pH 10 to pH 13.

Wherein the plasticizer component further comprises ethanol and the content of TBPH is from 46 mass% to 55 mass%, the content of water is from 14 mass% to 20 mass%, the content of PG and ethanol is 25 mass% 39% by mass.

On the basis of PG and ethanol, ethanol may be 30 mass% or less.

A method of manufacturing a cigarette filter according to an embodiment of the present invention includes preparing a lyocell tow comprising a plurality of lyocell fibers, a step of preparing a solution containing tetrabutylphosphonium hydroxide (TBPH), water (H2O), and propylene glycol Preparing a plasticizer solution, and contacting the lyocell tow with a plasticizer solution.

In the step of preparing the plasticizer solution, the mass ratio of TBPH to the plasticizer solution is 46 mass% to 55 mass%, the mass ratio of water to the plasticizer solution is 14 mass% to 20 mass%, and the mass ratio of PG to the plasticizer solution is 25 Mass% to 39 mass%.

The step of preparing the plasticizer solution comprises preparing TBPH by mixing an aqueous solution of TBPBr (tetrabutylphosphonium bromide) or an aqueous solution of TBPI (tetrabutylphosphonium iodide) and an ion exchange resin, adding PG to prepare a plasticizer solution .

The step of preparing the plasticizer solution may further include washing the ion exchange resin.

The ion exchange resin may be a polymer material containing hydroxide ions.

After the step of preparing the plasticizer solution, the step of evaporating the water to concentrate the plasticizer solution may be further included.

The step of concentrating the plasticizer solution may be carried out in an atmosphere of 20 ° C to 25 ° C.

The hydrogen ion concentration index of the plasticizer solution may be from pH 10 to pH 13.

In the step of preparing the plasticizer solution, the plasticizer solution further contains ethanol, and the content of TBPH is from 46 mass% to 55 mass% and the content of water is from 14 mass% to 20 mass% based on the total amount of the plasticizer solution, PG and ethanol are 25 mass% to 39 mass%, and the amount of ethanol can be 30 mass% or less based on PG and ethanol.

According to one embodiment of the present invention, the hardness of the cigarette filter can be improved by including or using a tow comprising a lyocell and a suitable plasticizer therefor.

1 is a SEM photograph of a lyocell tow according to an embodiment.
2 is a graph showing mass ratios among the components of the plasticizer component.
FIGS. 3A and 3B are graphs and tables showing mass ratios among the constituents of the plasticizer component according to comparative examples, and FIG. 3C is a SEM photograph of a lyocell tow containing the plasticizer component of sample 1 (# 1).
4A and 4B are graphs and tables showing mass ratios between the constituents of the plasticizer component according to the examples and comparative examples, and Fig. 4C is a SEM photograph of the lyocell tow containing the plasticizer component of the sample A (#A) 4E is an SEM photograph of a lyocell tow containing a plasticizer component of sample C (#C), and Fig. 4F is a SEM photograph of a lyocell tow containing a plasticizer component of sample B Is an SEM photograph of a lyocell tow containing a plasticizer component of sample D (#D), and Figure 4g is an SEM photograph of a lyocell tow containing a plasticizer component of sample E (#E).
5A is an SEM photograph of a lyocell tow containing a water-free plasticizer component, and Fig. 5B is an SEM photograph of a lyocell tow containing a water-added plasticizer component.
6 is a table showing the mass ratio of the plasticizer component according to the embodiment and the mass ratio of the plasticizer component according to the comparative example.
7A and 7B are tables showing the degree of decomposition of TBPH according to the concentration temperature.

BRIEF DESCRIPTION OF THE DRAWINGS The above and other features and advantages of the present invention will be more apparent from the following detailed description taken in conjunction with the accompanying drawings, in which: FIG. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. In order to clearly illustrate the present invention, parts not related to the description are omitted, and the same reference numerals are used for the same or similar components throughout the specification. In the case of publicly known technologies, a detailed description thereof will be omitted.

