TW201204274A

TW201204274A - Method of producing cigarette filter

Info

Publication number: TW201204274A
Application number: TW99124109A
Authority: TW
Inventors: Hiroki Shikata; Masato Miyauchi; Ayako Chiku
Original assignee: Japan Tobacco Inc
Priority date: 2010-07-22
Filing date: 2010-07-22
Publication date: 2012-02-01

Abstract

The present invention provides a method of producing cigarette filter using acetate tow or acetate film, wherein a spice is penetrated into the deep part of acetate filer or acetate film constituting the acetate tow.

Description

201204274 六、發明說明：【發明所屬之技術領域】本發明係關於一種經香料加香之香煙濾嘴（filter)之製造方法。【先前技術】以往已知有一種將於濾嘴插塞（filterPlug)製造步驟中所使用之可塑劑中溶解及分散有香料之加香液添加於醋酸鹽絲束（acetate tow)而成之經香料加香之濾嘴。例如，專利文獻1係揭示一種將於濾嘴插塞之製造步驟中所使用之可塑劑中溶解及分散有薄荷醇（menth〇i)之加香液添加於醋酸鹽絲束而成之濾嘴及其製造方法。在此方法中，使加香液含有蔗糖高級脂肪酸酯。此外，其中記一糸由此種簡單的加香操竹 /-h 'Λ. 種if 心作’使所添加之香料在發較少且使保香性較佳 —丄 4間的揮過滤嘴的煙。再者，发士 ^^放至通級脂肪酸酯之性質，而 ^ 像庶糠高而以如黏接體或膠體（gel)之液的形式殘存於濾嘴，蚀去上丨私；又頰的固溶香性。冑香_以《嘴揮發，而提升保此外，亦已知一鍤—人丄、上 , . I έ在渡嘴插塞中浸潰有香粗絲（thread)的經香料如香之遽嘴。例如，專利文^之煙 (Γ ))之製造I置及製造方法。在此等方=嘴的量係將為了控制香财效率㈣換及香方决中’ 煙絲進行對位。 322223 3 201204274 在薄荷醇製品中’薄荷醇從據嘴往煙中的釋放量係隨時間經過^咸少。尤其在夏天於自動販賣機中之溫度條件下保存製品時，會有從據嘴的釋放量減少之情形。結果，已知會有薄荷醇製品在煙中的薄荷醇量降低，而損及薄荷醇製品之吸煙時之香味的情形。在此，顯不關於煙中薄荷醇量經時變化之實驗結果。灶以下列方式來試製經薄荷醇加香之濾'嘴。將薄荷醇溶解 27/ί»於屬於可塑劑之甘油三醋酸酯（杜中而調製加香液。在使用濾嘴絲束（filtert〇w)(4Y35〇〇〇)之濾嘴插塞的製造步驟中，添加已加溫成約⑽之加香液而使甘油三醋酸酯含有率為6wt%，獲得濾嘴長度每25mm之薄荷醇含量為3mg的經薄荷醇加香之濾嘴。將所獲得之經薄荷醇加香之濾嘴、與未經薄荷醇加香之香煙桿（r〇d)(七星薄荷煙（Seven Stars Menthol)用）捲起，以軟包（s〇ft pack)來包裝而製作樣本（sampie)製品。將所獲得之樣本製品在22¾ (經調節之室内）及55°C之溫度條件下保存，每隔預定期間即回收，且在ISO吸煙條件下吸煙，以測量每一根香煙的煙中薄荷醇量。吸煙條件係將抽吸 (puff)頻率設為每60秒一次，抽吸2秒鐘，抽吸量為 35mL。將捕集於劍橋式滤嘴（Cambridge filter )之薄荷醇以甲醇溶媒萃取’且使用氣相層析儀（gas chromatograph ) GC (HEWLETT PACKARD 公司製 6890series)來定量。此外，為了求出從濾嘴釋放薄荷醇的量，而進行了以下的實驗。將上述試製的經薄荷醇加香之濾嘴放入密封包 4 322223 201204274 裝中’在22°C (經調節之室内）及55°C之溫度條件下保存。每隔預定期間即取出經薄荷醇加香之濾嘴，與市售的柔和七星超淡煙（MILD SEVEN super light)之濾嘴部替換而製作香煙樣本。以膠帶（tape)將濾嘴開口部封住，與上述同樣地在ISO吸煙條件下吸煙以測量煙中薄荷醇量。第1圖係顯示薄荷醇香煙之煙中薄荷醇量的經時變化。三角符號係使用在22。(：下保存之濾嘴之香煙的結果，圓圈符號係顯示使用在55°C下保存之濾嘴之香煙的結果。從此等結果可得知，薄荷醇香煙之煙中薄荷醇量，即使是在22°C下保存之濾嘴亦隨時間經過而降低，而且在55 °C之高溫下保存的濾嘴，其降低尤其顯著。第2圖係顯示從濾嘴釋放薄荷醇量的經時變化。已確認到從濾嘴釋放的薄荷醇量係隨時間經過而降低，且當温度變高時，則有顯著的降低。因此，可得知薄荷醇香煙的煙中薄荷醇量的降低，係由於從濾嘴釋放薄荷醇量的降低而導致。從濾' 嘴釋放薄何醇里的降低原因’據稱係因薄荷醇滲透至醋酸鹽纖維（acetate fiber)深部所致（s.A.Wilson, Theoretical aspects of menthol migration and transfer, 47th201204274 VI. Description of the Invention: [Technical Field of the Invention] The present invention relates to a method of manufacturing a perfumed cigarette filter. [Prior Art] There has been known a method in which a flavoring liquid in which a fragrance is dissolved and dispersed in a plasticizer used in a filter plug manufacturing step is added to an acetate tow. Spice and fragrant filter. For example, Patent Document 1 discloses a filter in which a perfuming liquid in which a menthol (menh〇i) is dissolved and dispersed in a plasticizer used in a manufacturing step of a filter plug is added to an acetate tow. And its manufacturing method. In this method, the perfuming liquid contains a sucrose higher fatty acid ester. In addition, it is noted that the simple addition of the fragrant bamboo /-h 'Λ. kind of if the heart is made to make the added spices less and the fragrance is better - 丄 4 between the filter smoke. Furthermore, the hair is placed on the nature of the fatty acid ester, and the image is high in the form of a liquid such as a glue or a gel, which remains in the filter and eclipses the smear; The solid solubility of the cheeks. Musk _ "The mouth is volatilized, and the promotion is also added. It is also known as a cockroach - 丄, 上, . I 浸浸 έ έ 渡渡渡渡渡渡渡渡渡渡渡渡 έ έ έ έ έ έ έ έ έ έ έ έ έ έ . For example, the manufacturing method and manufacturing method of the patent paper (Γ). In this case, the amount of the mouth will be adjusted in order to control the efficiency of the fragrant (four) and the scent of the scent. 322223 3 201204274 In the menthol product, the release of menthol from the mouth to the smoke is less than that of the time. Especially when the product is stored under the temperature conditions in the vending machine in the summer, there is a case where the amount of release from the mouth is reduced. As a result, it is known that the amount of menthol in the menthol product is lowered, and the scent of the menthol product when smoking is damaged. Here, the experimental results of the change in the amount of menthol in the smoke were not shown. The stove was tested in the following manner to make a menthol-filled filter. Dissolve menthol in 27/ί» in a triglyceride belonging to a plasticizer (Duzhong to prepare a flavoring liquid. Manufacture of a filter plug using a filter tow (4Y35〇〇〇) In the step, the flavoring liquid which has been heated to about (10) is added so that the triacetin content is 6 wt%, and a menthol-scented filter having a menthol content of 3 mg per 25 mm of the filter length is obtained. The menthol-scented filter is rolled up with a non-menthol-scented cigarette rod (r〇d) (for Seven Stars Menthol) and packaged in a soft pack (s〇ft pack). A sampie product is prepared. The obtained sample product is stored in a 223⁄4 (conditioned room) and at a temperature of 55 ° C, recovered every predetermined period of time, and smoked under ISO smoking conditions to measure each The amount of menthol in the smoke of a cigarette. The smoking condition is to set the puff frequency once every 60 seconds, pump for 2 seconds, and the suction volume is 35 mL. It will be trapped in the Cambridge filter (Cambridge filter) ) menthol is extracted with methanol solvent' and gas chromatograph GC (HE) In order to determine the amount of menthol released from the filter, the following experiment was carried out. The above-mentioned menthol-scented filter was placed in a sealed bag 4 322223 201204274 Store in '22 ° C (conditioned room) and 55 ° C temperature. Remove the menthol-scented filter every predetermined period, and the commercially available soft seven-star super light smoke (MILD SEVEN super A cigarette sample was prepared by replacing the filter