WO2018087869A1

WO2018087869A1 - Spherical powder aggregate, and production method therefor

Info

Publication number: WO2018087869A1
Application number: PCT/JP2016/083428
Authority: WO
Inventors: 文貴寺尾; 正立松
Original assignee: 日本たばこ産業株式会社
Priority date: 2016-11-10
Filing date: 2016-11-10
Publication date: 2018-05-17

Abstract

Provided is a spherical powder aggregate which is formed from a material including microcrystalline cellulose and a binder, and which has a particle size of 1.0-6.0 mm, a breaking strength of 1.5-5.0 N, and a strain ratio of 5.0-15.0%. Also provided is a production method for the spherical powder aggregate.

Description

Spherical powder aggregate and method for producing the same

The present invention relates to a spherical powder aggregate and a method for producing the same.

Cigarettes are known that enjoy the taste and / or scent by sucking the powder in the filter. For example, Patent Document 1 discloses that a particulate material is accommodated in a chamber in a filter, and the particulate material is supplied to a delivery end via a fluid passage.
Patent Document 2 describes, as a technique related to tobacco products, enclosing a fragrance in solid particles made of natural polysaccharides or derivatives thereof.
U.S. Patent No. 6,057,049 describes tobacco beads comprising tobacco particles that are placed in a filter to remove at least one smoke component from mainstream smoke.
Patent Document 4 describes a smoking article in which a sustained-release liquid delivery material is incorporated in a filter portion. The liquid delivery material described in Patent Document 4 includes a polymer matrix containing a matrix-forming polymer and a plasticizer, and alginic acid and pectin are described as the matrix-forming polymer.

JP-A-60-192581 JP-A 64-27461 JP-T 2008-531008 Special table 2014-532435 gazette

In the inventions described in

Patent Documents

1 and 2, a powder is used as a perfume itself or a perfume carrier.
However, none of the powders used in these inventions are molded by themselves, and there is no description in these patent documents about spherical powder aggregates that form fine powders after breakage .

Patent Documents

1 and 2 do not describe microcrystalline cellulose as a powder raw material.
Patent Document 3 describes tobacco beads, which contain tobacco particles as an essential component as described above. Patent Document 3 describes microcrystalline cellulose as an arbitrary material for constituting tobacco beads, but does not describe beads having the microcrystalline cellulose as a main component and containing no tobacco particles. Patent Document 3 describes obtaining tobacco beads by extruding a material.
In addition, when microcrystalline cellulose is compressed with a tableting machine, particles can be easily entangled and molded, so that it is widely used as a nucleating agent for tablets and the like.
In addition, as a general molding method of powder used in the field of foods, etc., a method including a wet extrusion granulation step and a sizing step, or a powder is molded into a spherical shape using a round machine to obtain a molded product The method is known.
However, the conventional powder molding methods used in the field of foods and the like, and the moldings obtained by using the tableting method are very hard and are broken by human fingers to give a fine granular shape. It was difficult to do. Therefore, it is expected that the tobacco beads described in Patent Document 3 using extrusion molding cannot be easily broken by a human finger. In the first place, Patent Document 3 does not describe any destruction of tobacco beads with human fingers.
Next, in the inventions described in

Patent Documents

2 and 3, it is assumed that the liquid fragrance is supported, and after the liquid fragrance is supported, the liquid fragrance exudes from the carrier. There is no particular mention of the problem. In this regard, Patent Document 3 describes that the volatile liquid compound is stored in the matrix of tobacco beads and the storage period is extended, but this is a problem different from the exudation of liquid fragrance. is there.
On the other hand, Patent Document 4 describes that when a user applies a predetermined force, the flavor composition confined in the matrix structure of the flavor delivery material is released from the matrix structure. It is not the powder that forms the matrix structure, but the polymer that requires ionic crosslinking. Further, it is not described that the flavor delivery material is destroyed by a user's hand.

Therefore, in the present invention, it is applicable to smoking articles and the like, and has a hardness that can be broken down by a person's finger to make it fine and a suitable displacement at the time of breaking so that a person can feel good splitting comfort. It is an object of the present invention to provide a spherical powder aggregate having good absorbability when a liquid is added and a method for producing the spherical powder aggregate.

As a result of intensive studies by the present inventors, a spherical powder aggregate composed of a material containing microcrystalline cellulose and a binder, the particle diameter of the powder aggregate is 1.0 to 6.0 mm, and the fracture strength is It was found that when it is 1.5 to 5.0 N and the strain rate is 5.0 to 15.0%, it can be easily broken by a human finger and a fine granular powder is produced after the breaking. .
Furthermore, the spherical powder aggregate having the above configuration is excellent in liquid absorbency.
Further, as a result of intensive studies by the present inventors, a slurry containing microcrystalline cellulose, a binder, and ethanol is dropped onto a vibrating powder to form a spherical intermediate composition composed of the slurry and the powder. And a spherical powder having the above-mentioned physical properties by the method for producing a spherical powder aggregate, comprising the step of drying the spherical intermediate composition so that the liquid content of the spherical intermediate composition is reduced to 2% by weight or less. Aggregates were found to be obtained.