Throughout the specification, when an element is referred to as "comprising ", it means that it can include other elements as well, without excluding other elements unless specifically stated otherwise.

Hereinafter, a cigarette filter including a lyocell according to an embodiment of the present invention will be described.

The cigarette filter including the lyocell according to the embodiment includes a lyocell tow including a plurality of lyocell fibers, and tetrabutylphosphonium hydroxide (TBPH), water (H ₂ O), and propylene glycol (PG) Lt; / RTI > In a lyocell tow, adjacent lyocell fibers may be cross-linked to each other at at least one junction. When TBPH, water, and PG are applied as a plasticizer to a cigarette filter containing lyocell tow, the hardness of the cigarette filter can be improved.

Referring to FIG. 1, in the Liocell tow according to the embodiment, adjacent Liocell fibers are joined and cross-connected to each other, so that the shape of the Liocell fiber is not recognized. This is because the bonding of the lyocell fibers was performed by the plasticizer component. As a result, the hardness of the lyocell tow can be increased and the hardness of the lyocell tow filter can be increased.

Referring to Fig. 2, in the three component plasticizer component, the mass ratio of TBPH may be about 46 mass% to about 55 mass%. Within this mass ratio, the joining of the lyocell fibers can be made more fully and the hardness of the lyocell tow and the tobacco filter containing it can be further increased. Accordingly, in the process of manufacturing the cigarette filter, the phenomenon in which the cigarette filter is caught in the drum can be further reduced.

In the plasticizer component, the mass ratio of water may be about 14 mass% to about 20 mass%, and within this range, the plasticizing ability of the plasticizer component can be further improved.

On the other hand, in the plasticizer component, the mass ratio of PG may be about 25 mass% to about 39 mass%. Accordingly, the hardness of the cigarette filter can be further improved, and the amount of impurities generated in the process of manufacturing the cigarette filter can be further minimized.

Such plasticizer components may not contain alkali metal cations such as sodium cations (Na ⁺ ) or potassium cations (K ⁺ ). The alkali metal cation lowers the plasticity of the plasticizer component and lowers the hardness of the lyocell tow.

Further, the plasticizer component according to the embodiment may not contain impurities such as TBP (tributylphosphine), or may contain a minimum amount of impurities. For example, TBP is an impurity produced by decomposition of TBPH, and can reduce the mass ratio of TBPH. Thus, if the impurities in the plasticizer component are minimized, the plasticizing ability of the plasticizer component can be improved.

On the other hand, the hydrogen ion concentration index of the plasticizer component in contact with the lyocell tow may be about pH 10 to about pH 13. [ Within this range, the plasticizing ability of the plasticizer component can be improved, and the lyocell tow containing the plasticizer component can have sufficient hardness.

The plasticizer component may further comprise ethanol. Wherein the TBPH is from about 46 mass% to about 55 mass%, the water is from about 14 mass% to about 20 mass%, the PG and ethanol are from about 25 mass% to about 39 mass% .

Here, ethanol and PG function as a solvent. When the sum of the mass ratio of ethanol and the mass ratio of PG is within the above-mentioned numerical value range, the plasticizing ability of the plasticizer component can be improved.

In such a four-component plasticizer component, ethanol may be about 30 mass% or less based on the sum of the PG content and the ethanol content. In such a numerical range, the tentative ability of the tentative component can be more excellent, and the lyocell tow can have sufficient hardness.

Hereinafter, a method of manufacturing a cigarette filter including a lyocell tow according to an embodiment of the present invention will be described.

A method of preparing a cigarette filter comprising a lyocell tow comprises the steps of preparing a lyocell tow comprising a plurality of lyocell fibers, preparing tetrabutyl phosphonium hydroxide (TBPH), water (H ₂ O), and propylene glycol (PG) Preparing a contained plasticizer solution, and contacting the lyocell tow with a plasticizer solution.

First, in the step of preparing the plasticizer solution, the mass ratio of TBPH to the plasticizer solution may be about 46 mass% to about 55 mass%, and the mass ratio of water to plasticizer solution may be about 14 mass% to about 20 mass% The mass ratio of PG to the plasticizer solution may be from about 25 mass% to about 39 mass%.