portion of the light. The filter opening was sealed with a tape, and smoked under ISO smoking conditions to measure the amount of menthol in the smoke. Figure 1 shows menthol The amount of menthol in cigarette smoke changes over time. The triangle symbol is used as a result of 22 (: the result of the cigarette under the filter, and the circle symbol shows the result of using the cigarette of the filter stored at 55 °C. From these results, it can be known that the amount of menthol in the smoke of the menthol cigarette is reduced even with the filter stored at 22 ° C over time, and the filter preserved at a high temperature of 55 ° C is lowered. Especially remarkable. Figure 2 The change in the amount of menthol released from the filter is shown. It has been confirmed that the amount of menthol released from the filter decreases with time, and when the temperature becomes high, there is a significant decrease. The decrease in the amount of menthol in the cigarette of the alcoholic cigarette is caused by a decrease in the amount of menthol released from the filter. The reason for the decrease in the release of the thin alcohol from the filter 'mouth' is said to be due to the penetration of menthol to the acetate fiber ( Acetate fiber) (SAWilson, Theoretical aspects of menthol migration and transfer, 47th

Tobacco Chemist’ Reserch Conference，1993, Gatlinburg)。最近’已付知藉由活用顯微鏡雷射拉曼系統（laser Raman system)之高度的空間解析能力與2次元拉曼映像（Raman mapping)功能，即可測量醋酸鹽纖維内之薄荷醇分布。因此，在各種條件下保存薄荷醇，以調查醋酸鹽纖維 322223 5 201204274 内之薄荷醇分布。茲準備柔和七星Impact One薄荷煙盒子版(MILD SEVEN Impact One Menthol Box)用之滤嘴，分別在22°C (經調節之室内）下保存2.5個月、在22°C下保存 8個月、或在55°C下保存1星期。對於各個濾嘴，使用 Nicolet Almega 拉曼分光器（Nicolet™ Almega™ XR， Thermo Fisher Scientific Inc” Waltham, Massachusetts)進行拉曼2次元面分析，測量在構成濾嘴之醋酸鹽纖維内的薄荷醇之分布。以曝光時間1秒鐘、曝光次數2次、及背景（background)曝光次數512次來測量資料。光學系統之條件如下。雷射波長：532nm、雷射輸出水準：i〇〇〇/0 (10mW )、光柵（grating ) : 672線/ mm、分光器孔徑Tobacco Chemist' Reserch Conference, 1993, Gatlinburg). Recently, it has been known that the menthol distribution in acetate fibers can be measured by utilizing the high spatial resolution capability of the laser Raman system and the two-dimensional Raman mapping function. Therefore, menthol was preserved under various conditions to investigate the distribution of menthol in acetate fiber 322223 5 201204274. Prepare a filter for the Mild SEVEN Impact One Menthol Box, which is stored at 22 ° C (conditioned room) for 2.5 months and at 22 ° C for 8 months. Or store at 55 ° C for 1 week. For each filter, a Raman 2 dimensional analysis was performed using a Nicolet Almega Raman spectrometer (NicoletTM AlmegaTM XR, Thermo Fisher Scientific Inc. Waltham, Massachusetts) to measure the menthol in the acetate fibers constituting the filter. Distribution. The data was measured with an exposure time of 1 second, an exposure frequency of 2 times, and a background exposure of 512 times. The conditions of the optical system are as follows. Laser wavelength: 532 nm, laser output level: i〇〇〇/0 (10mW), grating (grating): 672 lines / mm, splitter aperture

(aperture): 50# m 針孔（pinh〇le)、物鏡：1〇〇倍（NA —0.9 )。映像形態係設為區域映像（area map )，且設X方向步階尺寸（step size)為i.〇em、Y方向步階尺寸為1〇 // m。並且另行將構成各個濾嘴之醋酸鹽纖維進行光學顯微鏡觀察像的攝影。根據由拉曼紐之騎鹽基材而來的 2943cm1之峰值’獲得醋酸鹽之橫剖面之外觀作為化學影像（chemicai image)。此外，根據由拉曼光譜之薄荷醇而來之769cm-〗之峰值與由醋酸鹽基材而來之912⑽·】之峰值的強度比，獲得在酷酸鹽纖維之橫剖面内之薄荷醇之八布作為化學影像。藉由使用2個峰值之強度比 : 干擾的影響。在醋酸鹽纖維内的薄荷醇之分布，依保存條件係如以 322223 6 201204274 下所示。在22°C下保存2.5個月之濾嘴中，薄荷醇係偏存於醋酸鹽纖維表面。在22°C下保存8個月之濾嘴中，薄荷醇係滲透至醋酸鹽纖維之深部。在55°C下保存1星期之濾嘴（受到熱履歷之濾嘴）中，可得知薄荷醇均勻地分布於醋酸鹽纖維内。因此，一如預期，從濾嘴釋放薄荷醇量的降低，顯然係由於薄荷醇滲透至醋酸鹽纖維深部所致。專利文獻1之將薄荷醇溶解於甘油三醋酸酯中之方法、及專利文獻2及3之將浸潰有薄荷醇之煙絲導入濾嘴中之方法，目的僅在於將薄荷醇加香於濾嘴，而其目的並非控制在醋酸鹽纖維内的薄荷醇之分布。在專利文獻1中，由於容易使薄荷醇與蔗糖高級脂肪酸酯一起以黏接體或膠體之類的固溶液的形式而殘存，因此，有抑制在醋酸鹽纖維内之薄荷醇之分布之經時變化的可能性。然而，會由於蔗糖高級脂肪酸酯之親油性及界面活性效果而促進含有水分之煙中成分的吸附，而對吸煙時之香味造成影響。此外，薄荷醇對於醋酸鹽纖維深部的滲透係方向均衡地自然進行。因此，只要薄荷醇從蔗糖高級脂肪酸酯分離並擴散，就會滲透至醋酸鹽纖維深部。因此，從專利文獻1中，並未暗示在存放香煙時使薄荷醇從濾嘴釋放至煙中的量穩定化之内容。 [先前技術文獻] [專利文獻] [專利文獻1]日本特公昭43-28077號公報 7 322223 201204274 [專利文獻2]美國專利第4281671號說明書 [專利文獻3]美國專利第7074170號說明書【發明内容】本發明之目的係提供一種香煙濾嘴之製造方法，係在存放香煙時，可使香料從經香料加香之濾嘴釋放至煙中的量穩定化。本發明係一種香煙濾嘴之製造方法，係使用醋酸鹽絲束或醋酸鹽薄膜（acetate film)以製造香煙濾嘴之方法，其、散為.使香料參透至構成前述醋酸鹽絲束之醋酸鹽纖維或酷醆鹽薄膜之深部。本發明之方法亦可為如下述之方法：包含下述步驟：將纖維素醋酸鹽（cellul〇se acetate)溶解於溶媒中，且進仃紡紗、捲縮、乾燥捆包而製作醋酸鹽絲束之步驟；以及在别迷醋酸鹽絲束中添加可塑劑並捲起而製作滤嘴插塞之步驟；其中，在由前述纖維素醋酸鹽之溶液進行紡紗之前， :香料添加於前述纖維素醋酸鹽，藉此而使香料渗透至所製作之醋酸鹽纖維之深部。本發明之方法亦可為如下述之方法：包含下述步驟：將纖維素醋酸鹽溶解於溶媒中，且進行紡紗、捲縮、乾燥捆包而製作醋酸鹽絲束之步驟；以及在前述醋酸鹽絲束中添加可塑劑並捲起而製作濾嘴插塞之步驟；其中，在由前述纖維素醋酸鹽之溶液進行紡紗起直到製作前述醋酸鹽絲束之期間’將香料添加於前述纖維素醋酸鹽；並且在直到 J述Sf酸鹽滤嘴插塞之製造步驟完成為止，施行熱處理使 322223 8 201204274 香料擴散’喊香·透至前述⑽鹽纖維之深部。、本發明之方法亦可為如下述之方法：包含下述步驟：將纖維素醋酸鹽溶解於溶媒巾，且進行纺紗、捲縮、乾燥捆包而製作醋酸鹽絲束之步驟；以及在前述醋酸鹽絲束中、添加可塑劑並捲起而製作滤嘴插塞之步H中，在前述醋酸鹽絲束中添加可塑劑時添加香料；並且在直到前述醋酸顏嘴減之製造步歡成為止，施行減理使香料擴散，而使香料滲透至前述醋酸鹽纖維之深部。本發明之方法亦可為如下述之方法：㈣㈣薄片 (acetate flake)、可塑劑及香料溶解於溶媒而調製溶液，且由則述/谷液製作醋酸鹽薄膜並使香料滲透至前述醋酸鹽薄膜之深部，而由前述醋酸鹽薄膜製作香煙濾嘴。【實施方式】依據本發明之方法，係在濾嘴製造階段中預先使香料滲透至醋酸鹽纖維之深部。因此，從存放初期起，在醋酸鹽纖維内之香料之濃度梯度即為和緩’即使是在存放中，於醋酸鹽纖維中之香料之擴散速度亦慢，而香料擴散至醋酸鹽纖維深部的量亦變少。結果，在存放時之從濾嘴釋放至煙中之香料量的經時變化會變少。此外，對煙絲另行併用加香時，由於在存放時從煙絲分配裘濾嘴之香料會停留於醋酸鹽纖維表面，因此，可一面抑制香料釋放至煙中之量的經時變化，一面提升香料從濾嘴釋放的效率。以往在濾嘴製造階段中的香料加香’係如專利文獻1 所S載’雖例如與可塑劑（甘油三醋酸酯）添加同時進行， 9 322223 201204274 惟並未進行使香料渗透至醋酸鹽纖維之深部。與可塑劑（甘油三醋酸酯）添加同時進行香料加香時，由於香料滲透至醋酸鹽纖維之深部的速度變慢，因此在製造濾嘴後’香料會偏存於醋酸鹽纖維表面，且在存放中香料會滲透至醋酸鹽纖維之深部。第3圖係顯示本發明之香煙濾嘴之製造方法。如第3 圖所示，香煙濾嘴之製造方法係區分為纖維素醋酸鹽製造步驟、紡紗步驟、醋酸鹽濾嘴插塞製造步驟。在纖維^醋酸鹽製造步驟中，係藉由棉短絨（c〇tt〇nHnter)溶解紙漿之前處理、醋化、熟成、沉澱、精製來製造纖維素醋酸鹽' 在紡紗步驟中，係藉由混合纖維素醋酸鹽薄片、溶解於溶媒、過濾脫泡、紡紗、捲縮、乾燥捆包來製造醋酸鹽絲束。在醑酸鹽濾嘴插塞製造步驟中，係藉由絲束處理^添加塑劑（甘油三醋酸酯）、添加粒、捲包、捲取來製造醋酸鹽遽嘴插塞。 ^在本發明中，為了使香料滲透至醋酸鹽纖維之深部，係使用例如以下方法。 (1)在紡紗步驟中，在纖維素醋酸鹽薄片中添加料，而調製混合有香料之錯酸鹽原料。⑺在紡紗步驟中， 2解有醋酸鹽原料之丙酮（咖。ne)溶媒中添加香料。似2 A⑺之方Μ ’係經由之後的步驟，而可使香科滲透至醋酸鹽纖維之深部。优杳紗用在之纺^步/驟中，使香料溶解於醋酸鹽之濕式纺、之油劑（〇山ng agent)中。（4)在紡紗步驟中， 322223 10 201204274 將醋酸鹽絲束與香料釋放材料一同捆包於托板（pallet)。在（3)及（4)之方法中，較佳係在直到醋酸鹽濾嘴插塞之製造步驟結束為止，施行熱處理（例如存放在55乞下）使香料擴散’而使香料加速滲透至醋酸鹽纖維之深部。 (5)在醋酸鹽濾嘴插塞製造步驟中，將含有香料之可塑劑添加於醋酸鹽絲束。在（5)之方法中，亦較佳係在直到醋酸鹽濾嘴插塞之製造步驟結束為止，施行熱處理（例如存放在55 C下）使香料擴散，而使香料加速渗透至醋酸鹽纖維之深部。接著’說明在吸煙時從濾嘴釋放香料之效率的評估方法。在吸煙時從濾嘴釋放香料之效率，係可與藉由熱脫離法所測量之在低温域（至4〇°c為止）下之薄荷醇之熱脫離率有關。以下列方式試製薄荷醇香煙。將市售之薄荷醇香煙及柔和七星超淡煙，在各個濾嘴與香煙桿之間進行切斷，製作以黏接膠帶將薄荷醇香煙之濾嘴與柔和七星超淡煙之香煙桿予以連接的香煙樣本。