CN103703116B - 香料担载吸附剂粒子、香烟用过滤嘴、带过滤嘴的香烟及香料担载吸附剂粒子的制造方法 - Google Patents
香料担载吸附剂粒子、香烟用过滤嘴、带过滤嘴的香烟及香料担载吸附剂粒子的制造方法 Download PDFInfo
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- CN103703116B CN103703116B CN201280035193.3A CN201280035193A CN103703116B CN 103703116 B CN103703116 B CN 103703116B CN 201280035193 A CN201280035193 A CN 201280035193A CN 103703116 B CN103703116 B CN 103703116B
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- Prior art keywords
- spice
- filter
- adsorber particles
- supports
- cigarette
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Abstract
本发明提供一种香料担载吸附剂粒子,其具备具有700m2/g以上的BET比表面积的吸附剂核粒子、和担载于所述吸附剂核粒子表面且含有香料及保持所述香料的香料保持材料的香味产生介质,其中,所述香料保持材料以所述香料担载吸附剂粒子的总重量的5~20%的量存在,所述香料以所述保持材料的重量的10~50%的量存在。
Description
技术领域
本发明涉及一种香料担载吸附剂粒子、香烟用过滤嘴、带过滤嘴的香烟及香料担载吸附剂粒子的制造方法。
背景技术
在香烟过滤嘴中装入担载了香料的活性炭粒子,源自该香料的香味释放于香烟主流烟中,对其进行品味。例如专利文献1公开了一种在活性炭等粒子状载体的表面包覆有含有香料的葡聚糖膜的香料珠。该香料珠通过下述方法制造:将粒子状载体放入流动造粒干燥机,一边鼓入例如80℃以下的暖风一边将含有香料的葡聚糖水溶液或水分散液连续或间歇地喷雾于粒子状载体的表面,并使其干燥。
但是,在专利文献1的方法中,在处理大量的香料的情况下,较耗费时间,其结果,难以增加香料担载量。
现有技术文献
专利文献
专利文献1:WO2008/072627
发明内容
发明所要解决的问题
因此,本发明的第一目的在于,以较短时间的处理提供担载较大量的香料的香料担载吸附剂粒子。
另外,本发明的目的在于,提供一种含有这种香料担载吸附剂粒子的香烟用过滤嘴、及带过滤嘴的香烟。
进而,本发明的目的在于,提供一种香料担载吸附剂粒子的制造方法。
用于解决问题的方法
为了解决上述问题,根据本发明的第一方面,提供一种香料担载吸附剂粒子,其具备:具有700m2/g以上的BET比表面积的吸附剂核粒子、和担载于所述吸附剂核粒子表面且含有香料及保持所述香料的香料保持材料的香味产生介质,其中,所述香料保持材料以所述香料担载吸附剂粒子的总重量的5~20%的量存在,所述香料以所述保持材料的重量的10~50%的量存在。
另外,根据本发明的第二方面,提供一种香烟过滤嘴,其具备:含有本发明的香料担载吸附剂粒子的过滤部。进而,根据本发明的第三方面,提供一种带过滤嘴的香烟,其具备:香烟杆、和与所述香烟杆的一端连接的本发明的香烟过滤嘴。
