TWI642366B - Spherical powder aggregate and method for manufacturing the same - Google Patents
Spherical powder aggregate and method for manufacturing the same Download PDFInfo
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Abstract
本發明提供包含微結晶纖維素及黏結劑,且粉末凝聚體之粒徑為1.0至6.0mm,破壞強度為1.5至5.0N,應變率為5.0至15.0%之球狀之粉末凝聚體及其製造方法。 The present invention provides a spherical powder aggregate comprising microcrystalline cellulose and a binder, and the powder agglomerate has a particle diameter of 1.0 to 6.0 mm, a breaking strength of 1.5 to 5.0 N, and a strain rate of 5.0 to 15.0%, and a production thereof. method.
Description
本發明有關球狀之粉末凝聚體及其製造方法。 The present invention relates to a spherical powder aggregate and a method for producing the same.
已知藉由抽吸濾嘴內的粉末,享受味道或香氣,或其兩者之香煙。例如專利文獻1中,揭示於濾嘴內之腔室收容粒狀物質,透過流體通路而將粒狀物質供給至送出端之內容。 It is known to enjoy a taste or aroma, or both, by aspirating the powder in the filter. For example, Patent Document 1 discloses that a granular substance is accommodated in a chamber in a filter, and a granular substance is supplied to a delivery end through a fluid passage.
此外,專利文獻2中,關於煙草製品的技術,已記載將天然多糖類或其衍生物所構成之固體粒子,封入香料之內容。 Further, in Patent Document 2, as for the technique of tobacco products, the solid particles composed of natural polysaccharides or derivatives thereof are encapsulated in the contents of the perfume.
專利文獻3中,係記載為了從主流煙將至少一種煙成分除去而配置在濾嘴內之包含煙草粒子之煙草珠粒。 Patent Document 3 describes tobacco beads containing tobacco particles which are disposed in a filter in order to remove at least one smoke component from mainstream smoke.
專利文獻4中,係記載在濾嘴部組裝入持續釋出性的液體送出材料之吸煙物品。專利文獻4所記載的液體釋出材料係含有包含基質形成聚合物與塑化劑之聚合物基質,作為形成基質之聚合物,係已記載有海藻酸以及果膠。 Patent Document 4 describes a smoking article in which a liquid discharge material of a continuous release property is incorporated in a filter unit group. The liquid release material described in Patent Document 4 contains a polymer matrix containing a matrix-forming polymer and a plasticizer. As the polymer forming the matrix, alginic acid and pectin have been described.
[專利文獻1]日本特開昭60-192581號公報 [Patent Document 1] Japanese Laid-Open Patent Publication No. 60-192581
[專利文獻2]日本特開昭64-27461號公報 [Patent Document 2] Japanese Patent Laid-Open No. 64-27461
[專利文獻3]日本特表2008-531008號公報 [Patent Document 3] Japanese Patent Publication No. 2008-531008
[專利文獻4]日本特表2014-532435號公報 [Patent Document 4] Japanese Patent Publication No. 2014-532435
專利文獻1及2所述之發明係使用粉末作為香料自身或香料之擔體。 The invention described in Patent Documents 1 and 2 uses a powder as a carrier of the fragrance itself or a fragrance.
但是,該等之發明所使用之粉末,任一者均非由其自身所成形者,該等之專利文獻中並未記載破壞後形成細粒粉末之球狀之粉末凝聚體。此外,專利文獻1及2中,並未記載作為粉末原料之微結晶纖維素。 However, none of the powders used in the inventions are formed by themselves, and the patent documents do not describe the spherical powder aggregates which form fine powder after the destruction. Further, in Patent Documents 1 and 2, microcrystalline cellulose as a powder raw material is not described.
專利文獻3中,雖然記載有煙草珠粒,但如上述般在該等中係含有作為必要成份之煙草粒子。專利文獻3中雖然記載微結晶纖維素作為構成煙草珠粒時之任意的材料,但並未記載以微結晶纖維素作為主成分,而不含有煙草粒子的珠粒。在專利文獻3中,係記載將材料進行壓出成形而得到煙草珠粒。 In Patent Document 3, tobacco beads are described, but as described above, tobacco particles as essential components are contained therein. In Patent Document 3, microcrystalline cellulose is described as an arbitrary material when constituting tobacco beads, but beads containing microcrystalline cellulose as a main component and not containing tobacco particles are not described. Patent Document 3 describes that a material is subjected to extrusion molding to obtain tobacco beads.
另外,若將微結晶纖維素以打錠機壓縮,則粒子互糾結並可容易成型,故使用此作為錠劑等之核劑係已廣為人知。 Further, when the microcrystalline cellulose is compressed by a tableting machine, the particles are entangled and can be easily molded. Therefore, it has been widely known to use a nucleating agent such as a tablet.
此外,在食品等領域所使用之粉末的一般成形法,已 知有:包含濕式壓出造粒步驟以及整粒步驟之方法,及使用製丸粒機而將粉末成形為球狀而製得成形物之方法。 Further, in a general molding method of a powder used in the field of foods and the like, a method including a wet extrusion granulation step and a granulation step, and a powder pelletized machine are used to form a powder into a spherical shape. Method of forming a product.
但是,以往所知之食品等領域所使用之一般的粉末之成形法、或使用打錠法所得之成形物係非常硬,難以藉由人的手指破壞成細粒狀。因此,使用壓出成形之專利文獻3所記載之煙草珠粒,可預想無法容易地藉由人的手指進行破壞。原本在專利文獻3中係完全未記載將煙草珠粒藉由人的手指進行破壞。 However, the conventional powder molding method used in the field of foods and the like, or the molded article obtained by the tableting method is very hard, and it is difficult to break into fine particles by human fingers. Therefore, it is expected that the tobacco beads described in Patent Document 3 by extrusion molding cannot be easily broken by a human finger. Originally, in Patent Document 3, it is not described at all that the tobacco beads are destroyed by a human finger.
其次,在專利文獻2或3所記載的發明中,係設想到擔載液體香料者,未特別記載有關擔載液體香料之後,液體香料從擔體滲出的問題。有關此點,在專利文獻3係雖然記載在煙草珠粒的基質中貯存揮發性液體化合物,並延長保存期間,但此係與液體香料之滲出為不同的問題。 Next, in the invention described in Patent Document 2 or 3, it is assumed that the person who carries the liquid fragrance does not specifically describe the problem that the liquid fragrance oozes out from the support after the liquid fragrance is carried. In this regard, in Patent Document 3, it is described that the volatile liquid compound is stored in the matrix of the tobacco beads, and the storage period is prolonged, but this is different from the oozing of the liquid fragrance.
另一方面,在專利文獻4中雖然記載使用者施加指定的力道,以將封閉在香味送出材料的基質構造中的香味組成物,從基質構造釋出,但形成基質構造並非粉末,離子交聯為必要的聚合物。此外,並未記載藉由使用者的手破壞該香味送出材料之事。 On the other hand, in Patent Document 4, it is described that the user applies a specified force to release the flavor composition enclosed in the matrix structure of the flavor delivery material from the matrix structure, but the matrix structure is not powder, ion crosslinking Is the necessary polymer. Further, there is no description of the fact that the fragrance delivery material is destroyed by the user's hand.
由於該等之情事,本發明之課題係提供一種可適用於吸煙物品等,具有可藉由人的手指破壞而形成細粒狀程度之硬度、與用以讓使用者輕鬆地弄碎的感覺之適當的破壞時位移,同時並添加液體時的吸收性為良好之球狀之粉末凝聚體、以及該球狀之粉末凝聚體之製造方法。 In view of such circumstances, the subject of the present invention is to provide a smoking article or the like which has a hardness which can be broken by a human finger to form a fine grain and a feeling of being easily broken by a user. A method of producing a spherical agglomerate of powder and a method of producing the spherical powder agglomerate, which are suitable for displacement at the time of destruction, and at the same time, when the liquid is added, the absorbability is good.
本案發明者積極研究的結果,得知一種球狀之粉末凝聚體,其係由包含微結晶纖維素以及黏結劑之材料所構成,且,粉末凝聚體之粒徑為1.0至6.0mm,破壞強度為1.5至5.0N,應變率為5.0至15.0%,可容易地藉由人的手指破壞,同時在破壞後產生細粒狀的粉末。 As a result of active research by the inventors of the present invention, a spherical powder agglomerate composed of a material containing microcrystalline cellulose and a binder is known, and the particle size of the powder agglomerate is 1.0 to 6.0 mm, and the breaking strength is obtained. The strain rate is from 5.0 to 5.0 N, and the strain rate is from 5.0 to 15.0%, which can be easily broken by a human finger while producing a fine-grained powder after the destruction.
進一步,具有上述之構成之球狀之粉末凝聚體,係液體之吸收性優異。 Further, the spherical powder aggregate having the above configuration is excellent in liquid absorbability.