以薄荷醇香煙而言，係從銷售店購入市售之mild SEVEN AQUA MENTHOL ONE BOX ' MILD SEVEN ONE MENTHOL BOX、SEVEN STARS LIGHT MENTHOL BOX、SEVEN STARS LIGHT MENTHOL、SALEM LIGHT BOX、SALEM ONE BOX、SALEM ALASKA MENTHOL、 MARLBORO ICEMINT BOX、MARLBORO ULTRA LIGHT MENTHOL BOX、MARLBORO BLACK MENTHOL BOX、 11 322223 201204274(aperture): 50# m pinhole (pinh〇le), objective lens: 1〇〇 times (NA – 0.9). The image form is set to an area map, and the step size of the X direction is i.〇em, and the step size of the Y direction is 1〇 // m. Further, the acetate fibers constituting each of the filters were imaged by optical microscopic observation. The appearance of the cross section of the acetate was obtained as a chemical image (chemicai image) based on the peak of 2943 cm1 from the salt-base substrate of Raman New. Further, according to the intensity ratio of the peak of 769 cm- by the mannitol of the Raman spectrum to the peak of 912 (10)· by the acetate substrate, menthol in the cross section of the curric acid fiber is obtained. Eight cloth is used as a chemical image. By using the intensity ratio of 2 peaks: the effect of interference. The distribution of menthol in the acetate fiber is as shown below under 322223 6 201204274. In the filter which was stored at 22 ° C for 2.5 months, menthol was partially deposited on the surface of the acetate fiber. In the filter which was stored at 22 ° C for 8 months, menthol penetrated into the deep part of the acetate fiber. In the filter which was stored at 55 ° C for one week (filter subjected to heat history), it was found that menthol was uniformly distributed in the acetate fiber. Therefore, as expected, the reduction in the amount of menthol released from the filter is apparently due to the penetration of menthol into the deep portion of the acetate fiber. Patent Document 1 discloses a method of dissolving menthol in triacetin, and a method of introducing menthol-impregnated tobacco into a filter according to Patent Documents 2 and 3, and the purpose is only to add menthol to the filter. And its purpose is not to control the distribution of menthol in acetate fibers. In Patent Document 1, since menthol and the sucrose higher fatty acid ester are easily left together in the form of a solid solution such as a binder or a colloid, there is a tendency to suppress the distribution of menthol in the acetate fiber. The possibility of change. However, the adsorption of components of the moisture-containing smoke is promoted by the lipophilicity and interfacial activity of the sucrose higher fatty acid ester, and the flavor at the time of smoking is affected. Further, menthol naturally proceeds uniformly in the direction of the permeation line in the deep portion of the acetate fiber. Therefore, as long as menthol is separated and diffused from the sucrose higher fatty acid ester, it penetrates into the deep part of the acetate fiber. Therefore, from Patent Document 1, there is no suggestion that the amount of menthol released from the filter into the smoke when storing the cigarette is stabilized. [Prior Art] [Patent Document 1] [Patent Document 1] Japanese Patent Publication No. Sho 43-28077 No. 7 322223 201204274 [Patent Document 2] US Patent No. 4,281,671 [Patent Document 3] US Pat. No. 7,074,170 The object of the present invention is to provide a method for producing a cigarette filter which stabilizes the amount of fragrance released from the perfume-scented filter into the smoke when the cigarette is stored. The present invention relates to a method for producing a cigarette filter, which is a method for producing a cigarette filter by using an acetate tow or an acetate film, which is obtained by dispersing the fragrance into the acetic acid constituting the acetate tow. The deep part of the salt fiber or cool salt film. The method of the present invention may also be a method comprising the steps of: dissolving cellulite acetate in a solvent, and spinning, crimping, and drying the bundle to prepare an acetate wire. a step of bundling; and a step of preparing a filter plug by adding a plasticizer to the acetate tow and rolling it up; wherein: before the spinning by the solution of the cellulose acetate, the fragrance is added to the fiber Acetate, whereby the perfume penetrates into the deep part of the acetate fiber produced. The method of the present invention may also be a method comprising the steps of: dissolving cellulose acetate in a solvent, and spinning, crimping, and drying the bale to prepare an acetate tow; and a step of adding a plasticizer to the acetate tow and winding up to form a filter plug; wherein, during the spinning from the solution of the cellulose acetate to the preparation of the acetate tow, the fragrance is added to the foregoing Cellulose acetate; and until the manufacturing step of the Sf acid salt filter plug is completed, heat treatment is performed to diffuse the 322223 8 201204274 fragrance into the deep part of the above (10) salt fiber. The method of the present invention may also be a method comprising the steps of: dissolving cellulose acetate in a solvent towel, and spinning, crimping, and drying the bale to prepare an acetate tow; In the acetate acetate tow, in the step H of adding a plasticizer and rolling up to form a filter plug, adding a fragrance when a plasticizer is added to the acetate tow; and in the manufacturing process until the acetic acid nozzle is reduced Once it is finished, the reduction is performed to spread the fragrance, and the fragrance is allowed to penetrate into the deep portion of the acetate fiber. The method of the present invention may also be a method as follows: (4) (iv) an acetate flake, a plasticizer and a perfume are dissolved in a solvent to prepare a solution, and an acetate film is prepared from the solution of the solution and the perfume is permeated to the acetate film. In the deep part, a cigarette filter is produced from the aforementioned acetate film. [Embodiment] According to the method of the present invention, the perfume is previously