3A to 3C show SEM photographs of the sample 1 and the mass ratio of the plasticizer component according to the comparative examples (# 1 to # 12).

In the case of Sample 1 (# 1) to Sample 5 (# 5) and Sample 9 (# 9) to Sample 12 (# 12) in which the mass ratio of TBPH is less than 46 mass% .

In addition, in the case of Sample 6 (# 6) to Sample 8 (#) in which the mass ratio of water is less than 14 mass%, the bonding of the lyocell fibers may hardly occur compared to the embodiments.

In the case of Sample 1 (# 1) to Sample 6 (# 6) and Sample 10 (# 10) to Sample 12 (# 12) in which the mass ratio of PG is more than 39 mass% .

4A to 4G, the plasticizing ability according to the mass ratio of each component of the plasticizer solution according to the embodiments can be confirmed.

Specifically, the sample A (#A) is a plasticizer solution according to the embodiment, and can show colorlessness without generating impurities. Sample B (#B) is a plasticizer solution according to another embodiment, which has no purity but has a pale yellow color. This pale yellow can be removed by setting the concentration temperature to a low temperature of about room temperature.

The plasticizing performance of the plasticizer solution according to the sample A (#A) and the sample B (#B) can have excellent plasticizing performance, as shown in Figs. 4C and 4D.

On the other hand, the sample C (#C) is a plasticizer solution according to the comparative example, which can have some degree of plasticity, but can generate impurities and have a yellow color. Here, the impurity may be TBP. It is also possible to have a yellow color by setting the concentration temperature at a high temperature. Further, in the case of the plasticizer solution according to Sample C (#C), the plasticity ability can be somewhat lowered, including TBPH exceeding about 55 mass%.

Sample D (#D) is a plasticizer solution according to another comparative example, containing less than about 46% by weight of TBPH and containing greater than about 39% by weight of PG, It can have a plasticity ability.

Sample E (#E) is a plasticizer solution according to another comparative example and can have significantly lower plasticizing ability, as shown in Figure 4G, because it contains less than about 14% by weight of water.

FIG. 6 is a table showing NMR component concentration of a plasticizer solution containing TBPH, water, and PG, and a plasticizer solution containing TBPH, water, and ethanol.

Referring to FIG. 6, in the case of using the ethanol as a solvent instead of PG, the plasticizer solution may decompose TBPH and contain a relatively large amount of impurities such as TBP. As a result, the mass ratio of TBPH can be reduced and the plasticizing ability of the plasticizer solution can be reduced. In this case, the decomposition index may be about 55.

On the other hand, in the case of the plasticizer solution in which PG is used as the solvent, the amount of impurities can be reduced, and the decomposition index in this case can be about 34. [

Here, the decomposition index can be defined by the following equation (1).

The target concentration means the mass ratio of the target TBPH in the plasticizer solution.

However, unlike the table of FIG. 6, in the case where PG and ethanol are simultaneously contained in the plasticizer solution, the plasticizing ability of the plasticizer solution can be maintained.

For example, in the step of preparing the plasticizer solution, the plasticizer solution may further contain ethanol. Wherein the TBPH is from about 46 mass% to about 55 mass%, the water is from about 14 mass% to about 20 mass%, the PG and ethanol are from about 25 mass% to about 39 mass% . However, based on the sum of the content of PG and the content of ethanol, ethanol may be about 30 mass% or less.

Within the above-mentioned mass ratios, the joining of the lyocell fibers can be made sufficiently and the hardness of the lyocell tow and the tobacco filter containing it can be increased. Accordingly, in the manufacturing process of the cigarette filter, the tobacco filter can be prevented from being caught in the drum. In addition, the amount of impurities generated during the manufacturing process of the cigarette filter can be minimized.