此外,本案發明者積極研究的結果,得知一種球狀之粉末凝聚體之製造方法,其係藉由包含:將包含微結晶纖維素,黏結劑以及乙醇之漿體滴入於振動中的粉體,而形成由漿體與粉體所構成之球狀中間組成物之第一步驟;以及,以球狀中間組成物的液體含量減少至2重量%以下的方式使其乾燥之第二步驟;可獲得具有上述物性之球狀之粉末凝聚體。 Further, as a result of active research by the inventors of the present invention, a method for producing a spherical powder agglomerate is known which comprises: a powder which is dropped into a vibration by a slurry containing microcrystalline cellulose, a binder, and ethanol. a first step of forming a spherical intermediate composition composed of a slurry and a powder; and a second step of drying the liquid content of the spherical intermediate composition to 2% by weight or less; A spherical powder agglomerate having the above physical properties can be obtained.
亦即,本發明係如下述。 That is, the present invention is as follows.
[1]一種球狀之粉末凝聚體,係包含微結晶纖維素以及黏結劑,粉末凝聚體之粒徑為1.0至6.0mm,粉末凝聚體之破壞強度為1.5至5.0N,應變率為5.0至15.0%。 [1] A spherical powder agglomerate comprising microcrystalline cellulose and a binder, the particle size of the powder agglomerate is 1.0 to 6.0 mm, the breaking strength of the powder agglomerate is 1.5 to 5.0 N, and the strain rate is 5.0 to 15.0%.
[2]如[1]所述之球狀之粉末凝聚體,其中,前述粉末凝聚體之密度為0.2至0.8g/cm3。 [2] The spherical powder agglomerate according to [1], wherein the powder agglomerate has a density of 0.2 to 0.8 g/cm 3 .
[3]如[1]或[2]所述之球狀之粉末凝聚體,其中,前述黏結劑係選自澱粉、明膠、阿拉伯膠、聚乙烯醇以及羧甲基纖 維素之1種以上之水溶性聚合物。 [3] The spherical powder aggregate according to the above [1], wherein the binder is one or more selected from the group consisting of starch, gelatin, gum arabic, polyvinyl alcohol, and carboxymethyl cellulose. Water soluble polymer.
[4]如[1]至[3]中任一項所述之球狀之粉末凝聚體,其中,於前述粉末凝聚體中之微結晶纖維素以及黏結劑之合計之含量為70.5至98重量%。 [4] The spherical powder agglomerate according to any one of [1] to [3] wherein the total content of the microcrystalline cellulose and the binder in the powder aggregate is 70.5 to 98 by weight. %.
[5]如[1]至[4]中任一項所述之球狀之粉末凝聚體,其中,前述粉末凝聚體含有香料。 [5] The spherical powder aggregate according to any one of [1] to [4] wherein the powder agglomerate contains a fragrance.
[6]一種球狀之粉末凝聚體之製造方法,係包含:將包含微結晶纖維素,黏結劑以及乙醇之漿體滴入於振動中的粉體,形成由漿體與粉體所構成之球狀中間組成物之第一步驟;以及以球狀中間組成物的液體含量減少至2重量%以下的方式使其乾燥之第二步驟。 [6] A method for producing a spherical powder agglomerate, comprising: a powder comprising a slurry of microcrystalline cellulose, a binder, and ethanol dropped into a vibration to form a slurry and a powder. a first step of the spherical intermediate composition; and a second step of drying the liquid content of the spherical intermediate composition to less than 2% by weight.
[7]如[6]所述之球狀之粉末凝聚體之製造方法,其中,前述粉體為微結晶纖維素。 [7] The method for producing a spherical powder aggregate according to [6], wherein the powder is microcrystalline cellulose.
[8]如[6]或[7]所述之球狀之粉末凝聚體之製造方法,其中,前述黏結劑係選自澱粉、明膠、阿拉伯膠、聚乙烯醇以及羧甲基纖維素之1種以上之水溶性聚合物。 [8] The method for producing a spherical powder agglomerate according to [6], wherein the binder is selected from the group consisting of starch, gelatin, gum arabic, polyvinyl alcohol, and carboxymethyl cellulose. More than one water soluble polymer.
[9]如[6]至[8]中任一項所述之球狀之粉末凝聚體之製造方法,其中,於前述漿體中之微結晶纖維素之含量為15至25重量%。 [9] The method for producing a spherical powder aggregate according to any one of [6] to [8] wherein the content of the microcrystalline cellulose in the slurry is 15 to 25% by weight.
[10]如[6]至[9]中任一項所述之球狀之粉末凝聚體之製造方法,其中,於前述第二步驟中之乾燥係藉由熱風乾燥進行。 [10] The method for producing a spherical powder agglomerate according to any one of [6] to [9] wherein the drying in the second step is performed by hot air drying.
[11]如[6]至[10]中任一項所述之球狀之粉末凝聚體之製造方法,其係使球狀中間組成物一邊振動一邊進行前述第二 步驟中之乾燥。 [11] The method for producing a spherical powder aggregate according to any one of [6] to [10] wherein the spherical intermediate composition is dried while being vibrated in the second step.
本發明之球狀之粉末凝聚體係其破壞強度可容易地藉由人的手指破壞,且具有用以讓人可感受到良好的破壞感覺的適當破壞時位移。因此,將本發明之球狀之粉末凝聚體配置在如香煙的吸煙物品所使用之濾嘴等時,藉由吸煙者的手指破壞球狀之粉末凝聚體時,在內包有香料的情況,可將主流煙與在粉末凝聚體所內包之香料一起送達至使用者。此外,添加液體時的吸收性良好。藉此,使本發明之球狀之粉末凝聚體吸收液體香料時,可期待例如作為香料擔載體或香味保持劑之角色。 The spherical powder agglomeration system of the present invention can be easily broken by human fingers and has a suitable breakage displacement for allowing a good feeling of destruction to be felt. Therefore, when the spherical powder aggregate of the present invention is disposed in a filter or the like used for a smoking article of a cigarette, when the spherical powder aggregate is destroyed by the finger of the smoker, the fragrance is contained therein. The mainstream smoke can be delivered to the user along with the perfume contained in the powder agglomerate. Moreover, the absorbability at the time of adding a liquid is favorable. Thereby, when the spherical powder aggregate of the present invention absorbs the liquid fragrance, it is expected to function as a fragrance carrier or a flavor retention agent, for example.
此外,依據本發明之球狀之粉末凝聚體之製造方法,可提供粉末凝聚體,其係具有可容易地藉由人的手指破壞,及用以讓人可感受到良好的破壞感覺的適當的破壞時位移。 Further, according to the method for producing a spherical powder agglomerate of the present invention, it is possible to provide a powder agglomerate which is suitable for being easily broken by a human finger and for allowing a person to feel a good feeling of destruction. Displacement when broken.
1‧‧‧流變計之接觸體 1‧‧‧ Contactor of rheometer
2‧‧‧球狀之粉末凝聚體 2‧‧‧Spherical powder aggregates
3‧‧‧破壞後之粉末凝聚體 3‧‧‧After the destruction of the powder aggregates
第1圖係顯示測定球狀之粉末凝聚體之破壞強度時之粉末凝聚體之各狀態圖。 Fig. 1 is a view showing states of the powder agglomerates when the breaking strength of the spherical powder aggregates is measured.
第2圖係顯示測定球狀之粉末凝聚體之破壞強度時之流變計之接觸體之位移與應力之關係的概略圖。 Fig. 2 is a schematic view showing the relationship between the displacement of the contact body of the rheometer and the stress when the breaking strength of the spherical powder aggregate is measured.
第3圖係表示球狀之粉末凝聚體之破壞前與破壞後之各狀態圖(照片)。 Fig. 3 is a view showing each state (photograph) of the spherical powder aggregate before and after the destruction.
第4圖係顯示藉由流變計測定實施例之粉末凝聚體時 之荷重與經過時間之關係圖。 Fig. 4 is a graph showing the relationship between the load and the elapsed time when the powder agglomerates of the examples were measured by a rheometer.
第5圖係顯示藉由流變計測定以製丸粒機所形成之成形物時之荷重與經過時間之關係圖。 Fig. 5 is a graph showing the relationship between the load and the elapsed time when a molded article formed by a pelletizer is measured by a rheometer.
第6圖係顯示藉由流變計測定Viscopearl A時之荷重與經過時間之關係圖。 Figure 6 is a graph showing the relationship between the load and the elapsed time when the Viscopearl A is measured by a rheometer.
第7圖係顯示藉由流變計測定Viscopearl P時之荷重與經過時間之關係圖。 Figure 7 is a graph showing the relationship between the load and the elapsed time when the Viscopearl P is measured by a rheometer.
以下,針對本發明表示實施形態以及例示物等詳細說明,但本發明不限於以下之實施形態以及例示物等,在不超出本發明之要旨之範圍可任意地變更實施。 In the following, the present invention is not limited to the embodiments and the examples, and the present invention is not limited to the embodiments and the examples, and the invention can be arbitrarily changed without departing from the scope of the invention.