That is, the present invention is as follows.
[1] A spherical powder aggregate composed of a material containing microcrystalline cellulose and a binder, the particle diameter of the powder aggregate is 1.0 to 6.0 mm, and the fracture strength of the powder aggregate is 1. A spherical powder aggregate having a strain rate of 5 to 5.0 N and a strain rate of 5.0 to 15.0%.
[2] The spherical powder aggregate according to [1], wherein the density of the powder aggregate is 0.2 to 0.8 g / cm ³ .
[3] The spherical powder aggregate according to [1] or [2], wherein the binder is at least one water-soluble polymer selected from starch, gelatin, gum arabic, polyvinyl alcohol, and carboxymethylcellulose.
[4] The spherical powder aggregate according to any one of [1] to [3], wherein the total content of microcrystalline cellulose and binder in the powder aggregate is 70.5 to 98% by weight.
[5] The spherical powder aggregate according to any one of [1] to [4], wherein the powder aggregate contains a fragrance.
[6] A first step of dropping a slurry containing microcrystalline cellulose, a binder and ethanol onto a vibrating powder to form a spherical intermediate composition composed of the slurry and the powder; A method for producing a spherical powder aggregate, comprising a second step of drying so that the liquid content is reduced to 2% by weight or less.
[7] The method for producing a spherical powder aggregate according to [6], wherein the powder is microcrystalline cellulose.
[8] The method for producing a spherical powder aggregate according to [6] or [7], wherein the binder is at least one water-soluble polymer selected from starch, gelatin, gum arabic, polyvinyl alcohol and carboxymethylcellulose. .
[9] The method for producing a spherical powder aggregate according to any one of [6] to [8], wherein the content of microcrystalline cellulose in the slurry is 15 to 25% by weight.
[10] The method for producing a spherical powder aggregate according to any one of [6] to [9], wherein the drying in the second step is performed by hot air drying.
[11] The method for producing a spherical powder aggregate according to any one of [6] to [10], wherein the drying in the second step is performed while vibrating the spherical intermediate composition.

The spherical powder aggregate of the present invention has an appropriate breaking displacement so that the breaking strength thereof can be easily broken by a human finger, and a person can feel a good feeling of splitting. Therefore, when the spherical powder aggregate of the present invention is arranged in a filter part used for a smoking article such as a cigarette, when the spherical powder aggregate is broken by a smoker's finger, Can deliver to the user the perfume contained in the powder agglomerate with the mainstream smoke. Moreover, the absorptivity at the time of adding a liquid is favorable. Thus, when the liquid fragrance is absorbed in the spherical powder aggregate of the present invention, for example, a role as a fragrance carrier or a flavor retainer can be expected.
In addition, according to the method for producing a spherical powder aggregate of the present invention, a powder aggregate having a fracture strength that can be easily broken by a human finger and an appropriate displacement at the time of breakage so that a person can feel good comfort. Can be provided.

It is a figure which shows each state of a powder aggregate at the time of measuring the fracture strength of a spherical powder aggregate. It is the schematic which shows the relationship between the displacement of a rheometer contact, and stress at the time of measuring the fracture strength of a spherical powder aggregate. It is a figure (photograph) which shows each state before and after destruction of a spherical powder aggregate. It is a figure which shows the relationship between the load in the case of the measurement of the powder aggregate of an Example, and elapsed time by a rheometer. It is a figure which shows the relationship between the load in the case of the measurement of the molded object shape | molded with the round making machine by a rheometer, and elapsed time. It is a figure which shows the relationship between the load in the time of the measurement of the biscopar A by a rheometer, and elapsed time. It is a figure which shows the relationship between the load in the time of the measurement of the biscopar P by a rheometer, and elapsed time.

Hereinafter, the present invention will be described in detail with reference to embodiments, examples, etc., but the present invention is not limited to the following embodiments, examples, etc., and can be arbitrarily set within the scope of the present invention. Can be changed and implemented.

The spherical powder aggregate of the present invention is a spherical powder aggregate composed of a material containing microcrystalline cellulose and a binder, and has a particle size of 1.0 to 6.0 mm, manufactured by Rheometer (Sun Science Co., Ltd.). CR-3000EX-S) has a load cell maximum stress of 200 N under the condition of MODE 3 and a breaking strength of 1.5 to 5.0 N when the moving speed of the table is measured at 20.0 mm / min. A contactor for compressive strength test is used.
The breaking strength is more preferably 2.0 to 4.0 N as an appropriate breaking strength when being broken by a human hand.
The strain rate of the spherical powder aggregate of the present invention is 5.0 to 15.0%. The strain rate as used herein refers to the distance traveled from the time when the contact element contacts the powder aggregate to the time when the powder aggregate is broken when the fracture strength is measured by the rheometer. It is a numerical value obtained by multiplying the value divided by the diameter by 100, and is also called displacement at break. The smaller the strain rate, the more the fracture occurs when the powder aggregate has a smaller compression width.
An embodiment in which the strain rate of the spherical powder aggregate is 5.0 to 12.0% can also be mentioned.