Meanwhile, the step of preparing the plasticizer solution may be performed by mixing TBPBr (tetrabutylphosphonium bromide) aqueous solution or TBPI (tetrabutylphosphonium iodide) aqueous solution with an ion exchange resin to produce TBPH, adding PG to the plasticizer Solution. ≪ / RTI >

The reaction scheme 1 below shows the process of producing TBPH using an aqueous solution of TBPI, and the process of producing TBPH using the aqueous solution of TBPBr is also the same.

[Reaction Scheme 1]

TBPH according to conventional techniques was prepared using a precipitation method using NaOH or KOH. On the other hand, in the case of using the ion exchange resin, the amount of the alkali metal cation such as Na + or K + can be minimized, and the degradation of the alkaline metal cation can be minimized.

Here, the ion exchange resin may have a structure represented by the following chemical formula (1) and may be a polymer material containing hydroxide ions. The ion exchange resin may be a copolymer including, for example, styrene and divinylbenzene as monomers.

[Chemical Formula 1]

Meanwhile, the method of manufacturing a cigarette filter including a lyocell tow according to an embodiment may further include washing the ion exchange resin before preparing the plasticizer solution.

The washing of the ion exchange resin may be, for example, washing with water or ethanol, and washing with water and washing with ethanol may be alternately performed.

When the washing of the ion exchange resin is carried out, the amount of impurities can be remarkably reduced compared with the case of not cleaning, and thus the plasticizing ability of the solution of the plasticizer can be improved.

On the other hand, after the step of preparing the plasticizer solution, the step of evaporating the water and concentrating the plasticizer solution may be further included.

Here, the step of concentrating the plasticizer solution may be carried out in an atmosphere at about 20 ° C to about 25 ° C.

Referring to FIGS. 7A and 7B, when the plasticizer solution is concentrated at a temperature of about 65 ° C to about 70 ° C (# 1), the amount of impurity TBP is greatly increased, have.

On the other hand, when the plasticizer solution is concentrated at a temperature of about 20 ° C to about 25 ° C (# 3), the amount of TBP as an impurity is greatly reduced and the amount of decomposed TBPH is small, Can be seen.

EXAMPLES Hereinafter, the present invention will be described in more detail with reference to Examples. However, the following Examples are merely examples of the present invention, but the present invention is not limited to the following Examples.

Example 1 below shows a process for producing TBPH using an aqueous solution of TBPI, but the present invention is not limited thereto, and TBPH can also be prepared using an aqueous solution of TBPBr.

Example 1

First, 30.348 g of TBP and 45 ml of diethyl ether are added to a 500 ml three-necked flask, followed by stirring for 5 minutes to prepare a TBP solution. To this solution was slowly added 3.123 g of BuI at about 25 DEG C dropwise, and the reaction solution was heated to about 50 DEG C and reacted for about 6 hours under reflux. The reaction solution after heating has two phases, solid and liquid.

Subsequently, the mixture was filtered using a vacuum flask to obtain a solid. About 1 L of diethyl ether was added to the obtained solid, stirred for about 10 minutes, and filtered to obtain a solid. Repeat this process two times in total.

The solid product TBPI obtained after purification is recovered and dried at room temperature or dried under reduced pressure and at about 100 캜 for about 30 minutes using an evaporator.

Then, add 10 g of TBPI and 200 ml of water to a 1000 ml flask and stir. Add approximately 195 g of ion exchange resin (wet) to approximately 800 ml of water and stir for 30 minutes. Filter the water. This process is repeated one more time. The ion-exchange resin finally obtained is dried in air for about 4 hours or for about 5 hours, and the mass of the ion-exchange resin is 195 g.

About 45 g of the obtained ion-exchange resin was put into an aqueous solution of TBPI, and stirred at about 35 ° C for about 3 hours.

At this time, hydrogen peroxide is used to confirm the conversion of TBPI to TBPH. A small amount of reaction solution is collected during the reaction, and hydrogen peroxide is added to observe the color change. If the color of the solution changes to yellow, stirring is further carried out, and if there is no change, the reaction is terminated.