本發明之球狀之粉末凝聚體為由包含微結晶纖維素以及黏結劑之材料所構成,且,粒徑為1.0至6.0mm,藉由流變計(SUN科學公司製之CR-3000EX-S)於MODE3之條件下以測力器(load cell)最大應力為200N,桌台之移動速度為以20.0mm/min之條件測定時的破壞強度為1.5至5.0N。測試時使用壓縮強度試驗用之接觸體。 The spherical powder aggregate of the present invention is composed of a material containing microcrystalline cellulose and a binder, and has a particle diameter of 1.0 to 6.0 mm, and is a rheometer (CR-3000EX-S manufactured by SUN Scientific Co., Ltd.). Under the condition of MODE3, the maximum stress of the load cell is 200N, and the breaking speed of the table is 20.0mm/min, and the breaking strength is 1.5 to 5.0N. The contact body for the compressive strength test was used for the test.
上述之破壞強度,就藉由人的手所破壞時之適度的破壞強度而言,以2.0至4.0N為更佳。 The above-mentioned breaking strength is preferably 2.0 to 4.0 N in terms of moderate breaking strength when the human hand is broken.
此外,本發明之球狀之粉末凝聚體之應變率為5.0至15.0%。在此所謂之應變率,係在藉由上述之流變計測定破壞強度時,將接觸體與粉末凝聚體接觸後至粉末凝聚體被破壞為止所移動的距離,除以粉末凝聚體之粒徑後之值,乘以100所得之數值,亦稱為破壞時位移。此應變率愈小, 粉末凝聚體之壓縮寬度愈小的狀態會引起破壞。 Further, the spherical powder agglomerates of the present invention have a strain rate of 5.0 to 15.0%. Here, the strain rate is a distance moved by contact between the contact body and the powder agglomerate until the powder aggregate is destroyed, and the particle size of the powder agglomerate is measured when the fracture strength is measured by the rheometer described above. The value obtained by multiplying by 100 is also called the displacement at break. The smaller the strain rate, the smaller the compression width of the powder agglomerates causes damage.
球狀之粉末凝聚體之應變率可舉例5.0至12.0%之態樣。 The strain rate of the spherical powder agglomerates can be exemplified in the range of 5.0 to 12.0%.
本發明所謂之粉末凝聚體,係指由構成其之材料所構成的結晶粒子聚集而形成一個球狀塊者。例如,藉由本發明之製造方法所製作之粉末凝聚體,係將包含乙醇之漿體與粉體之混合物,如後述般,在滴入粉中而造粒後經過燥步驟而使乙醇揮發所得之物,在其過程將溶解於漿體之微結晶纖維素及黏結劑等作為結晶粒子等而析出及凝集,形成球狀塊者。由於如此之形成,故本發明之粉末凝聚體為多孔質。 The term "powder aggregate" as used in the present invention means a group of crystal particles composed of materials constituting the same to form a spherical block. For example, the powder agglomerate produced by the production method of the present invention is a mixture of a slurry containing a mixture of ethanol and a powder, which is granulated by dropping into a powder as described later, and then evaporating the ethanol by a drying step. In the process, microcrystalline cellulose, a binder, and the like which are dissolved in the slurry are precipitated and aggregated as crystal particles or the like to form a spherical block. Due to such formation, the powder agglomerates of the present invention are porous.
在本發明之球狀之粉末凝聚體中之「球狀」,不限於真球,亦包含略球狀物及橢圓體。 The "spherical shape" in the spherical powder aggregate of the present invention is not limited to a true ball, and includes a slightly spherical shape and an ellipsoid.
球狀之粉末凝聚體之粒徑為1.0至6.0mm。於本發明中,球狀之粉末凝聚體之粒徑係意指最大徑。此粒徑考量到使用於如香煙用途時,較佳為2.5至5.5mm之態樣,更佳為3.0至4.5mm。 The spherical powder agglomerates have a particle diameter of 1.0 to 6.0 mm. In the present invention, the particle size of the spherical powder agglomerates means the largest diameter. The particle size is preferably from 2.5 to 5.5 mm, more preferably from 3.0 to 4.5 mm, when used for cigarette use.
於本發中之「粒徑」係意指最大徑。 "Particle size" in this context means the largest diameter.
球狀之粉末凝聚體之粒徑係在藉由後述的方法製作時,可藉由調整將包含微結晶纖維素、黏結劑、乙醇之材料滴入於粉中時所使用之噴嘴的口徑來調整。 When the particle diameter of the spherical powder agglomerate is produced by a method described later, it can be adjusted by adjusting the diameter of a nozzle used when a material containing microcrystalline cellulose, a binder, and ethanol is dropped into the powder. .
本發明所使用之微結晶纖維素係例如可使用從纖維性植物所得之α-纖維素以酸部分解聚合而精製者,且為粉末者。具體而言,可使用市售之ENDURANCE(商 品名:光洋商會)。微結晶纖維素可使用平均粒徑為50至100μm左右者。 The microcrystalline cellulose used in the present invention can be obtained by, for example, partially depolymerizing an α-cellulose obtained from a fibrous plant with an acid, and is a powder. Specifically, a commercially available ENDURANCE (trade name: Koyo Chamber of Commerce) can be used. As the microcrystalline cellulose, those having an average particle diameter of about 50 to 100 μm can be used.
於球狀之粉末凝聚體中,相對球狀之粉末凝聚體之全量,微結晶纖維素之含量可舉例70至95重量%之態樣,較佳為75至90重量%之態樣。 In the spherical powder agglomerate, the content of the microcrystalline cellulose may be, for example, 70 to 95% by weight, preferably 75 to 90% by weight, based on the total amount of the spherical powder agglomerates.
微結晶纖維素之含量為上述範圍時,可得到作為粉末凝聚體之破壞強度較佳之值。 When the content of the microcrystalline cellulose is in the above range, a value which is preferable as a breaking strength of the powder agglomerate can be obtained.
前述黏結劑可使用澱粉、明膠、阿拉伯膠、聚乙烯醇、羧甲基纖維素等水溶性聚合物。其中,較佳可使用羧甲基纖維素。 As the above-mentioned binder, a water-soluble polymer such as starch, gelatin, gum arabic, polyvinyl alcohol or carboxymethyl cellulose can be used. Among them, carboxymethylcellulose is preferably used.
於球狀之粉末凝聚體中,相對球狀之粉末凝聚體之全量,黏結劑之含量可舉例10至20重量%之態樣,較佳為13至18重量%之態樣。 In the spherical powder agglomerate, the content of the binder may be, for example, 10 to 20% by weight, preferably 13 to 18% by weight, based on the total amount of the spherical powder agglomerates.
為如此之含量時,可得到作為球狀之粉末凝聚體之破壞強度較佳之值。 When it is such a content, the breaking strength of the spherical powder aggregate can be obtained as a preferable value.
本發明之球狀之粉末凝聚體中可含有蔗糖等甜味劑或呈味劑。呈味劑無特別限制,可舉例蔗糖素(sucralose)、食用油、食用調味料、食用香料、口腔清涼劑等單獨物或混合物。 The spherical powder aggregate of the present invention may contain a sweetener such as sucrose or a flavoring agent. The flavoring agent is not particularly limited, and examples thereof include a single substance or a mixture of sucralose, edible oil, edible seasoning, flavorant, and oral cooling agent.
相對球狀之粉末凝聚體之全量,於球狀之粉末凝聚體中之如此之呈味劑之含量可舉例0.5至5.0重量%之態樣。 The content of such a flavoring agent in the spherical powder agglomerate may be, for example, 0.5 to 5.0% by weight in terms of the total amount of the spherical powder agglomerates.
此外,本發明之球狀之粉末凝聚體中可含有香料。香料的種類並無特別限制,可使用既有的香料。其中,適合為粉末香料以及油性香料。主要的粉末香料可 舉例將洋甘菊、葫蘆巴、薄荷腦、薄荷、肉桂、香草等作為粉末者。此外,主要的油性香料可舉例熏衣草、肉桂、荳蔻、芹菜、丁香、苦香樹、肉荳蔻、檀香、佛手柑、天竺葵、蜂蜜精華、玫瑰精油、香草、檸檬(Lemon)、柑橘(Orange)、薄荷、肉桂、香菜、白蘭地、茉莉、洋甘菊、薄荷醇、決明子、依蘭、鼠尾草、綠薄荷、茴香、青椒、生薑、茴香、香菜、咖啡等之油。該等之粉末香料以及油性香料,可單獨使用,此外亦可混合而使用。使用粉末香料時,其粒徑較佳為500μm以下。香料較佳為液體或口腔內可實質溶解者。香料成分的添加量,相對於微結晶纖維素,較佳為10重量%以下。 Further, the spherical powder agglomerates of the present invention may contain a fragrance. The type of the fragrance is not particularly limited, and an existing fragrance can be used. Among them, suitable for powder flavors and oily flavors. The main powder flavors can be exemplified by chamomile, fenugreek, menthol, mint, cinnamon, vanilla, and the like. In addition, the main oily flavors are lavender, cinnamon, cardamom, celery, clove, bitter tree, nutmeg, sandalwood, bergamot, geranium, honey extract, rose oil, vanilla, lemon, citrus ( Orange), mint, cinnamon, coriander, brandy, jasmine, chamomile, menthol, cassia seed, ylang-ylang, sage, spearmint, fennel, green pepper, ginger, fennel, coriander, coffee, etc. These powder flavors and oily flavors may be used singly or in combination. When a powder flavor is used, the particle diameter thereof is preferably 500 μm or less. The perfume is preferably a liquid or a substance that is substantially soluble in the oral cavity. The amount of the flavor component added is preferably 10% by weight or less based on the microcrystalline cellulose.