The powder agglomerate as used in the present invention is one in which crystal particles made of a material constituting the same aggregate to form one spherical mass. For example, the powder agglomerate produced by the production method of the present invention was obtained by volatilizing ethanol over a drying process after granulating a slurry-powder mixture containing ethanol dropwise into the powder as described later. In this process, microcrystalline cellulose, binder and the like dissolved in the slurry are precipitated and aggregated as crystal particles to form a spherical mass. Because of this, the powder aggregate of the present invention is porous.
The “spherical shape” in the spherical powder aggregate of the present invention is not limited to a true spherical shape but also includes a substantially spherical shape and an ellipsoid.
The particle size of the spherical powder aggregate is 1.0 to 6.0 mm. In the present invention, the particle diameter of the spherical powder aggregate means the maximum diameter. Considering the use of this particle size for cigarette applications, an embodiment in which the particle diameter is 2.5 to 5.5 mm is preferable, and 3.0 to 4.5 mm is more preferable.
The “particle diameter” in the present invention means the maximum diameter.
The particle diameter of the spherical powder aggregate can be adjusted by adjusting the diameter of a nozzle used when a material containing microcrystalline cellulose, a binder, and ethanol is dropped in the powder when it is produced by the method described later.

As the microcrystalline cellulose used in the present invention, for example, α-cellulose obtained from a fibrous plant is partially depolymerized with an acid and purified, and a powdered one can be used. Specifically, commercially available endurance (trade name: Koyo Shokai) can be used. Microcrystalline cellulose having an average particle size of about 50 to 100 μm can be used.
In the spherical powder aggregate, the microcrystalline cellulose content may be 70 to 95% by weight, preferably 75 to 90% by weight, based on the total amount of the spherical powder aggregate.
When the content of microcrystalline cellulose is within the above range, a preferable value can be obtained as the breaking strength of the powder aggregate.

As the binder, water-soluble polymers such as starch, gelatin, gum arabic, polyvinyl alcohol, carboxymethyl cellulose and the like can be used. Among these, carboxymethylcellulose can be preferably used.
In the spherical powder aggregate, the binder content may be 10 to 20% by weight, preferably 13 to 18% by weight, based on the total amount of the spherical powder aggregate.
With such a content, a preferable value can be obtained as the breaking strength of the spherical powder aggregate.

The spherical powder aggregate of the present invention may contain sweeteners such as sucrose and flavoring agents. There is no restriction | limiting in particular as a taste agent, Single or mixtures, such as a sucralose, edible oil, an edible seasoning, an edible fragrance | flavor, an oral freshener, can be mentioned.
An example in which the content of such a flavoring agent in the spherical powder aggregate is 0.5 to 5.0% by weight with respect to the total amount of the spherical powder aggregate.

Further, the spherical powder aggregate of the present invention may contain a fragrance. It does not restrict | limit especially as a kind of fragrance | flavor, The existing fragrance | flavor can be used. Of these, powder flavors and oily flavors are suitable. Examples of the main powder flavor include powdered chamomile, fenugreek, menthol, mint, cinnamon and herbs. The main oily fragrances include lavender, cinnamon, cardamom, celery, clove, cascarilla, nutmeg, sandalwood, bergamot, geranium, honey essence, rose oil, vanilla, lemon, orange, mint, cinnamon skin, caraway, Examples include oils such as cognac, jasmine, chamomile, menthol, cashmere, ylang ylang, sage, spearmint, fennel, pimento, ginger, anise, corianda and coffee. These powdery fragrances and oily fragrances may be used alone or in combination. When using a powder fragrance | flavor, it is preferable that the particle size is 500 micrometers or less. It is preferred that the fragrance is substantially soluble in the liquid or oral cavity. The amount of the fragrance component added is preferably 10% by weight or less based on the microcrystalline cellulose.
When a liquid fragrance is used, the liquid fragrance can be added after the spherical powder aggregate of the present invention is produced. Since the spherical powder aggregate of the present invention is excellent in liquid absorbability, the liquid fragrance is efficiently absorbed into the powder aggregate. Moreover, it can be expected that the liquid fragrance once absorbed is difficult to ooze out of the powder aggregate. This is due to the fact that the powder agglomerates of the present invention are porous up to the inside thereof, which is a property that conventionally known cellulose granules do not have.