进而,根据本发明的第四方面,提供一种香料担载吸附剂粒子的制造方法,该方法包括:一边在减压下对具有700m2/g以上的BET比表面积的吸附剂核粒子进行搅拌,一边将含有香料和香料保持材料的液态的香味释放组合物喷雾在所述吸附剂核粒子上。
发明的效果
根据本发明,可以以较短时间的处理提供担载较大量香料的香料担载吸附剂粒子。
附图说明
图1为表示用于制造本发明的香料担载吸附剂粒子的装置的一个例子的概略剖面图;
图2为表示本发明的一个实施方式的带过滤嘴的香烟的概略剖面图;
图3为表示本发明的其它实施方式的带过滤嘴的香烟的概略剖面图;
图4是表示捕捉香烟主流烟中成分的装置的部分剖面概略图;
图5为表示所担载的香料及香料保持材料的量的测定结果的图。
符号说明
10…圆锥型螺条式混合机/干燥机、12…处理槽、121…处理槽的倒圆锥部、122…处理槽的圆筒部、12a…处理物的排出口、14…双螺旋带状搅拌桨、16…旋转轴、18a~18e…支承杆、20a~20b…涡流消除器、22…夹套、22a…蒸汽导入口、22b…蒸汽排出口、24…顶板、26…电动机、28…减速机、24a…被处理物的投入口、30…袋滤器、32…冷凝器、321…冷凝器的内筒、322…冷凝器的外筒、P1…减压泵、34…喷嘴、36…液态的香味释放组合物(LFC)收纳容器、P2…送液泵、38…温度传感器、40…吸附剂核粒子(AP)收纳容器、
50,60…带过滤嘴的香烟、52…香烟杆、521…烟草填充材料、522…香烟卷纸、54,62…过滤嘴、541…装有香料担载吸附剂粒子的过滤部、542…普通过滤部、FCA…香料担载吸附剂粒子、541a,542a…醋酸纤维素纤维、
541b,542b,66…过滤嘴卷绕纸、56…接装纸、621…第一普通过滤部、622…第二普通过滤部、64…空腔、
70…香烟主流烟中成分的捕捉装置、711…剑桥过滤嘴、CIG…香烟、71…粒状物质的捕捉器、71a…烟草主流烟流入口、71b…烟草主流烟流出口、72…采样器、TA…捕捉烟草主流烟中的气相成分的药液、73…杜瓦瓶、RM…制冷剂、74,75…导管、76…自动吸烟器、76a…抽吸口
具体实施方式
下面,对本发明的实施方式详细地进行说明。
本发明的香料担载吸附剂粒子具备:吸附剂核粒子、和担载于上述吸附剂核粒子表面且含有香料及保持该香料的香料保持材料的香味产生介质。上述香料保持材料以上述香料担载吸附剂粒子的总重量的5~20%的量存在,上述香料以上述保持材料的重量的10~50%的量存在。
本发明中所使用的吸附剂核粒子具有700m2/g以上的BET比表面积。在本说明书中,BET比表面积是指依据公知的BET法求出的比表面积。如果BET比表面积不足700m2/g,则不能充分吸附香烟主流烟中的成分。在本发明中,吸附能以作为香烟主流烟中代表性成分之一的丙酮等为基准。吸附剂核粒子优选具有1000m2/g以上的BET比表面积。吸附剂核粒子的BET比表面积通常为2000m2/g以下。
这种吸附剂核粒子的例子包括活性炭粒子、沸石粒子、硅胶粒子。
吸附剂核粒子优选具有75~1000μm的平均粒径,例如可优选使用平均粒径为75μm~600μm的粒子。
包覆吸附剂核粒子表面的香味产生介质含有香料、和保持该香料的香料保持材料。
香料的例子包括亲水性香料和疏水性香料。亲水性香料的例子包括烟叶提取物、天然植物性香料(例如甘草、长角豆、李子提取物、桃提取物等)、酸类(例如苹果酸、酒石酸、柠檬酸、丁酸等)、糖类(例如葡萄糖、果糖、高果糖浆等)。疏水性香料的例子包括薄荷醇、可可类(粉末、提取物等)、酯类(例如醋酸异戊酯、酢酸芳樟酯、丙酸异戊酯、丁酸芳樟酯等)、天然精油类(作为植物性精油,例如为香草提取物、绿薄荷、胡椒薄荷、决明子、茉莉等;作为动物性精油,例如为麝香、龙涎香、灵猫香、海狸香等)、单体香料(例如为茴香脑、柠檬烯、沉香醇、丁香酚、香草醛等)。