使用液體者作為香料時,可於製作本發明之球狀之粉末凝聚體之後添加液體香料。本發明之球狀之粉末凝聚體由於液體之吸收性優異,故液體香料效率佳地被吸收至粉末凝聚體內。此外,可期待暫時被吸收之液體香料難以滲出至粉末凝聚體之外部。此係本發明之粉末凝聚體其至內部為止之多孔質所致者,且不具有以往所知之纖維素顆粒的性質。 When a liquid is used as the fragrance, 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 flavor is efficiently absorbed into the powder aggregate. Further, it is expected that the liquid fragrance temporarily absorbed is hard to bleed out to the outside of the powder agglomerate. This is a result of the fact that the powder agglomerates of the present invention are porous to the inside and do not have the properties of the conventionally known cellulose particles.
於球狀之粉末凝聚體中之微結晶纖維素之黏結劑之合計的含量可舉例70.5至98重量%之態樣,較佳為85至92重量%。 The total amount of the binder of the microcrystalline cellulose in the spherical powder agglomerates may be, for example, 70.5 to 98% by weight, preferably 85 to 92% by weight.
此外,於球狀之粉末凝聚體中之微結晶纖維素與黏結劑之重量比可舉例9:1至7:2。 Further, the weight ratio of the microcrystalline cellulose to the binder in the spherical powder agglomerates may be, for example, 9:1 to 7:2.
於球狀之粉末凝聚體中之液體含量較佳為0.3至2.0 重量%,進一步較佳為0.5至1.5重量%。為如此之液體含量時,有助於確保以下所說明之球狀之粉末凝聚體之破壞強度。 The liquid content in the spherical powder agglomerates is preferably from 0.3 to 2.0% by weight, further preferably from 0.5 to 1.5% by weight. When it is such a liquid content, it contributes to ensuring the breaking strength of the spherical powder agglomerates described below.
另外,球狀之粉末凝聚體由以下說明之方法製作時,上述之液體含量係指水與乙醇之合計的含量。 Further, when the spherical powder aggregate is produced by the method described below, the above liquid content means the total content of water and ethanol.
本發明之粉末凝聚體之破壞強度如上述為1.5至5.0N,為如此之破壞強度之範圍,意味粉末凝聚體之密度為較低之狀態,藉由製作密度低且空隙多的狀態之粉末凝聚體,於粉末凝聚體之製作後添加液體香料時,液體香料係有效率地被吸收至粉末凝聚體內。 The breaking strength of the powder agglomerate of the present invention is 1.5 to 5.0 N as described above, and is such a range of the breaking strength that it means that the density of the powder agglomerates is low, and the powder is condensed by producing a state of low density and a large number of voids. In the case of adding a liquid fragrance after the preparation of the powder agglomerate, the liquid fragrance is efficiently absorbed into the powder agglomerate.
本發明之粉末凝聚體之密度為發揮上述之機能,可舉例0.2至0.8g/cm3之態樣,較佳為0.3至0.6g/cm3。 The density of the powder agglomerates of the present invention is such that it exhibits the above-described functions, and can be, for example, 0.2 to 0.8 g/cm 3 , preferably 0.3 to 0.6 g/cm 3 .
粉末凝聚體之密度係藉由下列的方法得到。準備複數的測定樣品(例如10粒),以流變計測定各樣品的樣品高度,得到各別的數值的平均值作為平均直徑。依據其平均直徑以所算出的體積值作為平均體積。將各粉末凝聚體之平均重量除以其平均體積而得。 The density of the powder agglomerates was obtained by the following method. A plurality of measurement samples (for example, 10 particles) are prepared, and the sample height of each sample is measured by a rheometer, and the average value of each value is obtained as an average diameter. The calculated volume value is taken as the average volume according to its average diameter. The average weight of each powder agglomerate is divided by its average volume.
在本發明之粉末凝聚體中係其內部的空隙並非僅集中於中心部分,而是均勻地存在於粉末凝聚體內,且於表面亦存在裂縫狀的空隙,故有助於容易吸收或保持例如香料般的液體物質。因而,可期待如此的液體物質在藏置中完全不會從粉末凝聚體滲出,或被抑制。 In the powder agglomerate of the present invention, the voids inside are not concentrated only in the central portion, but are uniformly present in the powder agglomerates, and crack-like voids are also present on the surface, thereby facilitating easy absorption or retention of, for example, perfume. a liquid substance. Therefore, it is expected that such a liquid substance does not ooze out from the powder agglomerate at all, or is suppressed.
本發明之球狀之粉末凝聚體可吸收與粉末凝聚體之重量等倍以上之量之液體。 The spherical powder aggregate of the present invention can absorb a liquid which is equal to or more than the weight of the powder agglomerate.
本發明之球狀之粉末凝聚體可在其周圍塗布塗布劑。如此之塗布劑,例如可舉例融點為50℃以上之油脂。藉由含有融點為50℃以上之油脂,於球狀之粉末凝聚體添加液體香料時,可良好地抑制對其周圍的滲出。 The spherical powder agglomerates of the present invention may be coated with a coating agent around them. As such a coating agent, for example, a fat or oil having a melting point of 50 ° C or more can be exemplified. When a liquid fragrance is added to a spherical powder agglomerate by containing a fat or oil having a melting point of 50 ° C or higher, bleeding around the periphery can be satisfactorily suppressed.
融點為50℃以上之油脂,可舉例融點為50℃以上之硬化油。 A grease having a melting point of 50 ° C or more can be exemplified by a hardened oil having a melting point of 50 ° C or more.
所謂硬化油係將在成為原料之常溫下對液狀的油脂加成氫所得之加工油,本發明較佳係使用融點為50℃以上之硬化油。 The hardened oil is a processing oil obtained by adding hydrogen to a liquid fat or oil at a normal temperature as a raw material. In the present invention, a hardened oil having a melting point of 50 ° C or higher is preferably used.
融點為50℃以上之硬化油,可舉例棕櫚極度硬化油、高芥菜種極度硬化油、菜種極度硬化油、大豆極度硬化油、動物性硬化油脂等之食用之硬化油。 The hardening oil having a melting point of 50 ° C or more may, for example, be a hardened oil of palm extreme hardening oil, extremely hardened oil of high mustard species, extremely hardened oil of vegetable species, extremely hardened oil of soybean, animal hardened oil, and the like.
融點為50℃以上之油脂可僅使用1種類,亦可混合使用2種類以上。 Only one type of fat or oil having a melting point of 50 ° C or more may be used, or two or more types may be used in combination.
本發明之對球狀之粉末凝聚體塗布的方法並無特別限定,可使用公知的方法。 The method for applying the spherical powder agglomerate of the present invention is not particularly limited, and a known method can be used.
<破壞強度及其測定法> <breaking strength and its determination method>
本發明之球狀之粉末凝聚體係其破壞強度為1.5至5.0N。 The spherical powder agglomeration system of the present invention has a breaking strength of 1.5 to 5.0 N.
破壞強度的測定係可經由第1圖之(a)至(d)所示之各狀態進行。第2圖係概略顯示該等的各時點之位移(應變的距離)與應力之關係。 The measurement of the breaking strength can be carried out in each state shown in (a) to (d) of Fig. 1 . Fig. 2 is a view schematically showing the relationship between the displacement (distance of strain) at each time point and the stress.
第1圖之(a)係顯示流變計之接觸體下降,該接觸體接觸球狀之粉末凝聚體之狀態(第2圖之(a)之時點)。 Fig. 1(a) shows a state in which the contact body of the rheometer is lowered, and the contact body contacts the spherical powder agglomerate (at the time point (a) of Fig. 2).
第1圖之(b)係顯示流變計之接觸體繼續下降,球狀之粉末凝聚體開始應變,對接觸體產生應力之狀態。如第2圖之(b)所示,應變之距離與應力之關係基本上為一次直線。 Fig. 1(b) shows a state in which the contact body of the rheometer continues to descend, and the spherical powder agglomerates start to strain and stress the contact body. As shown in (b) of Fig. 2, the relationship between the strain distance and the stress is substantially a straight line.
第1圖之(c)係顯示球狀之粉末凝聚體有某程度應變後,被破壞的狀態。如第2圖之(c)所示,被破壞之前之應力之最大值(最大荷重)相當於破壞強度,將其時點之位移設為破壞時位移。破壞之後釋放應力,瞬間靠近0N。 Fig. 1(c) shows a state in which the spherical powder agglomerates are destroyed after being strained to some extent. As shown in (c) of Fig. 2, the maximum value (maximum load) of the stress before being destroyed corresponds to the breaking strength, and the displacement at the time point is set as the displacement at the time of destruction. After the damage, the stress is released and it is close to 0N.