In the spherical powder aggregate, the total content of the microcrystalline cellulose and the binder can be 70.5 to 98% by weight, and preferably 85 to 92% by weight.
The weight ratio of microcrystalline cellulose to binder in the spherical powder aggregate can be 9: 1 to 7: 2.
The liquid content in the spherical powder aggregate is preferably 0.3 to 2.0% by weight, and more preferably 0.5 to 1.5% by weight. In the case of such a liquid content, it contributes to securing the breaking strength of the spherical powder aggregate described below.
In addition, when producing a spherical powder aggregate with the method demonstrated below, said liquid content means content of the sum total of water and ethanol.

The breaking strength of the powder aggregate of the present invention is 1.5 to 5.0 N as described above, and such a range of breaking strength means that the density of the powder aggregate is low. When a powder agglomerate having a low density and a large number of voids is produced, when a liquid fragrance is added after the powder agglomerate is produced, the liquid fragrance is efficiently absorbed into the powder agglomerate.
In order to achieve the above functions, the density of the powder aggregate of the present invention can be 0.2 to 0.8 g / cm ³ , and can be 0.3 to 0.6 g / cm ^3. preferable.
The density of the powder aggregate is obtained by the following method. A plurality of measurement samples are prepared (for example, 10 grains), the sample height of each sample is measured with a rheometer, and an average value of each numerical value is obtained to obtain an average diameter. The volume value calculated based on the average diameter is defined as the average volume. The average volume is obtained by dividing the average weight of each powder aggregate.
In the powder agglomerate of the present invention, the internal voids are not concentrated only in the central part but are uniformly present in the powder agglomerate, and there are crack-like voids on the surface. Can be easily absorbed and retained. Therefore, it can be expected that such a liquid substance does not ooze out from the powder aggregate during storage.
The spherical powder aggregate of the present invention can absorb liquid in an amount equal to or more than the weight of the powder aggregate.

The spherical powder aggregate of the present invention may be coated with a coating agent around it. Examples of such a coating agent include fats and oils having a melting point of 50 ° C. or higher. By containing fats and oils having a melting point of 50 ° C. or more, when a liquid fragrance is added to a spherical powder aggregate, it is possible to more effectively suppress oozing out to the surroundings.
Examples of the fats and oils having a melting point of 50 ° C. or higher include hardened oils having a melting point of 50 ° C. or higher.
The hardened oil is a processing oil obtained by adding hydrogen to a raw oil that is liquid at room temperature. In the present invention, a hardened oil having a melting point of 50 ° C. or higher is preferably used.
Examples of the hardened oil having a melting point of 50 ° C. or higher include edible hardened oils such as palm hardened oil, Hyelsin rapeseed hardened oil, rapeseed hardened oil, soybean hardened oil, animal hardened oil and fat.
Only 1 type may be used for the fats and oils whose melting | fusing point is 50 degreeC or more, and 2 or more types can also be mixed and used for it.
The method for coating the spherical powder aggregate of the present invention is not particularly limited, and a known method can be used.

<Fracture strength and measurement method>
The spherical powder aggregate of the present invention has a breaking strength of 1.5 to 5.0 N.
The measurement of the breaking strength is performed through the respective states shown in (a) to (d) of FIG. FIG. 2 schematically shows the relationship between the displacement (strain distance) and the stress at each time point.
FIG. 1A shows a state in which the rheometer contact is lowered and the contact is in contact with the spherical powder aggregate (at the time of FIG. 2A).
FIG. 1 (b) shows a state in which the rheometer contact continues to descend, and the spherical powder aggregate begins to be distorted, causing stress to the contact. As shown in FIG. 2B, the relationship between the strain distance and the stress is basically a linear line.
FIG. 1C shows a state in which the spherical powder aggregate is broken after being distorted to some extent. As shown in FIG. 2 (c), the maximum value (maximum load) of the stress immediately before breaking corresponds to the breaking strength, and the displacement at that time is defined as the breaking displacement. The stress is released immediately after the fracture and instantaneously approaches 0N.
FIG. 1D shows a state in which the contact piece descends continuously after the spherical powder aggregate is broken, and the broken pieces of the spherical powder aggregate broken in the above-mentioned (c) are broken more finely. ((D) of FIG. 2). As shown in FIG. 2 (d), the stress from the individual broken pieces is generated even at this stage.
FIG. 3 is a photograph showing the spherical powder aggregates in the states (a) and (b), the spherical powder aggregates in the state (c), and the spherical powder aggregates in the state (d). is there.

As a rheometer used for measuring the breaking strength, for example, CR-3000EX-S manufactured by Sun Scientific Co., Ltd. can be used. As the contact, one for compressive strength test is used.
The descending speed of the contact is 20.0 mm / min, and the particle size of the spherical powder aggregate applied to the rheometer is 1.0 to 6.0 mm.