保持香料的保持材料包括膜形成材料及根据需要的乳化剂。本发明中所使用的膜形成材料的代表例为葡聚糖,葡聚糖例如包括支链淀粉、麦芽糊精、羟基丙基纤维素。葡聚糖为水溶性。葡聚糖等膜形成材料可以通过在由其形成的膜中加入香料来保持香料。膜形成材料相对于亲水性香料、疏水性香料的任一种均可以使用。
乳化剂的例子包括甘油脂肪酸酯、蔗糖脂肪酸酯(糖酯)、山梨糖醇酐脂肪酸酯、丙二醇脂肪酸酯、卵磷脂。在水性介质中,乳化剂分子通过将这些疏水性基团吸附于疏水性香料的油滴周围而保持疏水性香料,干燥后也保持疏水性香料。
在本发明的香料担载吸附剂粒子中,香料保持材料以香料担载吸附剂粒子的总重量的5~20%的量、优选5~10%的量存在。而且,香料以香料保持材料的重量的10~50%的量存在。
本发明的香料担载吸附剂粒子可以通过下述方法制备:一边在减压下对吸附剂核粒子进行搅拌,一边将含有香料和香料保持材料的液态的香味释放组合物喷雾在吸附剂核粒子上。
液态的香味释放组合物中所含的香料如上所述,香料保持材料也如上所述。
在液态的香味释放组合物仅含有亲水性香料作为香料的情况下,该组合物通常含有作为膜形成材料的葡聚糖、和亲水性香料,进而,优选含有作为溶解葡聚糖和亲水性香料的溶剂的水。
在液态的香味释放组合物含有疏水性香料作为香料的情况下(例如在液态香料发生组合物仅含有疏水性香料作为香料的情况下、或与亲水性香料一起含有疏水性香料作为香料的情况下),该香味释放组合物优选含有作为膜形成材料的葡聚糖、作为葡聚糖的溶剂的水、疏水性香料(及亲水性香料)、溶解疏水性香料的油性溶剂(例如植物性油脂或饱和脂肪酸三甘油酯、优选中链饱和脂肪酸三甘油酯)和乳化剂。该组合物在除疏水性香料外还含有亲水性香料的情况下,其亲水性香料溶解于水。
在制造香料担载吸附剂粒子时,在喷雾液态的香味释放组合物期间,吸附剂核粒子优选置于12.3kPa以下的减压下、例如7.4~12.3kPa的减压下。另外,此时,吸附剂核粒子优选在60℃以下的温度、例如40~60℃的温度。通过在减压下喷雾含有香料和香料保持材料的液态的香味释放组合物,可以使大量的香料担载于吸附剂核粒子,并且也具有可使高粘度的香味释放组合物(例如2Pa·s左右的粘度)从喷嘴喷雾这样的优点。
为了制造本发明的香料担载吸附剂粒子,可以利用圆锥型螺条式混合机/干燥机。圆锥型螺条式混合机/干燥机例如记载于日本特开2003-71263公报、日本特开2003-290641公报、日本特开2007-229633公报,另外,可由大川原制作所购得。
参照图1对这样的圆锥型螺条式混合机/干燥机的基本结构进行说明。图1概略地以剖面表示圆锥型螺条式混合机/干燥机10的一个例子。圆锥型螺条式混合机/干燥机10在内部进行混合/干燥处理,具备由倒圆锥部121和连接在其上的圆筒部122构成的处理槽12。具备设置在处理槽12内的双螺旋带状搅拌桨14。在处理槽12内中央纵向延伸的旋转轴16上,螺旋带状搅拌桨14安装于将该旋转轴16互相分开并固定的多个支承杆(在图1中为支承杆18a~18e)。在螺旋桨14的上方,在处理槽12的圆筒部122的内壁固定有例如由一对板状体构成的涡流消除器20a、20b。涡流消除器20a、20b使因带状搅拌桨14的作用沿处理槽12的内壁上升的处理物(在本发明中为吸附剂粒子)向处理槽12的中央附近移动,并且落于处理槽12的下部。