第1圖之(d)係顯示球狀之粉末凝聚體之破壞後亦繼續而接觸體下降,在上述(c)被破壞之球狀之粉末凝聚體之破壞片進一步微細地被破壞之狀態(第2圖之(d))。如第2圖之(d)所示,在此階段亦產生來自各個破壞片之應力。 (d) of FIG. 1 shows a state in which the spheroidal powder agglomerates continue to be degraded and the contact body is lowered, and the rupture sheet of the spherical pulverized powder agglomerate (c) is further finely destroyed ( (d) of Figure 2). As shown in (d) of Fig. 2, stress from each of the fracture sheets is also generated at this stage.
第3圖係各別顯示上述(a)以及(b)之狀態之球狀之粉末凝聚體、(c)的狀態之球狀之粉末凝聚體、(d)的狀態之球狀之粉末凝聚體之照片。 Fig. 3 is a view showing a spherical powder agglomerate in the state of the above (a) and (b), a spherical powder agglomerate in a state of (c), and a spherical powder agglomerate in a state of (d) Photo.
測定破壞強度時所使用之流變計,例如,可使用SUN科學公司製的CR-3000EX-S。測試時使用壓縮強度試驗用之接觸體。 For the rheometer to be used for measuring the breaking strength, for example, CR-3000EX-S manufactured by SUN Scientific Co., Ltd. can be used. The contact body for the compressive strength test was used for the test.
接觸體的下降速度係採用20.0mm/min,施加於流變計之球狀之粉末凝聚體之粒徑係採用1.0至6.0mm。 The descending speed of the contact body was 20.0 mm/min, and the particle size of the spherical powder agglomerates applied to the rheometer was 1.0 to 6.0 mm.
本發明之球狀之粉末凝聚體之製造方法,包含以下的步驟。 The method for producing a spherical powder aggregate of the present invention comprises the following steps.
將包含微結晶纖維素、黏結劑以及乙醇之漿體滴入至振動中的粉體,使形成由漿體與粉體所構成之球狀中間組 成物之第一步驟;以及將第一球狀中間組成物的液體含量減少至2重量%以下而用以獲得球狀之粉末凝聚體之第二步驟。 a first step of forming a spherical intermediate composition composed of a slurry and a powder by dropping a slurry containing microcrystalline cellulose, a binder, and ethanol into a vibrating powder; and forming a first spherical shape The second step of obtaining a spherical powder agglomerate is obtained by reducing the liquid content of the intermediate composition to 2% by weight or less.
於第一步驟中,首先,準備包含微結晶纖維素、黏結劑、以及乙醇之漿體。 In the first step, first, a slurry containing microcrystalline cellulose, a binder, and ethanol is prepared.
該漿體係可藉由於乙醇中添加微結晶纖維素與黏結劑來準備。調製漿體時可使用適當的分散機。 The slurry system can be prepared by adding microcrystalline cellulose and a binder to the ethanol. A suitable disperser can be used to modulate the slurry.
乙醇的純度較佳為90重量%以上,更佳為接近100%。換言之,含有作為雜質的水儘可能地少為較佳,但乙醇通常係可為取得的含水乙醇(水分含量為7重量%左右)。 The purity of ethanol is preferably 90% by weight or more, more preferably nearly 100%. In other words, it is preferable to contain as little water as possible as possible, but ethanol is usually obtained as aqueous ethanol (having a moisture content of about 7 wt%).
於漿體中之乙醇的含量,係以滴入至振動中之粉體時的漿體(以下,亦稱為滴入用漿體)之全量作為基準,可舉例65至80重量%之態樣,從對滴入用漿體賦予適度的黏度之觀點來看,以70至75重量%為較佳。 The content of the ethanol in the slurry is based on the total amount of the slurry (hereinafter, also referred to as the slurry for dropping) which is dropped into the powder in the vibration, and can be exemplified by 65 to 80% by weight. From the viewpoint of imparting a moderate viscosity to the slurry for dropping, it is preferably 70 to 75% by weight.
相對於滴入用漿體之全量,微結晶纖維素之含量可舉例15至25重量%之態樣,從對最終生成物之球狀之粉末凝聚體賦予適度的破壞強度及適當的密度之觀點來看,較佳為20至25重量%。相對於滴入用漿體之全量,若增大微結晶纖維素之含量,可提高球狀之粉末凝聚體之破壞強度。 The content of the microcrystalline cellulose can be, for example, 15 to 25 wt% with respect to the total amount of the slurry for dropping, from the viewpoint of imparting a moderate breaking strength and an appropriate density to the spherical powder agglomerates of the final product. In view, it is preferably from 20 to 25% by weight. When the content of the microcrystalline cellulose is increased relative to the total amount of the slurry for dropping, the breaking strength of the spherical powder aggregate can be improved.
相對於滴入用漿體之全量,黏結劑之含量可舉例2至6重量%之態樣,從對最終生成物之球狀之粉末凝聚體賦予適度的破壞強度之觀點來看,以3至5重量%為較佳。 The content of the binder may be, for example, 2 to 6% by weight with respect to the total amount of the slurry for dropping, from the viewpoint of imparting a moderate breaking strength to the spherical powder agglomerates of the final product, from 3 to 5% by weight is preferred.
前述黏結劑係可使用澱粉、明膠、阿拉伯膠、聚乙烯醇、羧甲基纖維素等水溶性聚合物。其中,較佳係可使用羧甲基纖維素。 As the binder, a water-soluble polymer such as starch, gelatin, gum arabic, polyvinyl alcohol or carboxymethyl cellulose can be used. Among them, carboxymethylcellulose is preferably used.
在第一步驟中,係將包含前述材料之漿體滴入於振動中之粉體中(滴入粉中)。對於滴入,係可舉例使用具有適當的噴嘴徑之噴嘴而實施之態樣。相對於滴入之漿體,粉體之量係以粉體相對於漿體為過剩存在的方式進行調整。 In the first step, a slurry containing the aforementioned material is dropped into the powder in the vibration (dropped into the powder). For the dropwise addition, a state in which a nozzle having an appropriate nozzle diameter is used can be exemplified. The amount of the powder is adjusted in such a manner that the powder is excessively present with respect to the slurry with respect to the slurry to be dropped.
作為滴入漿體之滴入目標的粉體,係與球狀之粉體凝聚體所含之微結晶纖維素相同,可舉例粉體之微結晶纖維素。使用微結晶纖維素作為滴入目標的粉體時,在粉體中滴入漿體時,漿體與粉體之相容性變佳,最終生成物之球狀的粉末凝聚體之性狀安定,故為較佳。另一方面,即便滴入之漿體所含之核劑與滴入目標之粉體為不同的材料,只要為於漿體滴入時之漿體與粉體之相容性佳,且可生成造成球狀之粉體凝聚體之第一球狀中間組成物者即可,粉體之材料無特別限制。 The powder to be dropped into the slurry is the same as the microcrystalline cellulose contained in the spherical powder agglomerate, and the microcrystalline cellulose of the powder can be exemplified. When microcrystalline cellulose is used as the powder to be dropped into the target, when the slurry is dropped into the powder, the compatibility between the slurry and the powder is improved, and the spherical powder agglomerates of the final product are stable. Therefore, it is better. On the other hand, even if the nucleating agent contained in the slurry to be dropped is different from the powder to be dropped into the target, the compatibility between the slurry and the powder at the time of dropping the slurry is good, and it can be produced. The first spherical intermediate composition which causes the spherical powder agglomerates may be used, and the material of the powder is not particularly limited.
將漿體滴入至粉體時,每單位時間之滴入數:可舉例180至200滴/分,每一滴的重量:25至30mg/滴。 When the slurry is dropped into the powder, the number of drops per unit time: 180 to 200 drops/min, and the weight of each drop: 25 to 30 mg/drip.
漿體係滴入於振動中之粉體中。藉由滴入於振動中之粉體,漿體的液滴係直接維持球狀或略球狀而快速地吸收包圍其周圍之粉體,產生第一球狀中間組成物。關於振動供料機之振動數,只要為第一球狀中間組成物可維持球狀 的程度即可,無特別限制。可舉例如振動數:40至60Hz。 The slurry system is dropped into the powder in the vibration. By dropping the powder in the vibration, the droplets of the slurry directly maintain the spherical shape or the slightly spherical shape and quickly absorb the powder surrounding the surrounding, thereby producing the first spherical intermediate composition. The number of vibrations of the vibrating feeder is not particularly limited as long as the first spherical intermediate composition can maintain a spherical shape. For example, the number of vibrations is 40 to 60 Hz.
使粉體振動之手段,係可舉例振動供料機。振動供料機當使用兼具搬送手段時,可藉由將漿體之滴入所使用之噴嘴固定,使滴入目標之粉體一邊移動一邊振動,連續地滴入漿體,以連續地生成第一球狀中間組成物。此外,使用兼具搬送手段之振動供料機時,可將生成之第一球狀中間組成物回收至配置在送出端之回收容器。另外,藉由改變漿體滴入所使用之噴嘴之口徑,可調整為最終生成物之球狀之粉末凝聚體之粒徑。 The means for vibrating the powder can be exemplified by a vibrating feeder. When the vibrating feeder is used as a conveying means, the slurry can be fixed by dropping the slurry into the nozzle, and the powder that has fallen into the target vibrates while moving, continuously dropping into the slurry to continuously generate The first spherical intermediate composition. Further, when a vibration feeder having a conveying means is used, the generated first spherical intermediate composition can be recovered to a recovery container disposed at the delivery end. Further, by changing the diameter of the nozzle used for dropping the slurry, the particle size of the spherical powder aggregate of the final product can be adjusted.