infiltrated into the deep portion of the acetate fiber in the filter manufacturing stage. Therefore, from the initial stage of storage, the concentration gradient of the fragrance in the acetate fiber is gentle. Even during storage, the diffusion rate of the fragrance in the acetate fiber is slow, and the fragrance diffuses to the depth of the acetate fiber. It has also become less. As a result, the amount of the fragrance released from the filter to the smoke at the time of storage becomes less. In addition, when the tobacco is separately used for flavoring, since the flavor of the filter is distributed from the shredded tobacco at the time of storage, the perfume will stay on the surface of the acetate fiber, so that the flavor can be suppressed while suppressing the amount of the flavor released into the smoke. The efficiency of release from the filter. In the past, the flavoring of the flavor in the filter manufacturing stage was carried out, for example, in the case of the patent document 1 S, although it was carried out simultaneously with the addition of a plasticizer (triacetin), 9 322223 201204274, but the permeation of the perfume to the acetate fiber was not carried out. Deep. When the perfume is added with the addition of the plasticizer (triacetin), the rate of penetration of the perfume into the deep part of the acetate fiber becomes slower, so after the filter is manufactured, the fragrance will be deposited on the surface of the acetate fiber, and The perfume in the deposit will penetrate into the deep part of the acetate fiber. Fig. 3 is a view showing a method of manufacturing the cigarette filter of the present invention. As shown in Fig. 3, the manufacturing method of the cigarette filter is divided into a cellulose acetate production step, a spinning step, and a acetate filter plug manufacturing step. In the fiber acetate manufacturing step, the cellulose acetate is produced by the cotton linters (c〇tt〇nHnter) before the pulp is dissolved, vinegared, matured, precipitated, and refined. In the spinning step, The acetate tow is produced by mixing cellulose acetate flakes, dissolving in a solvent, filtering, defoaming, spinning, crimping, and drying the bales. In the citrate filter plug manufacturing step, an acetate nipple plug is produced by a tow processing method of adding a plasticizer (triglyceride), adding granules, wrapping, and coiling. In the present invention, in order to infiltrate the fragrance into the deep portion of the acetate fiber, for example, the following method is used. (1) In the spinning step, a filler is added to the cellulose acetate flakes to prepare a mixed acid salt raw material. (7) In the spinning step, 2 a solvent is added to the acetone (coffee) solvent in which the acetate raw material is dissolved. A square of 2 A(7) is passed through the subsequent steps to allow the medicinal substance to penetrate into the deep part of the acetate fiber. The yam yarn is used in the spinning step, and the perfume is dissolved in the wet spinning of the acetate, the oil agent (〇山ng agent). (4) In the spinning step, 322223 10 201204274 The acetate tow is bundled with the fragrance-releasing material on a pallet. In the methods of (3) and (4), it is preferred to perform heat treatment (for example, storage under 55 )) to spread the fragrance until the end of the manufacturing step of the acetate filter plug to accelerate the penetration of the fragrance to the acetic acid. The deep part of the salt fiber. (5) In the acetate filter plug manufacturing step, a plasticizer containing a fragrance is added to the acetate tow. In the method of (5), preferably, until the end of the manufacturing step of the acetate filter plug, heat treatment (for example, storage at 55 C) is performed to diffuse the fragrance, and the fragrance is accelerated to permeate to the acetate fiber. Deep. Next, an evaluation method for the efficiency of releasing the fragrance from the filter at the time of smoking is explained. The efficiency of releasing the perfume from the filter during smoking can be related to the thermal detachment rate of menthol in the low temperature range (up to 4 ° C) as measured by the thermal detachment method. The menthol cigarette was tested in the following manner. The commercially available menthol cigarette and the soft seven-star super-light smoke are cut between each filter and the cigarette rod, and the filter of the menthol cigarette is connected with the soft seven-star super-light cigarette rod with adhesive tape. Cigarette samples. In the case of menthol cigarettes, commercially available Mild SEVEN AQUA MENTHOL ONE BOX ' MILD SEVEN ONE MENTHOL BOX, SEVEN STARS LIGHT MENTHOL BOX, SEVEN STARS LIGHT MENTHOL, SALEM LIGHT BOX, SALEM ONE BOX, SALEM ALASKA MENTHOL , MARLBORO ICEMINT BOX, MARLBORO ULTRA LIGHT MENTHOL BOX, MARLBORO BLACK MENTHOL BOX, 11 322223 201204274

MARLBORO MENTHOL BOX、MARLBORO BLACK MENTHOL ONE KS BOX、LARK ULTRA MENTHOL KS BOX'KENT ULTRA1 KS BOX'KENT CITRIC MENTHOL1 BOX、KOOL (以上均為香煙名稱）來使用。此外，試製相對於每重量單位之纖維素醋酸鹽絲束，甘油三醋酸酯含量為0、2、6、或9wt%之濾嘴。纖維素醋酸鹽係使用 2.2Y40000。在 MILDSEVEN ONE MENTHOL BOX所使用之煙絲中將薄荷醇予以加香。在煙絲中之薄荷醇加香量係設為6mg/香煙。將上述濾嘴連接於香煙桿，以試製薄荷醇香煙。以下列方式進行吸煙實驗。使用附掛20支香煙之線 (linear)型吸煙器（Filtrona公司製，SM400，ISO標準器）。設定抽吸頻率為每60秒1次、抽吸2秒鐘、抽吸容量為35mL、燃燒長度為從香煙前端算起之51mm，以作為吸煙條件。濾嘴開孔部係以膠帶封住而供實驗用。將煙予以捕集於劍橋式濾嘴，且於吸煙實驗後將劍橋式濾嘴以甲醇溶媒振盪萃取，且藉由氣相層析儀GC ( HEWLEtt PACKARD公司製6890series )來測量主流煙中之薄荷醇量。此外，將供吸煙實驗用之薄荷醇香煙之濾嘴以鑷子拔除’且以甲醇溶媒振|萃取，再將殘存之薄荷醇含量藉由 GC㈣量。將所測量之煙中之薄荷醇量，除以濾嘴中之殘存薄荷醇含量與煙中之薄荷醇量的合計，而將所得值作為從據嘴釋放薄荷醇之釋放效率。 322223 12 201204274 另-方面，以下列方式進行薄荷醇之熱脫離實驗。將吸煙實驗所用之薄#醇香煙之據嘴以錄子拔除並予以解纖，且採取濾、嘴纖維16mg充填於玻璃管（glasstube)。將充填有樣本之玻璃管裝設於熱脫附系統（Thermal Desorption System，亦即 TDS )( gerstel 公司製），一面流通載氣—gaS)(He)，一面依據升溫程式而將充填於管中。之樣本麟加熱。使從樣本麟之絲通過已加熱成20(TC之通路，且以保持為爾之低溫之捕集器（杜叩） ^集。