The method for producing a spherical powder aggregate of the present invention includes the following steps.
A first step of dropping a slurry containing microcrystalline cellulose, a binder, and ethanol onto a vibrating powder to form a spherical intermediate composition composed of the slurry and the powder, and a first spherical intermediate composition A second step for reducing the liquid content to 2% by weight or less to obtain spherical powder aggregates.

In the first step, first, a slurry containing microcrystalline cellulose, a binder, and ethanol is prepared.
The slurry can be prepared by adding microcrystalline cellulose and a binder to ethanol. An appropriate disperser can be used when preparing the slurry.
The purity of ethanol is preferably 90% by weight or more, more preferably close to 100%. In other words, it is preferable that the amount of water contained as impurities is as small as possible, but the ethanol may be water-containing ethanol (water content is about 7% by weight) that is usually available.

The content of ethanol in the slurry can be 65 to 80% by weight based on the total amount of slurry (hereinafter also referred to as dropping slurry) when dripping onto the vibrating powder, and 70 to 70%. It is preferable that it is 75 weight% from a viewpoint of providing moderate viscosity to the slurry for dripping.

The content of the microcrystalline cellulose with respect to the total amount of the slurry for dripping can be 15 to 25% by weight, and 20 to 25% by weight can be used for the spherical powder aggregate that is the final product. It is preferable from the viewpoint of imparting an appropriate breaking strength and an appropriate density. Increasing the content of microcrystalline cellulose relative to the total amount of the slurry for dripping can increase the breaking strength of the spherical powder aggregate.

The content of the binder with respect to the total amount of the slurry for dripping can be 2 to 6% by weight, and 3 to 5% by weight is suitable for the spherical powder aggregate as the final product. It is preferable from the viewpoint of imparting breaking strength.
As the binder, water-soluble polymers such as starch, gelatin, gum arabic, polyvinyl alcohol, carboxymethyl cellulose and the like can be used. Among these, carboxymethylcellulose can be preferably used.

In the first step, the slurry containing the material is dropped into the vibrating powder (dropping in powder). About dripping, the aspect performed using the nozzle which has a suitable nozzle diameter can be mentioned. The amount of the powder with respect to the slurry to be dropped is adjusted so that the powder is excessive with respect to the slurry.
Examples of the powder to which the slurry is dropped include the same microcrystalline cellulose as the microcrystalline cellulose contained in the spherical powder aggregate. When microcrystalline cellulose is used as the powder to which the solution is added, the slurry and the powder become more familiar when the slurry is dropped into the powder, and the properties of the spherical powder aggregate that is the final product are stabilized. preferable. On the other hand, even if the nucleating agent contained in the slurry to be dropped and the powder at the dropping destination are different materials, the slurry and the powder are familiar with each other when the slurry is dropped, and a spherical powder aggregate is obtained. The material of the powder is not particularly limited as long as one spherical intermediate composition can be produced.

When the slurry is dropped onto the powder, the number of drops per unit time: 180 to 200 drops / minute, and the weight per drop: 25 to 30 mg / drop can be mentioned.
The slurry is dropped into the vibrating powder. By dropping the powder onto the vibrating powder, the slurry drops quickly absorb the powder surrounding the spherical shape while maintaining the spherical shape or the substantially spherical shape, and the first spherical intermediate composition is formed. The frequency of the vibration feeder is not particularly limited as long as the first spherical intermediate composition can maintain a spherical shape. For example, the vibration frequency can be 40 to 60 Hz.

As a means for vibrating the powder, a vibration feeder can be used. When using a vibrator that also serves as a conveying means, the nozzle used for dropping the slurry is fixed, and the powder at the dropping destination is vibrated while moving. An intermediate composition can be produced. In addition, when a vibration feeder that also serves as a conveying means is used, the produced spherical intermediate composition can be collected in a collection container disposed at the delivery end. In addition, the particle diameter of the spherical powder aggregate which is a final product can be adjusted by changing the diameter of the nozzle used for dripping the slurry.
The spherical intermediate composition is obtained by adding the powder at the dropping destination to the dropped slurry. The timing of dropping and the conveying speed by the vibration feeder that also serves as the conveying means can be adjusted as appropriate, and examples thereof include a speed at which a spherical intermediate composition is produced at 180 pieces / min.