球狀中間組成物係在滴入之漿體中加入滴入目標之粉體者。滴入的時機、及藉由兼具搬送手段之振動供料機的搬送速度係可適當調整,但可舉例如球狀之中間組成物以180個/分生成之速度。 The spherical intermediate composition is added to the instilled slurry by the powder dropped into the target. The timing of the dropping and the conveying speed of the vibrating feeder having the conveying means can be appropriately adjusted, but it is, for example, a speed at which the spherical intermediate composition is generated at 180 parts/min.
前述之球狀中間組成物係於第二步驟中,以其含量減少至2重量%以下的方式使其乾燥。將液體含量減少至2重量%以下的手段,可舉例使用熱風產生裝置,而使球狀中間組成物受熱風而乾燥。受熱風而使其乾燥時,較佳為使球狀中間組成物一邊振動一邊進行。藉由一邊振動一邊受熱風,可使球狀中間組成物均勻地受到溫風,乙醇的揮發不會產生局部不均。振動之條件無特別限制,惟可舉例振動數20至50Hz。 The spherical intermediate composition described above is dried in the second step in such a manner that its content is reduced to 2% by weight or less. The means for reducing the liquid content to 2% by weight or less can be exemplified by using a hot air generating device, and the spherical intermediate composition is dried by hot air. When it is dried by hot air, it is preferable to carry out the spherical intermediate composition while vibrating. By receiving the hot air while vibrating, the spherical intermediate composition can be uniformly subjected to warm air, and localization of ethanol does not cause local unevenness. The condition of the vibration is not particularly limited, but the vibration number is 20 to 50 Hz.
上述之液體含量係乙醇與水之合計之含量。 The above liquid content is the total amount of ethanol and water.
例如,使球狀中間組成物一邊振動一邊乾燥之時,較佳為將第一球狀中間組成物承載於如篩之通氣性良好的材 料上而進行。 For example, when the spherical intermediate composition is dried while vibrating, it is preferred to carry the first spherical intermediate composition on a material having a good air permeability such as a sieve.
在乾燥所使用之熱風之溫度較佳為85至95℃左右,更佳為88至92℃左右。為如此之溫度範圍時,可儘速從球狀中間組成物除去乙醇,故可在球狀中間組成物內均一地產生空隙。 The temperature of the hot air used for drying is preferably about 85 to 95 ° C, more preferably about 88 to 92 ° C. In such a temperature range, ethanol can be removed from the spherical intermediate composition as quickly as possible, so that voids can be uniformly generated in the spherical intermediate composition.
此外,只要可將於球狀中間組成物中之液體含量減少至2重量%以下,其乾燥時間則無限制,但可以例如3至10分鐘,較佳為4至8分鐘之間進行。 Further, as long as the liquid content in the spherical intermediate composition can be reduced to 2% by weight or less, the drying time is not limited, but may be carried out, for example, between 3 and 10 minutes, preferably between 4 and 8 minutes.
經過第二步驟,可得到液體含量為2重量%以下之球狀之粉末凝聚體。 After the second step, a spherical powder agglomerate having a liquid content of 2% by weight or less can be obtained.
所得之球狀之粉末凝聚體之液體含量,對其破壞強度大造成重大影響。 The liquid content of the obtained spherical powder agglomerates has a significant influence on the breaking strength.
對於所得之球狀之粉末凝聚體係於第二步驟之後,可藉由公知之分級手段,僅將具有預定的粒徑之粉末凝聚體分級。 After the obtained spherical powder agglomeration system is subjected to the second step, only the powder agglomerates having a predetermined particle diameter can be classified by a known classification means.
可舉例如,在1.0至6.0mm之粒徑之範圍,分級成具有所期望之粒徑範圍,例如2.5至4.5mm之粒徑範圍者之態樣。 For example, in the range of the particle diameter of 1.0 to 6.0 mm, it is classified into a particle size range having a desired particle size range, for example, 2.5 to 4.5 mm.
此外,上述之第二步驟之後,亦可含有對於球狀之粉末凝聚體添加香料之步驟。添加香料之時,可舉例如使用噴霧體噴霧液體香料之態樣,或使用含浸法含浸液體香料之態樣。 Further, after the second step described above, a step of adding a fragrance to the spherical powder agglomerate may be further included. When the fragrance is added, for example, a spray of a liquid fragrance is used, or an impregnation method is used to impregnate a liquid fragrance.
此外,在添加香料之步驟之前後,或不含添加香料步驟,亦可含有對球狀之粉末凝聚體塗布塗布劑之步驟。添 加香料之後,以塗布劑塗布粉末凝聚體時,可更良好地抑制香料從球狀之粉末凝聚體的滲出。 Further, the step of applying a coating agent to the spherical powder agglomerates may be carried out after the step of adding the fragrance or without the step of adding the fragrance. After the addition of the fragrance, when the powder agglomerates are coated with the coating agent, the bleeding of the fragrance from the spherical powder aggregates can be more satisfactorily suppressed.
對於所得之球狀之粉末凝聚體之破壞強度,可藉由與前述1記載的測定方法相同的方法進行測定。所得之球狀之粉末凝聚體之破壞強度為1.5至5.0N。此破壞強度可藉由調整在上述之第二步驟中的乾燥條件來調整。 The breaking strength of the obtained spherical powder aggregates can be measured by the same method as the measurement method described in the above 1. The resulting spherical powder agglomerates have a breaking strength of 1.5 to 5.0 N. This breaking strength can be adjusted by adjusting the drying conditions in the second step described above.
本發明之球狀之粉末凝聚體之使用法,可舉例使用於吸煙物品,更具體而言,可舉例於粉末凝聚體擔載香料後,配置於吸煙物品之濾嘴中來使用。 The method of using the spherical powder agglomerate of the present invention can be exemplified for use in a smoking article, and more specifically, it can be used by arranging a powder agglomerate to carry a fragrance and then arranging it in a filter of a smoking article.
更具體的吸煙物品之態樣,可例示一種吸煙物品,其係具備包含煙草絲之煙草棒以及透過外層紙而與前述煙草桿之端部接續之濾嘴,前述濾嘴具有本發明之球狀之粉末凝聚體、配置有該球狀之粉末凝聚體之濾嘴區,前述濾嘴區可為填充有過濾材,亦可為模穴形狀,前述濾嘴可由單一濾嘴區所構成,亦可由複數的濾嘴區所構成。 In a more specific aspect of the smoking article, a smoking article comprising a tobacco rod comprising tobacco yarn and a filter passing through the outer paper to the end of the tobacco rod, the filter having the spherical shape of the present invention a powder agglomerate, a filter region in which the spherical powder agglomerate is disposed, the filter region may be filled with a filter material, or may be a cavity shape, and the filter may be composed of a single filter region, or may be composed of A plurality of filter zones are formed.
若為如此之態樣,未使用時球狀之粉末凝聚體會保持在濾嘴內。另一方面,使用時,吸煙者藉由對濾嘴施加外力而使濾嘴內的球狀之粉末凝聚體破壞,以將香料內包於粉末凝聚體時,可將主流煙與粉末凝聚體所內包之香料一起送達至使用者。 In this case, the spherical powder agglomerates remain in the filter when not in use. On the other hand, when used, the smoker destroys the spherical powder agglomerates in the filter by applying an external force to the filter, and when the fragrance is encapsulated in the powder agglomerate, the mainstream smoke and the powder agglomerate can be used. The inner package of spices is delivered to the user together.
此外,本發明之粉末凝聚體,為了破壞而施加外壓時,由於在人易破壞之壓力之範圍被破壞,且具有人可感受到輕鬆地弄碎的感覺之適當的破壞時位移,故使用者可獲得 獨特輕鬆地弄碎的感覺。 Further, the powder agglomerate of the present invention is used when external pressure is applied for the purpose of destruction, since it is broken in the range of pressure which is easily broken by a person, and has an appropriate breakage displacement when a person can feel the feeling of being easily broken. You get the feeling of being uniquely and easily broken.
本發明係藉由實施例更具體說明,但本發明在不超過其要旨之範圍,並不限定於以下之實施例之記載。 The present invention is more specifically described by the examples, but the present invention is not limited to the scope of the gist of the invention.
<實施例1> <Example 1>
進行調製作用以製作球狀之粉末凝聚體之材料的漿體。 Modulation is carried out to prepare a slurry of a material of spherical powder aggregates.