結束管之升溫，將捕集器以取/分鐘急速地加 2露C：，且將未分離之捕集成分相濃縮並導入分離離，且以氣相層析儀/集^成分以分離管柱予以分MARLBORO MENTHOL BOX, MARLBORO BLACK MENTHOL ONE KS BOX, LARK ULTRA MENTHOL KS BOX'KENT ULTRA1 KS BOX'KENT CITRIC MENTHOL1 BOX, KOOL (all of which are cigarette names) are used. Further, a filter having a triacetin content of 0, 2, 6, or 9 wt% was produced with respect to the cellulose acetate tow per weight unit. Cellulose acetate is used in 2.2Y40000. Menthol is flavored in the cut tobacco used in MILDSEVEN ONE MENTHOL BOX. The menthol flavor in the cut tobacco is set to 6 mg/cigarette. The above filter was attached to a cigarette rod to try out a menthol cigarette. The smoking experiment was conducted in the following manner. A linear type smoking device (made by Filtrona, SM400, ISO standard) attached to 20 cigarettes was used. The suction frequency was set to be once every 60 seconds, suction for 2 seconds, suction capacity was 35 mL, and the burning length was 51 mm from the front end of the cigarette as a smoking condition. The filter opening portion is sealed with a tape for experimental use. The smoke was collected in a Cambridge filter, and after the smoking experiment, the Cambridge filter was extracted by methanol solvent shaking, and the mint in the mainstream smoke was measured by a gas chromatograph GC (6890 series manufactured by HEWLEtt PACKARD). The amount of alcohol. Further, the filter of the menthol cigarette used for the smoking test was extracted with a tweezers and extracted with methanol solvent, and the remaining menthol content was quantified by GC (four). The amount of menthol in the measured smoke was divided by the total amount of menthol remaining in the filter and the amount of menthol in the smoke, and the obtained value was taken as the release efficiency of menthol released from the mouth. 322223 12 201204274 In another aspect, the thermal detachment test of menthol was carried out in the following manner. The mouth of the thin alcoholic cigarette used in the smoking experiment was removed and decomposed by the recording, and 16 mg of the filter and mouth fiber was filled in a glass tube. The glass tube filled with the sample is placed in a thermal desorption system (TDS) (manufactured by Gerstel), and the carrier gas (gaS) (He) is flowed, and the tube is filled in the tube according to the temperature rising program. . The sample Lin heating. Let the filaments from the sample pass through the trap that has been heated to 20 (TC path, and keep the temperature at low temperature (cuckoo). End the tube's temperature rise, and add the trap to take/min. 2 Dew C:, and the unseparated capture phase is concentrated and introduced into the separation, and is separated by a gas chromatograph/collection component by a separation column.

TeChn〇1〇gies^ ^ ( ^ 衣队.7890A，MS : 597S「、办八乂 GC中之薄荷醇之峰值面積係與薄二° 所示。分別設定溫度為价升，皿及分析之步驟係如下靴、或 20(TC，而重:4〇 C、6〇t、80°C、1赃、保持30分鐘並在使捕二將樣本在預定之-定溫度中作。在各溫度下之薄荷B $脫離之後予以GC分析的操各溫度下之熱脫離量的累古=脫離量，係至該溫度為止之將熱脫離分析後之濾嘴^ 將殘存於濾嘴中之、谷媒振盪萃取，且藉由離資料，藉由以下公式复:醇予以定里。從所獲得之熱脫薄荷醇之熱脫離率。在低酿域（至4〇°C為止）下之 322223 13 201204274 在此，〇4〇係低溫域（至4(rc為止）之薄荷醇熱脫離率[%] ’八4〇係至40°C為止之GC之峰值面積累計值卜]， A·係至200°C為止之GC之峰值面積累計值[_]，仏⑽係至200 C為止之薄荷醇熱脫離率[%]，R係熱脫離後之濾嘴纖維16mg中之薄荷醇殘存量[mg]，τ係熱脫離前之濾嘴纖維16mg中之薄荷醇含量㈨幻。熱脫離前之濾嘴纖維 16mg中之薄荷醇含量T[mg]，係使用從濾嘴中之薄荷醇量及濾嘴重量所算出之薄荷醇含量來換算，而該濾嘴中之薄荷醇量係在計算從濾嘴釋放薄荷醇之釋放效率時所使用者。第4圖係顯示從濾嘴釋放薄荷醇之釋放效率、與在低溫域（至40°C為止）下之薄荷醇熱脫離率的關係。對於市售香煙係於購入後、而對於試製香煙（甘油三醋酸酯之含有率為〇至8wt%)則係於試製後，在2個：件下放置。第1個條件係設定為22。(：、相對濕度（RH) 60%。第2個條件係在收容於包裝（package)内之狀態下於55°C之乾燥機（ADVANTEC Fs_32q)内給予ι星^的熱履歷。在第4圖巾’係以黑色四角形顯示在第i個條件下之實驗結果’且以白色四角形顯示在第2個條件下之實驗結果。如第4圖所示，從濾嘴釋放薄荷醇之釋放效率，係與從熱脫離實驗所獲得的在低溫域下之薄荷醇熱脫離率^ 322223 14 201204274 關。因此，得知可藉由從㈣脫離之熱脫離（擴散）量來預測從遽嘴釋放薄荷醇之釋放量。之後，得知可採用由軌脫離實驗所得之在低溫域下之薄荷醇熱脫離率作為簡易之測量方法，以取代測量從濾嘴釋放薄荷醇此外，從第4圖可得知，若在听下給予薄荷醇香煙 1星期之熱履歷，則從濾嘴釋放薄荷醇之釋放率、亦即在在低溫域下之薄荷醇脫離率會顯著降低。此係相當於在夏季條件下存放後之煙中薄荷醇量之經時降低。因此，藉由以熱脫離實驗來測量在低溫域下之薄荷醇熱脫離率，;可來檢驗煙中薄荷醇量之經時變化之抑制效果。 (實施例1及2) [在將薄荷醇添加於醋酸鹽絲束之後，藉由施以高溫處理而使薄荷醇預吸附（pre-sorption)之濾嘴] 〇準備直徑為8mm、長度為25mm之纖維素醋酸鹽濾觜。將溥荷醇結晶放入燒杯（beaker)，進行加熱予以熔解，且使用微量吸管（micropipette)塗佈於濾嘴端面，藉此而在濾嘴中添加預定量的薄荷醇》薄荷醇添加量係設為 2.3mg (實施例1)或4.9mg (實施例2) 〇將所獲得之濾嘴置入密閉破璃容器中，且在乾燥機（ADVANTECFS-320) 中於55¾下保存Η天，藉此使薄荷醇滲透至構成濾嘴之酉曰酸鹽纖維深部。將所獲得之濾嘴稱為預吸附有薄荷醇之濾嘴。TeChn〇1〇gies^ ^ (^ 衣队.7890A, MS: 597S", the peak area of menthol in the gossip GC is shown as thin two °. Set the temperature to the price rise, the step of the dish and the analysis Attached to the following boots, or 20 (TC, and weight: 4 〇 C, 6 〇 t, 80 ° C, 1 赃, hold for 30 minutes and make the sample at a predetermined temperature in the second. At each temperature After the mint B $ is detached, the GC analysis is performed at the temperature of each temperature. The amount of heat removal is the amount of detachment, and the temperature is removed from the filter after the temperature is removed. Oscillation extraction, and by the separation of the data, by the following formula: alcohol to determine the heat from the obtained heat menthol hot detachment rate. Under the low brewing range (to 4 ° ° C) 322223 13 201204274 Here, the 低温4〇 system low temperature range (to 4 (rc) menthol hot detachment rate [%] 'eight 4 〇 to 40 ° C GC peak area cumulative value b], A · to 200 The cumulative value of the peak area of GC up to °C [_], the thermal detachment rate of menthol from 仏(10) to 200 C, and the menthol of 16 mg of filter fiber after R-thermal detachment Stock amount [mg], menthol content in 16 mg of filter fiber before τ system thermal detachment (9) illusion. Menthol content T [mg] in 16 mg of filter fiber before thermal detachment, using menthol from filter The amount of menthol calculated from the amount of the filter and the weight of the filter are converted, and the amount of menthol in the filter is calculated by calculating the release efficiency of menthol from the filter. Figure 4 shows the release of mint from the filter. The relationship between the release efficiency of alcohol and the thermal detachment rate of menthol in the low temperature range (up to 40 ° C). The commercially available cigarettes are purchased after the purchase, and the content of the triglyceride is reduced to 8wt%) is placed under two pieces after trial production. The first condition is set to 22. (:, relative humidity (RH) 60%. The second condition is contained in the package. In the