In the second step, the spherical intermediate composition is dried so that its liquid content is reduced to 2% by weight or less. As a means for reducing the liquid content to 2% by weight or less, a hot air generator is used to apply hot air to the spherical intermediate composition and dry it. When drying with hot air, the spherical intermediate composition is preferably vibrated. By applying hot air while oscillating, the hot air is uniformly applied to the spherical intermediate composition, and the volatilization of ethanol does not occur. The vibration condition is not particularly limited, and examples thereof include a frequency of 20 to 50 Hz.
The liquid content is the total content of ethanol and water.
For example, when the spherical intermediate composition is dried while being vibrated, the spherical intermediate composition is preferably placed on a material having good air permeability such as a sieve.
The temperature of the hot air used for drying is preferably 85 to 95 ° C, more preferably about 88 to 92 ° C. In such a temperature range, ethanol can be quickly removed from the spherical intermediate composition, so that voids can be uniformly formed in the spherical intermediate composition.
If the liquid content in the spherical intermediate composition can be reduced to 2% by weight or less, the drying time is not limited. For example, the drying time is 3 to 10 minutes, preferably 4 to 8 minutes. it can.
Through the second step, a spherical powder aggregate having a liquid content of 2% by weight or less is obtained.
The liquid content of the obtained spherical powder aggregate has a great influence on the breaking strength.

About the obtained spherical powder aggregate, after the second step, only the powder aggregate having a predetermined particle diameter may be classified by a known classification means.
For example, the particle size can be classified into those having a desired particle size range, for example, a particle size range of 2.5 to 4.5 mm within a particle size range of 1.0 to 6.0 mm.
Moreover, you may include the process of adding a fragrance | flavor with respect to a spherical powder aggregate after said 2nd process. When adding a fragrance | flavor, the aspect which sprays a liquid fragrance | flavor using a spray, for example, and the aspect which impregnates a liquid fragrance | flavor using an impregnation method are mentioned.
Moreover, before and after the step of adding the fragrance, or without adding the step of adding the fragrance, a step of coating the spherical powder aggregate with the coating agent may be included. When the powder aggregate is coated with the coating agent after the fragrance is added, the permeation of the fragrance from the spherical powder aggregate is more effectively suppressed.

The breaking strength of the obtained spherical powder aggregate can be measured by the same method as described in 1 above. The breaking strength of the resulting spherical powder aggregate is 1.5 to 5.0 N. This breaking strength can be adjusted by adjusting the drying conditions in the second step.

Examples of the method of using the spherical powder aggregate of the present invention include use in a smoking article. More specifically, after a fragrance is supported on the powder aggregate, it is placed in a filter of a smoking article and used. Can be mentioned.
As a more specific aspect of the smoking article, a cigarette rod including cigarettes and a filter connected to an end portion of the cigarette rod via a chip paper, the filter is a spherical powder of the present invention An agglomerate and a filter section in which the spherical powder agglomerate is disposed, the filter section may be filled with a filter medium or may have a cavity shape, and the filter comprises a single filter section. A smoking article may be illustrated, which may comprise a plurality of filter sections.
According to such an embodiment, the spherical powder aggregate is retained in the filter when not in use. On the other hand, when the smoker applies the external force to the filter to break the spherical powder aggregate in the filter, the fragrance is included in the powder aggregate together with the mainstream smoke. Perfume can be delivered to the user.
In addition, the powder aggregate of the present invention is appropriately displaced at the time of breakage so that when an external pressure is applied to break it, it is broken within a range of pressure that is easily broken by humans, and a person can feel good splitting comfort. Therefore, the user can obtain a unique comfortable cracking feeling.

The present invention will be described more specifically with reference to examples. However, the present invention is not limited to the description of the following examples unless it exceeds the gist.

<Example 1>
A slurry was prepared as a material for producing a spherical powder aggregate.
To 730 parts by weight of ethanol (hydrous ethanol: water content of about 7% by weight), 40 parts by weight of hydroxypropyl methylcellulose and 230 parts by weight of microcrystalline cellulose (Endurance MCC VE-090: Koyo Shokai) were added, and a dispersing machine ( The slurry was stirred at 3000 to 5000 rpm for 5 minutes using a homodisper.

The obtained slurry for dropping was dropped as a powder onto a vibration feeder laid so that powdered microcrystalline cellulose (the same as that contained in the slurry) was present excessively with respect to the dropped slurry. The vibration feeder was vibrated at 55 Hz when the slurry was dropped.
A slurry dropping rate of 180-200 drops / min and a weight per drop of 25-30 mg / drop were applied.
When the slurry is continuously dropped into the vibratory feeder at the above speed, the dropped droplet is embedded in the powdered microcrystalline cellulose and simultaneously entrains the surrounding microcrystalline cellulose, instantly forming a spherical composition (spherical intermediate composition) Formed).
The spherical intermediate composition was conveyed from the upstream side to the downstream side while vibrating on the vibration feeder, and was collected in a collection container disposed at the downstream end.

As the next step, the obtained spherical intermediate composition was dried with hot air. When drying with hot air, the spherical intermediate composition was placed on a vibrating sieve, 90 ° C. was applied as the supply air temperature, and drying was performed for 5 minutes. During drying, the sieve on which the spherical intermediate composition was arranged was vibrated (phase: 8 (20 to 30 Hz)), and the intermediate spherical composition on the sieve was vibrated so that the hot air was uniformly applied.
By this drying, the liquid content of the spherical intermediate composition was reduced to 2% by weight or less to obtain a spherical powder aggregate.