於乙醇(含水乙醇:水分含量約7重量%)730重量份中,添加羥丙基甲基纖維素40重量份以及微結晶纖維素(ENDURANCE MCC VE-090:光洋商會)230重量份,使用分散機(HOMOGENIZING DISPER)以3000至5000rpm攪拌5分鐘,得到漿體。 40 parts by weight of hydroxypropylmethylcellulose and 230 parts by weight of microcrystalline cellulose (ENDURANCE MCC VE-090: Guangyang Chamber of Commerce) were added to 730 parts by weight of ethanol (aqueous ethanol: moisture content: about 7% by weight), and dispersed. The machine (HOMOGENIZING DISPER) was stirred at 3000 to 5000 rpm for 5 minutes to obtain a slurry.
將所得之滴入用之漿體,滴入於以相對於所滴入之漿體為過剩量之方式裝填粉末狀的微結晶纖維素(與漿體所含者相同)有作為粉體之振動供料機中。滴入漿體時的振動供料機之振動數為55Hz使其振動 The obtained slurry is dropped into a slurry, and the powdered microcrystalline cellulose (same as the one contained in the slurry) is added to the slurry in an excess amount with respect to the instilled slurry, and the vibration is used as a powder. In the feeder. The vibration of the vibrating feeder when dropping into the slurry is 55 Hz to vibrate
漿體的滴入速度適用180至200滴/分,每一滴的重量適用25至30mg/滴。 The dropping speed of the slurry is applied to 180 to 200 drops/min, and the weight of each drop is 25 to 30 mg/drip.
若以上述速度將漿體連續地滴入於振動供料機中,滴入之液滴埋没於粉末狀的微結晶纖維素中的同時,捲入周圍的微結晶纖維素,瞬時形成球狀組成物(球狀中間組成物)。 If the slurry is continuously dropped into the vibrating feeder at the above speed, the dropped droplets are buried in the powdery microcrystalline cellulose, and are entrained in the surrounding microcrystalline cellulose to form a spherical composition instantaneously. Object (spherical intermediate composition).
球狀中間組成物係在振動供料機上一邊振動一邊從上 游側搬送至下游側,回收至配置在下游端之回收容器中。 The spherical intermediate composition is transported from the upstream side to the downstream side while vibrating on the vibrating feeder, and is collected in a recovery container disposed at the downstream end.
接下來的步驟,藉由熱風使所得之球狀中間組成物乾燥。藉由熱風之乾燥時,係將球狀中間組成物配置在振動式的篩上,給氣溫度適用90℃,使其乾燥5分鐘。乾燥之時,使配置有球狀中間組成物之篩振動(位相:8(20至30Hz)),並使篩上之中間球狀組成物振動,藉此,以便均勻地受到熱風。 In the next step, the resulting spherical intermediate composition is dried by hot air. When drying by hot air, the spherical intermediate composition was placed on a vibrating screen, and the feed gas temperature was applied at 90 ° C for 5 minutes. At the time of drying, the sieve in which the spherical intermediate composition was disposed was vibrated (phase: 8 (20 to 30 Hz)), and the intermediate spherical composition on the sieve was vibrated, thereby being uniformly subjected to hot air.
藉由該乾燥,使球狀中間組成物之液體含量減少至2重量%以下,得到球狀之粉末凝聚體。 By this drying, the liquid content of the spherical intermediate composition is reduced to 2% by weight or less to obtain a spherical powder aggregate.
<破壞強度的測定> <Measurement of Destructive Strength>
對於所得到之球狀之粉末凝聚體,使用流變計(SUN科學公司)製之CR-3000EX-S,進行測定如第1圖所示之各狀態之試驗。 The CR-3000EX-S by a rheometer (SUN Scientific Co., Ltd.) was used for the obtained spherical agglomerates, and the test of each state shown in FIG. 1 was performed.
藉由流變計進行測定時之接觸體的下降速度係採用20.0mm/min。接觸體係使用壓縮強度試驗用者。 The rate of decrease of the contact body when measured by a rheometer was 20.0 mm/min. The contact system uses the compressive strength test user.
另外,就比較例而言,對於藉由市售的纖維素顆粒(Viscopearl A,Viscopearl P:任一者均為RENGO公司製)與後述之方法以製丸粒機所成形之成形物,測定破壞強度與應變率。 In addition, in the comparative example, the molded article formed by the pelletizer was measured by a commercially available cellulose particle (Viscopearl A, Viscopearl P: either manufactured by RENGO) and a method described later, and the damage was measured. Strength and strain rate.
對於本發明之球狀之粉末凝聚體、Viscopearl A、Viscopearl P、製丸粒機所成形之成形物之各試料,各別準備5至10個,藉由上述之流變計,測定樣品高度(粒徑)、最大荷重(破壞強度)、移動距離、應變率。應變率係表示對於粒子的粒徑之至破壞時為止的接觸體移動的距離(移 動距離)之比例,表示此應變率愈大,至粒子被破壞為止愈大幅地崩壞。 For each of the samples of the spherical powder aggregate of the present invention, Viscopearl A, Viscopearl P, and the pellet-formed machine, 5 to 10 samples were prepared, and the sample height was measured by the rheometer described above ( Particle size), maximum load (destructive strength), moving distance, strain rate. The strain rate indicates the ratio of the distance (movement distance) of the contact body movement from the particle diameter of the particle to the time of destruction, indicating that the larger the strain rate is, the more the particle collapses as the particle is broken.
結果係表示於下列表1。 The results are shown in Table 1 below.
在上述所示之試驗使用之Viscopearl A,係將在黏液纖維(viscose)中添加多孔化劑之原料,從噴嘴朝向酸浴加壓降下,而凝固成球狀,同時進行氣體發泡,使經凝固之原料多孔化而得者。在日本特開2005-232379號有如此之纖維素顆粒之製法之具體的記載。 Viscopearl A used in the above-mentioned test, the raw material of the porous agent is added to the muscose fiber, and the pressure is lowered from the nozzle toward the acid bath to be solidified into a spherical shape, and the gas is foamed at the same time. The solidified raw material is made porous. A specific description of the method for producing such cellulose granules is disclosed in Japanese Laid-Open Patent Publication No. 2005-232379.
另一方面,Viscopearl P並非黏液纖維,而係於木材木漿或各種纖維中添加黏結劑並造粒而成者。 On the other hand, Viscopearl P is not a slime fiber, but is made by adding a binder and granulating it to wood pulp or various fibers.
以上述所示製丸粒機所成形之成形物,係以下列的順序製作。 The molded article formed by the pelletizer described above was produced in the following order.
首先,為得到安裝於製丸粒機之板狀混練物,於攪拌混合機內以水(40重量%)、微結晶纖維素(57重量%)、HPMC(羥丙基甲基纖維素)(3重量%)之順序投入,在室溫下混練1小時。 First, in order to obtain a plate-like kneaded material attached to a pelletizer, water (40% by weight), microcrystalline cellulose (57% by weight), and HPMC (hydroxypropylmethylcellulose) were mixed in a stirring mixer ( The order of 3 wt%) was carried out, and the mixture was kneaded at room temperature for 1 hour.
其次,將所得之黏土狀之混練物成型為板狀,安裝於製丸粒機。 Next, the obtained clay-like kneaded material was molded into a plate shape and attached to a pelletizer.
藉由將製丸粒機內之滾筒與成型板之間隙設定為4.0mm,進行製丸粒造粒以得到經球狀化之黏土狀混練物。 The granulated clay-like kneaded material was obtained by pelletizing the gap between the drum in the pelletizing machine and the forming plate to 4.0 mm.
將所得之經球狀化之黏土狀混練物曝露於70℃熱風下,使水分含量乾燥至0.8重量%以下,得到作為最終成果物之球狀之成形物。 The obtained spheroidized clay-like kneaded material was exposed to hot air at 70 ° C to dry the moisture content to 0.8% by weight or less to obtain a spherical molded product as a final product.
如上述之表1之結果所示,與本發明之粉末凝聚體相異,市售之纖維素顆粒或以製丸粒機所形成之成形物,僅管其粒徑與本發明之粉末凝聚體類似,但至破壞所需的荷重非常大,無法以人的手指容易地破壞者。相對 於此,本發明之球狀之粉末凝聚體係至破壞所需的荷重小,又應變率亦小,故可以人的手指簡單地破壞,此外,可給予使用者輕鬆地弄碎的感覺者。進一步,將本發明之粉末凝聚體破壞後,經過第3圖(c)而破壞至如(d)所示的細粉為止。 As shown by the results of Table 1 above, similar to the powder agglomerates of the present invention, commercially available cellulose particles or shaped articles formed by pelletizing machines, only the particle size thereof and the powder agglomerates of the present invention Similar, but the load required to destroy is very large and cannot be easily destroyed by human fingers. On the other hand, the spherical powder agglomeration system of the present invention has a small load required for destruction and a small strain rate, so that the human finger can be easily broken, and the user can be easily crushed. Further, after the powder aggregate of the present invention is destroyed, it is broken to the fine powder as shown in (d) after the third diagram (c).
將用以得到表1所示結果而進行之藉由流變計進行測定時之荷重與經過時間之關係顯示於第4至7圖。在第4至7圖中,縱軸表示荷重(N),橫軸表示時間(秒)。 The relationship between the load and the elapsed time when the measurement was carried out by the rheometer to obtain the results shown in Table 1 is shown in Figures 4 to 7. In Figures 4 to 7, the vertical axis represents the load (N) and the horizontal axis represents time (seconds).