Next, about 150 g of the 195 g of the ion exchange resin obtained above is charged into the ion exchange column, and then the TBPH aqueous solution is flowed. Wherein the flow rate can be from about 10 ml / min to about 20 ml / min.

About 2.104 g of PG (propylene glycol) was added to the TBPH aqueous solution obtained, and the water was evaporated under reduced pressure and at about 25 ° C for about 6 hours using an evaporator to obtain a total of three component solutions including TBPH, water and PG So that the mass is 14.029 g. When all 10 g TBPI are converted to TBPH, it can be assumed that 7.155 g TBPH is present in the solution, so that the mass fraction of final TBPH, water, and PG in the three component plasticizer solution may be 51: 15: 34 .

Thereafter, a plasticizer solution prepared by using air spray at room temperature is applied to a lyocell tow made of lyocell fibers. Then, a filter paper is filled with a plasticizer-coated tow to prepare a cigarette filter.

Thus, the hardness of the lyocell tow contacted with the plasticizer solution can be improved, and the hardness of the lyocell filter including the lyocell tow can also be improved.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, Of the right.

Claims (14)

A lyocell tow comprising a plurality of lyocell fibers,
The plurality of lyocell fibers are cross-linked to each other at at least one junction point by a plasticizer component comprising TBPH (Tetra Butyl Phophonium Hydroxide), water (H ₂ O), and PG (propylene glycol)
Wherein the TBPH is from 46 mass% to 55 mass%, the water is from 14 mass% to 20 mass%, and the PG is from 25 mass% to 39 mass%, based on the whole plasticizer component. delete The method of claim 1,
Wherein the hydrogen ion concentration index of the plasticizer component is from pH 10 to pH 13. The method of claim 1,
Wherein the plasticizer component further comprises ethanol,
Wherein the TBPH is from 46 mass% to 55 mass%, the water is from 14 mass% to 20 mass%, and the PG and the ethanol are from 25 mass% to 39 mass% based on the entire plasticizer component. 5. The method of claim 4,
And the ethanol is 30 mass% or less based on the PG and the ethanol. Preparing a lyocell tow comprising a plurality of lyocell fibers,
Preparing a plasticizer solution containing tetrabutylphosphonium hydroxide (TBPH), water (H ₂ O), and propylene glycol (PG); and
Contacting the plasticizer solution with the lyocell tow
Lt; / RTI >
Wherein the mass ratio of TBPH to the plasticizer solution is from 46 mass% to 55 mass%, the mass ratio of water to the plasticizer solution is 14 mass% to 20 mass%, the mass ratio of PG to the plasticizer solution is 25 mass% To 39% by mass,
The preparation of the plasticizer solution may be performed by mixing and stirring an aqueous solution of TBPBr (tetrabutylphosphonium bromide) or an aqueous solution of TBPI (tetrabutylphosphonium iodide) and an ion exchange resin to produce the TBPH, Wherein the PG is prepared by reacting a part of the aqueous solution mixed and agitated with the ion exchange resin before adding the PG to hydrogen peroxide to add the PG in the absence of color change. delete delete The method of claim 6,
Further comprising washing the ion exchange resin prior to the step of preparing the plasticizer solution. The method of claim 6,
Wherein the ion exchange resin is a polymer material containing hydroxide ions. The method of claim 6,
Further comprising, after the step of preparing the plasticizer solution, evaporating the water to concentrate the plasticizer solution. 12. The method of claim 11,
Wherein the step of concentrating the plasticizer solution is carried out in an atmosphere at 20 캜 to 25 캜. The method of claim 6,
Wherein the hydrogen ion concentration index of the plasticizer solution is in the range of pH 10 to pH 13. The method of claim 6,
In preparing the plasticizer solution,
Wherein the plasticizer solution further comprises ethanol,
Based on the entirety of the plasticizer solution, the TBPH is 46 mass% to 55 mass%, the water is 14 mass% to 20 mass%, the PG and the ethanol are 25 mass% to 39 mass%
And the ethanol is 30 mass% or less based on the PG and the ethanol.

Images