<Measurement of fracture strength>
The obtained spherical powder aggregate was subjected to a test for measuring each state shown in FIG. 1 using a CR-3000EX-S manufactured by Rheometer (Sun Scientific).
20.0 mm / min was adopted as the descending speed of the contact during measurement with the rheometer. A contactor for compressive strength test was used.
In addition, as a comparative example, the breaking strength and the strain rate were also measured for a commercially available cellulose granule (Bisco Pearl A, Visco Pearl P: both manufactured by Rengo Co., Ltd.) and a molded product formed by a round machine by the method described later. .
For each sample of the spherical powder aggregate of the present invention, Viscopearl A, Viscopearl P, and molded product formed by a round machine, 5 to 10 samples were prepared, and the sample height (particle size) was measured by the rheometer. The maximum load (breaking strength), moving distance, and strain rate were measured. The strain rate indicates the ratio of the distance (movement distance) that the contact has moved by the time of destruction to the particle size of the particle. Show.
The results are shown in Table 1 below.

The viscopearl A used in the above-described test is made to cause gas foaming at the same time that the raw material in which the porosifying agent is added to the viscose is pressed down from the nozzle toward the acid bath and solidified into a spherical shape. Thus, the solidified raw material is made porous. A specific description of the method for producing such cellulose granules is in JP-A-2005-232379.
On the other hand, Visco Pearl P is not viscose but is granulated by adding a binder to wood pulp and various fibers.

About the molded object shape | molded with the round machine shown above, it produced with the following procedures.
First, in order to obtain a plate-like kneaded product to be set in a round machine, water (40 wt%), microcrystalline cellulose (57 wt%), HPMC (hydroxypropyl methylcellulose) (3 wt%) are mixed in a stirring mixer. It put in order and knead | mixed at room temperature for 1 hour.
Next, the obtained clay-like kneaded material was molded into a plate shape and set in a round machine.
The gap between the drum and the molding plate in the round making machine was set to 4.0 mm, and rounded granulation was performed to obtain a spheroidized clay-like kneaded product.
The obtained spheroidized clay-like kneaded product was exposed to hot air at 70 ° C. and dried to a water content of 0.8% by weight or less to obtain a spherical molded product as a final product.

As shown in the results of Table 1 above, unlike the powder agglomerates of the present invention, commercially available cellulose granules and molded products formed with a round machine are similar in particle size to the powder agglomerates of the present invention. Despite this, the load required to break was very large and could not be easily broken by human fingers. On the other hand, the spherical powder aggregate of the present invention has a small load required for breaking and a small strain rate, so it can be easily broken with a human finger and gives a comfortable cracking comfort to the user. It was possible. Furthermore, after breaking the powder aggregate of the present invention, it was broken down to a fine powder as shown in (d) through FIG.

FIGS. 4 to 7 show the relationship between the load and the elapsed time during the measurement with the rheometer, which were performed to obtain the results shown in Table 1. FIG. 4 to 7, the vertical axis represents load (N) and the horizontal axis represents time (seconds).
From FIG. 4 (result of the powder aggregate of the present invention), when the maximum load is applied, the spherical powder aggregate breaks once, but each cracked piece is soft, slightly broken, and pressed by the contactor. You can see how it collapses with weak force. The strain is very small, and the contact breaks in about 0.5 to 1.0 seconds after the contact with the powder aggregate.
It can be seen from FIG. 5 (result of a molded product formed by a round machine) that the maximum load is very large (about 38 to about 60 N) and is not hard enough to be broken by a human finger. When broken, it breaks into pieces, but most of the pieces are about 1 second after crushing, and the size is such that they do not touch the contacts. From there, debris was further pushed by the contact, but it was found that each piece did not collapse and had some strength.
It can be seen from FIG. 6 (results of Viscopearl A) that the maximum load is very large (about 30 N). The object was deformed while being pushed until it broke after touching the contact, and it was in a state of being crushed rather than broken.
From FIG. 7 (result of viscopearl P), it can be seen that the maximum load is larger than that of viscopearl A. It was also found that the object continued to be deformed by being pushed after touching the contact (the load continued to be applied).

<Liquid absorbency>
Using the powder aggregate of the present invention and a molded product obtained using the above-mentioned round machine as a comparative example, a test for confirming the liquid absorbency was performed.
1.0 g of each sample was weighed into a beaker, and an excessive amount of water or oil (medium chain fatty acid triglyceride: 2-3 g) was added dropwise to the sample in the beaker. After 30 seconds, the granule surface was wiped with Kimwipe and weighed. The amount of adsorption per gram of each granule is shown in Table 2 below.