state of 55 ° C dryer (ADVANTEC Fs_32q) gives the heat history of the ι star ^. In the 4th towel 'shows the experimental results under the ith condition in black squares' and is displayed in white square Experimental results under the second condition. As shown in Figure 4, the thin film is released from the filter. The release efficiency of alcohol is related to the thermal detachment rate of menthol in the low temperature range obtained from the thermal detachment experiment ^ 322223 14 201204274. Therefore, it is known that the amount of heat detachment (diffusion) can be predicted from (4) The mouth rinse releases the release amount of menthol. After that, it is known that the thermal detachment rate of menthol in the low temperature range obtained by the rail detachment test can be used as a simple measurement method instead of measuring the release of menthol from the filter. As can be seen from the figure 4, if the heat history of the menthol cigarette is given for one week, the release rate of menthol from the filter, that is, the menthol detachment rate in the low temperature range is remarkably lowered. This is equivalent to a decrease in the amount of menthol in the smoke after storage in summer conditions. Therefore, the thermal detachment rate of menthol in the low temperature range was measured by a heat detachment test; the inhibitory effect of the change in the amount of menthol in the smoke over time was examined. (Examples 1 and 2) [A filter for pre-sorption of menthol by applying high temperature treatment after adding menthol to the acetate tow] 〇 Preparation diameter 8 mm, length 25 mm Cellulose acetate filter. The ruthenium crystallization is placed in a beaker, heated and melted, and applied to the filter end face using a micropipette, whereby a predetermined amount of menthol added to the filter is added. Set to 2.3 mg (Example 1) or 4.9 mg (Example 2). The obtained filter was placed in a closed glass container and stored in a dryer (ADVANTEC FS-320) at 553⁄4. This causes the menthol to penetrate into the deep portion of the silicate fiber constituting the filter. The obtained filter is referred to as a filter pre-adsorbed with menthol.

將所製作之預吸附有薄荷醇之濾嘴，連接於薄荷醇香煙之香煙桿（將 MILDSEVEN AQUA MENTHOL ONE BOX 15 322223 201204274 之濾嘴予以去除者），以製作香煙。為了進行比較，使用未添加薄荷醇之纖維素醋酸鹽濾嘴（比較例1)，且以與上述相同方式製作香煙。所製作之樣本之概要係顯示於第1表。 [第1表] 濾嘴中之薄荷醇之預吸附量 [mg/香煙] 濾嘴中之薄荷醇濃度[wt%] 煙絲中之薄荷醇量 [mg/香煙] 比較例1 0 0 8.4 實施例1 2.3 2 6.4 實施例2 4.9 4 4.4 將樣本置入螺旋蓋管瓶中，且在40°c之恆溫恆濕機 (ESPEC股份有限公司製，LHU-113)下保存7天、29天、 56天、或70天。測量濾嘴中及煙絲中之薄荷醇含量、與從濾嘴脫離之薄荷醇熱脫離量。 (1)薄荷醇分配測量結果將濾嘴及煙絲中之薄荷醇以甲醇溶媒振盪萃取，且使用氣相層析儀GC ( HEWLETT PACKARD公司製 6890series)來定量。設Mf作為濾嘴中之薄荷醇、及Mt作為煙絲中之薄荷醇量，且將遽嘴中之薄荷醇分配率F以下述公式來表示。 F = Mf/ (Mf+Mt) 第5圖係顯示濾嘴中之薄荷醇分配率之經時變化。如 16 322223 201204274 第5圖所不’使用實施例1及2之預吸附有薄荷醇之濾嘴時，濾嘴中之薄荷醇分配率之經時變化小。 (2)薄荷醇熱脫離量之測量進行預吸附有薄荷醇之濾嘴之熱脫離實驗。熱脫離實驗除變更升溫及分析之步驟以外，其餘均以與上述相同方式進行。在此，分別將溫度設為22t、40。(：、8(TC、或200 c，而重複進行將樣本在預定之一定溫度中保持3〇分鐘並在使捕集成分脫離之後予以GC分析的操作。第6圖係顯示在低溫域下之薄荷醇之脫離率之經時變化。如第6圖所示，使用實施例丨及2之預吸附有薄荷醇之;慮嘴時在低溫域下之薄荷醇之熱脫離率會隨時間經過而增加，相較於使用比較例i之未預吸附之遽嘴之情形，熱脫離率提升為2至3倍。 #在實施例1中，從煙絲分配薄荷醇時，滤嘴中之薄荷醇會隨時間經過而增加（第5圖）。然而，可抑制從煙絲分，於渡嘴之薄荷醇滲透至醋酸鹽纖維深部。因此，可將薄熱脫料維持為，。在實施例2巾，即使從煙絲分配广何醇’I嘴中之薄荷醇量亦幾乎不會隨㈣經過變化（第越继）在實施例2中’亦已有充分量的薄荷醇存在於醋酸於读^木^。因此’在薄荷醇香煙包裝内部，從煙絲分配 -嘴之何醇’係被認為會偏存於醋酸鹽纖維之表攻。維，〃，、上、、、σ果可得知，藉由使薄荷醇預吸附於醋酸鹽纖、、’、】在存放薄荷醇香煙製品時，可抑制薄荷醇滲透至醋 322223 17 201204274 酸鹽纖維深部，而可抑制煙中薄荷醇量之經時變化，且可提升釋放效率。 (實施例3及4) [將纖維素醋酸鹽薄片以含薄荷醇之丙酮溶解，而製作之由薄膜所構成之預吸附有薄荷醇之樣本] 調製將纖維素醋酸鹽薄片（DAICEL公司製，L-40) 以成為濃度2w/v%之方式溶解於丙_ (和光純藥製，試藥特級）’且進一步對於纖維素醋酸鹽溶解9.23wt%之甘油三醋酸酯與〇.53wt%或1.39wt%之薄荷醇的溶液。另一方面’為了比較’將纖維素醋酸鹽薄片溶解於丙酮，且進一步僅洛解甘油三醋酸g旨、但不溶解薄荷醇，而調製溶液。將所獲得之丙酮溶液2mL澆注於内徑27mm之玻璃培養皿，在丙酮氣體環境下，於室溫靜置5天使丙酮緩緩自然揮發，且進一步在室溫下進行一整晚減壓乾燥以製作纖維素醋酸鹽薄膜。丙酮之揮發係以下列方式進行。在氣體置換乾燥器（desiccator) (As—丨公司製）内，並排5個加有30mL丙酮之l〇〇mL的高型燒杯（tallbeaker)，且在此 4同型燒杯之周圍並排4個洗有上述纖維素醋酸鹽溶液之玻璃培養皿，將顛倒覆蓋有lOOOmL燒杯者設為i組，而在板（plate)上並排9組。使氣體置換乾燥器之氣體出口為大氣開放，將氣體置換乾燥器内設為由丙酮以接近飽和蒸氣之方式而充滿的氣體環境，藉此即可充分使丙酮從澆注之纖維素醋酸鹽溶液中揮發之揮發速度變慢。如此，在製作薄膜時使纖維素醋酸鹽溶液之丙酮揮發速度變慢時， 18 322223 201204274 即可製作透明度高、且成分及構造均勻的薄膜。從玻璃培養皿剝離纖維素醋酸鹽薄膜，將内徑8mm 薄膜予以打孔，作成薄膜樣本。將所獲得之薄膜樣本中= 量為1.9±0.05mg者供實驗使用。以薄荷醇含有率為〇.53wt%之薄膜作為實施例3，i 薄荷醇含有率$ l39wt%之薄膜作為實施例4，以無薄荷醇之薄膜作為比較例2。、〜ϋ 對於所獲得之樣本，與實施例！及2之情形同樣地，測量在低溫域（至4(rc)下之薄荷醇之熱脫離率。結展’ 薄荷醇之熱脫離率，在實施例3中為4 7%，在實施例4 ’ 為7.4%。此等值係與從第4圖所示的在55<t下保存〜期並給予熱履歷之薄荷醇錢中所取出之遽嘴在低溫之熱脫離率、以及實施例！及2之熱脫離率為相同水準。因此，以濕式方式將薄荷醇混合於纖維素醋酸鹽薄片」：與「在將薄荷ϋ添加於纖維素醋料纖維之後施以高^ 理」相同地’被認為具有使薄荷醇預吸附於纖維素醋纖維深部之效果^ 取接著，以下列方式確認薄荷醇均勻地吸附於纖維素醋酸鹽薄膜深部。將線（ΚΑΝΕΒ〇纖維股份有限公司製^ (cotton)線20/200黑色）穿過所製作之薄膜樣本以黏接膠帶固定並懸吊於螺旋蓋管瓶之蓋的内侧，在螺旋蓋管瓶中將薄荷醇5g溶解於PEG200 (和光純藥製，二級） l〇mL而加人，作成薄荷醇氣體n將螺旋蓋管瓶在如 °C之恆溫恆濕機（eSPEC股份有限公司製，LHu_ii3)中 322223 201204274 保存2天、7天、27天之你、a，曰，之後’測1薄獏中之薄荷醇含量。料醇含量係藉由將薄膜進行 ⑽™KARD 公.689ws)_4。 Ϊ7圖係顯示薄荷醇含有率之經時變化。如第7圖所二；貫：例3及4之預吸附有薄荷醇之薄膜，相較於比較 :未預吸附薄荷醇之薄膜’薄荷醇含有率之經時變化少。亦即，可得知在實施例3及4之薄膜中，難以使溶解 =臟00之薄荷醇蒸氣吸附，且在開始存放經過不久後之吸附速度亦較慢。由此可得知，用太法稭由實施例3及4之所用方法，即可使溥荷醇充分渗透至薄膜深部。從以上結果可得知，藉由濕式方式使薄荷醇混合即可使薄荷醇預吸附於纖維素醋酸鹽 = 在存放具有由該纖維素酷酸鹽薄膜所製作之，慮嘴的薄荷醇香煙製品時，可抑制薄荷素醋酸鹽濾嘴深部。 /透至，義維【圖式簡單說明】圖。第i圖係顯示薄荷醇香煙之煙中薄荷醇量的經時變化 $ 2圖係顯示從濾、嘴釋放薄荷醇之量之_變化圖。第3圖係顯示本發明之香煙遽嘴之製造方法第4圖係顯示從濾嘴釋放薄荷醇之释 . 溫域^至贼為止）下之薄荷醇之___二在低第5圖係顯示關於實施例丨、2及比較例1 嘴中之薄荷醇分配率之經時變化圖。在遽 322223 20 201204274 第6圖係顯示關於實施例1、2及比較例1中，在低溫域下之薄荷醇脫離率之經時變化圖。第7圖係顯示關於實施例3、4及比較例2中，薄荷醇含有率之經時變化圖。【主要元件符號說明】無0 21 322223The prepared pre-adsorbed menthol filter was attached to a menthol cigarette rod (the filter of MILDSEVEN AQUA MENTHOL ONE BOX 15 322223 201204274 was removed) to make a cigarette. For comparison, a cellulose acetate filter to which menthol was not added (Comparative Example 1) was used, and a cigarette was produced in the same manner as above. A summary of the samples produced is shown in Table 1. [Table 1] Pre-adsorption amount of menthol in the filter [mg/cigarette] Menthol concentration in the filter [wt%] Amount of menthol in the tobacco [mg/cigarette] Comparative Example 1 0 0 8.4 Example 1 2.3 2 6.4 Example 2 4.9 4 4.4 The sample was placed in a screw cap bottle and stored at a constant temperature and humidity machine (LPE-113, manufactured by ESPEC Co., Ltd., 40 ° C) for 7 days, 29 days, 56 Day, or 70 days. The amount of menthol in the filter and the cut tobacco