從第4圖(本發明之粉末凝聚體之結果)來看,得知雖然在施加最大荷重的時點球狀之粉末凝聚體一旦破碎,但破碎的各別的碎片為柔軟,零散崩落,被接觸體抵壓,同時並以微弱的力道崩壞的狀態。應變非常小,接觸體接觸於粉末凝聚體後約以0.5至1.0秒破碎。 From the fourth graph (the result of the powder agglomerate of the present invention), it is found that although the spherical powder agglomerates are broken when the maximum load is applied, the broken individual fragments are soft, scattered, and contacted. The body resists and at the same time collapses with a weak force. The strain is very small, and the contact body is broken about 0.5 to 1.0 second after contact with the powder agglomerate.
從第5圖(以製丸粒機所成形之成形物之結果)來看,得知最大荷重非常大(約38至約60N),並非以人的手指弄碎的硬度。若被破壞,則破碎成碎片,但幾乎全部的碎片破碎後約1秒左右成為如未接觸接觸體的大小。從該處得知,碎片進一步被接觸體壓住,但各別的碎片未崩碎,而具有某程度的強度。 From the fifth figure (the result of the formed product formed by the pelletizer), it is found that the maximum load is very large (about 38 to about 60 N), and the hardness is not broken by a human finger. If it is broken, it breaks into pieces, but almost all of the pieces become about the size of the uncontacted body after about 1 second. From this it is known that the fragments are further pressed by the contact body, but the individual fragments are not broken and have a certain degree of strength.
從第6圖(Viscopearl A之結果)來看,得知最大荷重非常大(約30N)。接觸接觸體後至破碎為止,對象物一邊被壓一邊變形,與其謂破碎,不如謂崩潰的狀態。 From the 6th figure (the result of Viscopearl A), it is known that the maximum load is very large (about 30N). After touching the contact body until it is broken, the object is deformed while being pressed, and it is not as broken as it is broken.
從第7圖(Viscopearl P之結果)來看,得知最大荷重比Viscopearl A更加大。此外,對象物接觸接觸體後,被壓而 持續變形(持續施加荷重)。 From the 7th figure (the result of Viscopearl P), it is known that the maximum load is larger than Viscopearl A. Further, after the object contacts the contact body, it is pressed and continuously deformed (continuous application of load).
<液體之吸收性> <Liquid absorption>
使用本發明之粉末凝聚體、與作為比較例之使用上述之製丸機所得成形物,進行確認有關液體之吸收性之試驗。 Using the powder agglomerate of the present invention and the molded article obtained by using the above-described pelletizer as a comparative example, a test for confirming the absorbability of the liquid was carried out.
於燒杯中秤量1.0g之各試料,於燒杯內的試料中滴入過剩量的水或油(中鏈脂肪酸三酸甘油酯:2至3g)。30秒後,以KimWipes拭取顆粒表面,進行秤量。將各別顆粒每1g的吸附量表示於下列的表2。 A sample of 1.0 g of each sample was weighed in a beaker, and an excess amount of water or oil (medium chain fatty acid triglyceride: 2 to 3 g) was dropped into the sample in the beaker. After 30 seconds, the surface of the granules was wiped with Kim Wipes and weighed. The amount of adsorption per 1 g of each particle is shown in Table 2 below.
從表2之結果,本發明之粉末凝聚體之吸水性、吸液性之任一者均優,以重量比計可吸收等倍量以上之液體。另一方面,使用以往的製丸機所得之成形物,係無法得到那樣的吸液性。咸認此係於顆粒內之空隙之存在量或空隙之存在狀態的差異所致者。 As a result of the results of Table 2, the powder agglomerates of the present invention are excellent in water absorbability and liquid absorbency, and can absorb a liquid of an equal amount or more by weight. On the other hand, such a liquid absorbing property cannot be obtained by using a molded article obtained by a conventional pelletizer. It is believed that the amount of voids present in the particles or the difference in the state of existence of the voids is caused.
<密度的測定> <Density determination>
測定本發明之粉末凝聚體與藉由上述之製丸粒機所成形之球狀成形物之密度。取樣依各別之製法所作成之球狀之粉末凝聚體10粒,求得平均直徑與平均重量。從其平均直徑算出球狀之粉末凝聚體之平均體積,以(平均重量)÷ (平均體積)之計算算出平均密度。 The density of the powder agglomerates of the present invention and the spherical shaped articles formed by the pelletizer described above were measured. Spherical powder agglomerates of 10 pellets were prepared by a separate method to obtain an average diameter and an average weight. The average volume of the spherical powder aggregates was calculated from the average diameter thereof, and the average density was calculated by calculation of (average weight) ÷ (average volume).
‧本發明之粉末凝聚體 ‧ powder aggregates of the invention
直徑(1粒):3.70mm(10粒直徑=3.70cm) Diameter (1 capsule): 3.70mm (10 capsules = 3.70cm)
體積(1粒):0.02650cm3 Volume (1 capsule): 0.02650cm 3
密度:0.48g/cm3 Density: 0.48g/cm 3
‧製丸粒機所形成之球狀成形物 ‧Spheroidal formed by pellet machine
直徑(1粒):3.65mm(10粒直徑=3.65cm) Diameter (1 capsule): 3.65mm (10 capsules = 3.65cm)
體積(1粒):0.02544cm3 Volume (1 capsule): 0.02544cm 3
密度:1.29g/cm3 Density: 1.29g/cm 3
如算出結果所示,本發明之粉末凝聚體與製丸粒機所成形之球狀成形物係在密度可看到大的差異。此係顯示依製法而產生在顆粒內之空隙的存在量或空隙的存在狀態的差異者,藉由此存在狀態的差異,本發明之粉末凝聚體係具有可由人的手指容易破壞的破壞強度,同時在破壞後並非大塊而成為產生細粒之球狀之粉末凝聚體。 As shown by the results of the calculation, the powder agglomerates of the present invention and the spherical shaped articles formed by the pelletizer have a large difference in density. This shows that the amount of voids present in the particles or the difference in the state of existence of the voids is produced by the method, and by virtue of the difference in the state of existence, the powder agglomerated system of the present invention has a breaking strength which can be easily broken by human fingers, and at the same time After the destruction, it is not a bulk and becomes a spherical aggregate of powder which produces fine particles.
本發明之球狀之粉末凝聚體,其破壞強度為可藉人的手指容易破壞的程度,破壞後產生該球狀之粉末凝聚體之細粒。因此,將本發明之球狀之粉末凝聚體配置於如香煙般的吸煙物品所使用之於內部具有朝吸口端的通路之濾嘴內、或吸嘴部的附近之濾嘴部內時,藉由吸煙者的手指所破壞之細粒,變得可容易到達吸煙者的口腔內,藉此,粉末狀的香味源對吸煙者之傳送效率會提升。 In the spherical powder aggregate of the present invention, the breaking strength is such that it can be easily broken by a human finger, and the fine particles of the spherical powder aggregate are generated after the destruction. Therefore, when the spherical powder agglomerate of the present invention is disposed in a filter such as a cigarette-like smoking article in a filter having a passage toward the suction end or a filter portion in the vicinity of the nozzle portion, smoking is performed. The fine particles destroyed by the fingers of the person can easily reach the mouth of the smoker, whereby the powdery flavor source can increase the transmission efficiency of the smoker.
此外,本發明之球狀之粉末凝聚體添加液體時的吸收 性良好,同時可期待其後的滲出之抑制。 Further, the spherical powder agglomerates of the present invention have good absorbability when liquid is added, and can be expected to suppress subsequent bleeding.
藉此,使本發明之球狀之粉末凝聚體吸收液體香料時,可期待例如作為香料擔載體或香味保持劑之角色,將其配置於吸煙物品的濾嘴內或濾嘴區段間,吸煙時將其破壞,藉此,可期待擔載或保持之香味成分釋出至粉末凝聚體之外部。 Therefore, when the spherical powder agglomerate of the present invention absorbs the liquid fragrance, it can be expected to be placed in the filter of the smoking article or between the filter sections, for example, as a fragrance carrier or a fragrance retaining agent. When it is destroyed, it is expected that the aroma component carried or retained can be released to the outside of the powder agglomerate.
進一步,依據本發明之球狀之粉末凝聚體之製造方法,可提供具有可藉由人的手指容易破壞的破壞強度、以及人可感受到輕易弄碎之感覺的適當之破壞時位移,同時在破壞後並非大塊而是產生細粒之球狀之粉末凝聚體。進一步藉由此製法,不用進行以往習知之用以得到多孔質構造而進行氣體發泡之步驟般的化學反應,且容易藉由機械安定地製造。 Further, according to the method for producing a spherical powder agglomerate of the present invention, it is possible to provide an appropriate breakage displacement having a breaking strength which can be easily broken by a human finger and a feeling that a person can feel the feeling of being easily broken, and After the destruction, it is not a large block but a spherical agglomerate of fine particles. Further, by this production method, it is not necessary to carry out a chemical reaction such as a step of performing gas foaming to obtain a porous structure, and it is easy to manufacture by mechanical stability.
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