From the results shown in Table 2, the powder aggregate of the present invention was excellent in both water absorbency and liquid absorbency, and was able to absorb a liquid having an equal volume or more by weight. On the other hand, in a molded product obtained using a conventional round machine, no liquid absorbency up to that point was obtained. This is considered to be due to the difference in the amount of voids in the granules and the state of the voids.

<Measurement of density>
The density of the spherical aggregate formed by the powder aggregate of the present invention and the above round machine was measured. Ten spherical powder aggregates prepared by the respective production methods were sampled, and the average diameter and average weight were determined. The average volume of the spherical powder aggregate was calculated from the average diameter, and the average density was calculated by calculating (average weight) ÷ (average volume).

-Powder aggregate diameter of the present invention (1 grain): 3.70 mm (10 grain diameter = 3.70 cm)
Volume (1 grain): 0.02650 cm ³
Density: 0.48 g / cm ³

-Diameter of spherical molded product formed by a round machine (1 grain): 3.65 mm (10 grain diameter = 3.65 cm)
Volume (1 grain): 0.02544 cm ³
Density: 1.29 g / cm ³

As shown by the calculation results, there was a large difference in density between the powder aggregate of the present invention and the spherical molded product formed by the round machine. This indicates that a difference in the amount of voids present in the granules and the state of voids occurred due to the production method, and the difference in the state of presence caused the powder aggregate of the present invention to be easily broken by human fingers. It has a strength and becomes a spherical powder aggregate in which fine particles are formed instead of a large lump after breaking.

The spherical powder aggregate of the present invention has such a breaking strength that it can be easily broken by a human finger, and fine particles of the spherical powder aggregate are generated after breaking. Therefore, when the spherical powder aggregate of the present invention is placed in a filter used in a smoking article such as a cigarette and having a passage to the mouth end inside, or in a filter part near the mouthpiece, the smoker's Fine particles destroyed by the finger can easily reach the smoker's mouth. Thereby, the delivery efficiency of the powdery flavor source to a smoker improves.
In addition, the spherical powder aggregate of the present invention has good absorbability when a liquid is added, and it can be expected to suppress subsequent bleeding.
As a result, when the liquid fragrance is absorbed in the spherical powder aggregate of the present invention, for example, it can be expected to serve as a fragrance carrier or flavor retainer, and this can be placed in the filter or between the filter segments of the smoking article. By destroying this during smoking, it can be expected that the flavor component that has been carried or held is released to the outside of the powder aggregate.
Furthermore, according to the method for producing a spherical powder aggregate of the present invention, it has a breaking strength that can be easily broken from a human finger and an appropriate displacement at the time of breaking so that a person can feel a good feeling of splitting. It is possible to provide a spherical powder agglomerate that later produces fine particles rather than large lumps. Furthermore, according to this production method, a conventionally known step of performing a chemical reaction such as a step of performing gas foaming to obtain a porous structure is unnecessary, and stable production by a machine is easy. is there.

1: Contact of rheometer 2: Spherical powder aggregate 3: Powder aggregate after fracture

Claims

A spherical powder aggregate composed of a material containing microcrystalline cellulose and a binder, wherein the particle diameter of the powder aggregate is 1.0 to 6.0 mm;
A spherical powder aggregate having a fracture strength of 1.5 to 5.0 N and a strain rate of 5.0 to 15.0%.
The spherical powder aggregate according to claim 1, wherein the density of the powder aggregate is 0.2 to 0.8 g / cm 3 .
The spherical powder aggregate according to claim 1 or 2, wherein the binder is at least one water-soluble polymer selected from starch, gelatin, gum arabic, polyvinyl alcohol and carboxymethylcellulose.
The spherical powder aggregate according to any one of claims 1 to 3, wherein the total content of microcrystalline cellulose and binder in the powder aggregate is 70.5 to 98 wt%.
The spherical powder aggregate according to any one of claims 1 to 4, wherein the powder aggregate contains a fragrance.
A first step of dropping a slurry containing microcrystalline cellulose, a binder and ethanol onto a vibrating powder to form a spherical intermediate composition composed of the slurry and the powder, and a liquid content of the spherical intermediate composition A method for producing a spherical powder agglomerate, comprising a second step of drying so as to reduce the content to 2% by weight or less.
The method for producing a spherical powder aggregate according to claim 6, wherein the powder is microcrystalline cellulose.
The method for producing a spherical powder aggregate according to claim 6 or 7, wherein the binder is at least one water-soluble polymer selected from starch, gelatin, gum arabic, polyvinyl alcohol and carboxymethylcellulose.
The method for producing a spherical powder aggregate according to any one of claims 6 to 8, wherein the content of microcrystalline cellulose in the slurry is 15 to 25% by weight.
The method for producing a spherical powder aggregate according to any one of claims 6 to 9, wherein the drying in the second step is performed by hot air drying.
The method for producing a spherical powder aggregate according to any one of claims 6 to 10, wherein the drying in the second step is performed while vibrating the spherical intermediate composition.