was measured and the amount of menthol removed from the filter was removed. (1) Measurement results of menthol distribution The menthol in the filter and cut tobacco was shaken and extracted with a methanol solvent, and quantified by a gas chromatograph GC (6890 series manufactured by HEWLETT PACKARD). Mf was used as the menthol in the filter, and Mt was used as the amount of menthol in the cut tobacco, and the menthol distribution ratio F in the mouth was expressed by the following formula. F = Mf / (Mf + Mt) Figure 5 shows the change over time in the distribution of menthol in the filter. For example, 16 322223 201204274 Fig. 5 does not use the filters of pre-adsorbed menthol of Examples 1 and 2, and the change in the distribution ratio of menthol in the filter is small. (2) Measurement of hot detachment amount of menthol A thermal detachment test of a filter pre-adsorbed with menthol was carried out. The heat detachment experiment was carried out in the same manner as described above except for the steps of changing the temperature rise and analysis. Here, the temperature is set to 22t and 40, respectively. (:, 8 (TC, or 200 c, and repeat the operation of holding the sample for 3 minutes at a predetermined temperature and performing GC analysis after the trapping component is removed. Fig. 6 shows the temperature in the low temperature range. The change in the detachment rate of menthol over time. As shown in Fig. 6, the pre-adsorption of menthol using Examples 丨 and 2; the thermal detachment rate of menthol in the low temperature range with time is considered. Increasing, the heat removal rate was increased by 2 to 3 times compared to the case of using the non-pre-adsorbed nozzle of Comparative Example i. # In Example 1, when menthol was dispensed from cut tobacco, the menthol in the filter would Increasing over time (Fig. 5). However, it is possible to inhibit penetration of the menthol from the tobacco into the deep portion of the acetate fiber. Therefore, the thin thermal stripping can be maintained as in Example 2, Even if the amount of menthol in the mouth of the tobacco distribution is almost no change with (4) (in the second step), in Example 2, a sufficient amount of menthol is present in the acetic acid to read the wood ^ Therefore, 'in the inside of the menthol cigarette package, from the shredded tobacco - the mouth of the alcohol' It is believed that it will be biased against the surface of acetate fiber. Dimensional, 〃, 、, 、, σ 可可可可藉存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放存放When the menthol is inhibited from penetrating into the deep portion of the vinegar 322223 17 201204274 acid salt, the change in the amount of menthol in the smoke can be suppressed, and the release efficiency can be improved. (Examples 3 and 4) [Cellulose acetate sheet Dissolved in a menthol-containing acetone to prepare a sample of pre-adsorbed menthol composed of a film] Preparation of a cellulose acetate salt sheet (L-40 manufactured by DAICEL Co., Ltd.) dissolved in a concentration of 2 w/v% a solution of 9.23% by weight of triacetin and 〇53% by weight or 1.39% by weight of menthol for cellulose acetate to be dissolved in the cellulose acetate. The solution was prepared by dissolving the cellulose acetate flakes in acetone and further decomposing only the glycerol triacetate g, but not dissolving the menthol. The 2 mL of the obtained acetone solution was poured into a glass petri dish having an inner diameter of 27 mm. In an acetone atmosphere, After standing at room temperature, 5 ounces of acetone slowly volatilized naturally, and further dried under reduced pressure overnight at room temperature to prepare a cellulose acetate film. The volatilization of acetone was carried out in the following manner. In a gas displacement dryer (desiccator) (As-manufactured by Asa Co., Ltd.), 5 tall beakers of l〇〇mL with 30 mL of acetone were placed side by side, and 4 cellulose acetate solutions were washed side by side around the 4 shaped beakers. The glass petri dish is set to be group i upside down and covered with 100 mL of beakers, and 9 groups are arranged side by side on the plate. The gas outlet of the gas displacement dryer is opened to the atmosphere, and the gas replacement dryer is set to be made of acetone. The gas atmosphere is filled close to the saturated vapor, whereby the volatilization rate of acetone from the cast cellulose acetate solution can be sufficiently slowed. Thus, when the acetone volatilization rate of the cellulose acetate solution is slowed down when the film is produced, 18 322223 201204274 can produce a film having high transparency and uniform composition and structure. The cellulose acetate film was peeled off from the glass culture dish, and a film having an inner diameter of 8 mm was perforated to prepare a film sample. The amount of the obtained film sample was 1.9 ± 0.05 mg for experimental use. A film having a menthol content of 53533% by weight was used as Example 3, a film having a menthol content of 3.99% by weight was used as Example 4, and a film having no menthol was used as Comparative Example 2. , ~ϋ For the samples obtained, and the examples! In the same manner as in 2, the thermal detachment rate of menthol in the low temperature range (to 4 (rc). The thermal detachment rate of menthol was measured, which was 4 7% in Example 3, in Example 4 ' is 7.4%. This value is the heat removal rate at the low temperature of the mouth of the mouth taken from the menthol money stored at 55 <t and given to the heat history as shown in Fig. 4, and examples! And the heat removal rate of 2 is the same. Therefore, the menthol is mixed in a wet manner with the cellulose acetate sheet": the same as "the high temperature is applied after adding the peppermint to the cellulose acetate fiber" 'It is considered to have the effect of pre-adsorbing menthol in the deep part of the cellulose vinegar fiber. Then, it was confirmed that menthol was uniformly adsorbed to the deep portion of the cellulose acetate film in the following manner. Cotton) 20/200 black) Pass through the prepared film sample with adhesive tape and suspend it on the inside of the lid of the screw cap bottle, and dissolve 5g of menthol in PEG200 in the screw cap vial (Wako Pure Chemical Co., Ltd.) System, level 2) l〇mL and add people to make menthol n The screw cap bottle is stored in a constant temperature and humidity machine (LSP_ii3, manufactured by eSPEC Co., Ltd., 322223 201204274) for 2 days, 7 days, 27 days, a, 曰, and then The menthol content is calculated by subjecting the film to (10) TMKARD male .689ws) _4. The Ϊ7 graph shows the temporal change in the menthol content. As shown in Fig. 7, the film of pre-adsorbed menthol of Examples 3 and 4 was compared with the comparison: the film of menthol not pre-adsorbed with menthol had little change with time. That is, it was found that in the films of Examples 3 and 4, it was difficult to adsorb the menthol vapor of the dissolution = dirty 00, and the adsorption speed was short after the start of storage. From this, it can be seen that the tartaric alcohol can be sufficiently infiltrated into the deep portion of the film by the method used in Examples 3 and 4. From the above results, it can be known that menthol is pre-adsorbed to cellulose acetate by mixing menthol in a wet manner = menthol cigarette having a mouth made of the cellulose silicate film In the case of a product, the deepness of the peppermint acetate filter can be suppressed. / Through, Yi Wei [Simple diagram] Figure. Figure i shows the change in the amount of menthol in the smoke of a menthol cigarette. The $2 graph shows the change in the amount of menthol released from the filter and mouth. Fig. 3 is a view showing the method of manufacturing the cigarette spout of the present invention. Fig. 4 is a view showing the release of menthol from the filter. The temperature of the menthol is ___ two in the lower fifth figure. The time-dependent changes in the distribution ratio of menthol in the mouths of Examples 丨, 2 and Comparative Example 1 are shown. In Fig. 322223 20 201204274 Fig. 6 is a graph showing changes with time in the menthol detachment rate in the low temperature range in Examples 1, 2 and Comparative Example 1. Fig. 7 is a graph showing changes with time in the content of menthol in Examples 3 and 4 and Comparative Example 2. [Main component symbol description] None 0 21 322223

Claims

201204274 七、申請專利範圍： 1. 一種香煙濾嘴之製造方法，係使用醋酸鹽絲束（acetate tow)或醋酸鹽薄膜（acetate film)以製造香煙濾、嘴之方法，其特徵為：使香料滲透至構成前述醋酸鹽絲束之醋酸鹽纖維(acetate fiber)或醋酸鹽薄膜之深部。 2. 如申請專利範圍第1項所述之香煙濾嘴之製造方法，其包含下述步驟：將纖維素醋酸鹽（cellulose acetate)溶解於溶媒中，且進行紡紗、捲縮、乾燥捆包以製作醋酸鹽絲束之步驟；以及在前述醋酸鹽絲束中添加可塑劑並捲起以製作濾嘴插塞(filterplug)之步驟；其中，在由前述纖維素醋酸鹽之溶液進行紡紗之前，將香料添加於前述纖維素醋酸鹽，藉此而使香料滲透至所製作之醋酸鹽纖維之深部。 3. 如申請專利範圍第1項所述之香煙濾嘴之製造方法，其包含下述步驟：將纖維素醋酸鹽溶解於溶媒中，且進行紡紗、捲縮、乾燥捆包以製作醋酸鹽絲束之步驟；以及在前述醋酸鹽絲束中添加可塑劑並捲起以製作濾嘴插塞之步驟；其中，在由前述纖維素醋酸鹽之溶液進行紡紗起直到製作前述醋酸鹽絲束之期間，將香料添加於前述纖維素醋酸鹽；並且在直到前述醋酸鹽濾嘴插塞之製造步驟完成為止，施行熱處理使香料擴散，而使香料滲透至前述醋酸鹽纖維之深部。 4. 如申請專利範圍第1項所述之香煙濾嘴之製造方法，其 22 322223 201204274 包含下述步驟：將纖維素醋酸鹽溶解於溶媒中，且進行紡紗、捲縮、乾燥捆包以製作醋酸鹽絲束之步驟；以及在前述醋酸鹽絲束中添加可塑劑並捲起以製作濾嘴插塞之步驟；其中，在前述醋酸鹽絲束中添加可塑劑時添加香料；並且在直到前述醋酸鹽濾嘴插塞之製造步驟完成為止，施行熱處理使香料擴散，而使香料渗透至前述醋酸鹽纖維之深部。 5_如申請專利範圍第1項所述之香煙濾嘴之製造方法，其中，將醋酸鹽薄片（acetate flake )、可塑劑及香料溶解於溶媒而調製溶液，且由前述溶液製作醋酸鹽薄膜而使香料滲透至前述醋酸鹽薄膜之深部，而由前述醋酸鹽薄膜製作香煙濾嘴。 6.如申請專利範圍第1至5項中任一項所述之香煙濾嘴之製造方法，其中，前述香料係薄荷醇。 23 322223201204274 VII. Patent application scope: 1. A method for manufacturing a cigarette filter, which is a method for manufacturing a cigarette filter or a mouth by using an acetate tow or an acetate film, which is characterized in that: It penetrates into the deep portion of the acetate fiber or the acetate film constituting the acetate tow. 2. The method for producing a cigarette filter according to claim 1, comprising the steps of: dissolving cellulose acetate in a solvent, and spinning, crimping, and drying the bundle. a step of producing an acetate tow; and a step of adding a plasticizer to the acetate tow and rolling up to prepare a filter plug; wherein, before spinning by the solution of the cellulose acetate described above The perfume is added to the cellulose acetate described above, whereby the perfume penetrates into the deep portion of the produced acetate fiber. 3. The method for producing a cigarette filter according to claim 1, comprising the steps of: dissolving cellulose acetate in a solvent, spinning, crimping, and drying to form an acetate. a step of tow; and a step of adding a plasticizer to the acetate tow and rolling up to form a filter plug; wherein, after spinning from the solution of the cellulose acetate, until the preparation of the acetate tow During this period, the fragrance is added to the cellulose acetate; and until the manufacturing step of the acetate filter plug is completed, heat treatment is performed to diffuse the fragrance, and the fragrance penetrates into the deep portion of the acetate fiber. 4. The method for producing a cigarette filter according to claim 1, wherein 22 322223 201204274 comprises the steps of: dissolving cellulose acetate in a solvent, and spinning, crimping, and drying the package. a step of preparing an acetate tow; and a step of adding a plasticizer to the acetate tow and rolling up to form a filter plug; wherein a flavor is added to the acetate tow; and a fragrance is added; Until the manufacturing step of the acetate filter plug is completed, heat treatment is performed to diffuse the fragrance, and the fragrance penetrates into the deep portion of the acetate fiber. The method for producing a cigarette filter according to the first aspect of the invention, wherein the acetate flake, the plasticizer and the fragrance are dissolved in a solvent to prepare a solution, and the acetate film is produced from the solution. The fragrance is allowed to permeate into the deep portion of the acetate film, and a cigarette filter is produced from the acetate film. The method for producing a cigarette filter according to any one of claims 1 to 5, wherein the fragrance is menthol. 23 322223