处理槽12的外周包有夹套22,为了加热容器内容物,在该夹套22内从蒸汽导入口22a通过管线L1导入蒸汽,其蒸汽从蒸汽排出口22b通过管线L2排出至体系外。
容器的上部开口部被顶板24封闭。在该顶板24上设置有电动机26和减速机28,减速机28的输出轴与处理槽12内所设置的旋转轴16连结。另外,顶板24设有被处理物(在本发明的情况下为吸附剂核粒子)的投入口24a,处理槽12的底部设有处理物(在本发明的情况下为香料担载吸附剂粒子)的排出口12a。
进而,顶板24安装有袋滤器30。该袋滤器捕捉处理槽12的内容物中的粒状物(在本发明的情况下为吸附剂粒子),使挥发物(在本发明的情况下为香味释放组合物中的水)通过,将其经由管线L3导入冷凝器32。冷凝器32由例如水冷式冷却器构成,挥发物通过内筒321内,挥发物被从管线L5导入外筒322内的冷却水冷却,成为冷凝液(水),从管线L6排出。导入于外筒322的水从管线L5排出。经由内筒管线L7与减压泵P1连接,通过驱动该减压泵P1来将处理槽12内减压。
圆锥型螺条式混合机/干燥机的基本结构如上所述,但为了制备本发明的香料担载吸附剂粒子,设置成用于将液态的香味释放组合物导入处理槽12内的喷嘴34贯穿顶板24,并从收纳液态的香味释放组合物LFC的容器36通过具备送液泵P2的管线L8将液态的香味释放组合物喷雾于处理槽12内。另外,在处理槽12的下部设置用于测定处理槽12内的吸附剂粒子的温度的温度传感器(例如热电偶)38。
为了使用图1所述的圆锥型螺条式混合机/干燥机10制造本发明的香料担载吸附剂粒子,在处理槽12内使收纳于容器40的吸附剂核粒子AP经由管线L9导入处理槽12内。通过在夹套22内导入温度80℃以上、优选温度100~120℃的蒸汽来对处理槽12内进行加热,通过电动机26的驱动一边使双螺旋带状搅拌桨14旋转而搅拌吸附剂粒子一边使收纳于容器36的液态的香味释放组合物通过送液泵P2的驱动经由管线L8从喷嘴34喷雾于处理槽12内。该喷雾中,优选将吸附剂粒子的温度保持为70℃以下、优选为60℃以下。通过导入于夹套22内的80℃以上的蒸汽来加热并蒸发导入于处理槽12内的液态的香味释放组合物中的水时,可通过从吸附剂粒子中夺去水的蒸发热来保持这样的吸附剂粒子的温度。
如上制造的香料担载吸附剂粒子仅在制造中挥发除去水分,制造中应用于吸附剂核粒子的液态香味释放组合物中除水分以外的成分基本都担载于吸附剂核粒子。因此,应用于吸附剂核粒子的液态香味释放组合物含有相对于所使用的吸附剂核粒子重量的5~20%、优选5~10%的量的香料保持材料,且含有相对于液态香味释放组合物中所含的香料保持材料重量的10~50%的量的香料。另外,可以将液态的香味释放组合物中所含的香料保持材料、特别是膜形成材料的一部分水溶液或者水分散液预先应用于吸附剂核粒子。膜形成材料的一部分水溶液或者水分散液的预先应用可抑制香料担载吸附剂粒子在制造初期中吸附剂核粒子的温度上升,另外,可抑制由吸附剂产生微粉末。
另外,本发明的香料担载吸附剂粒子在初期状态下可发挥相当于吸附剂核粒子固有的吸附能的50%以上的吸附能,优选相当于吸附剂核粒子固有的吸附能的70%以上的吸附能,更优选相当于吸附剂核粒子固有的吸附能的90%~大致100%的吸附能。在此,初期状态是指,香料担载吸附剂粒子与香烟主流烟接触前的状态。如以上所述,吸附剂核粒子固有的吸附能以香烟主流烟中的丙酮为基准。即,当本发明的香料担载吸附剂粒子与香烟主流烟接触时,可以立刻吸附香烟主流烟中的成分。随着香料担载吸附剂粒子与香烟主流烟接触,香料担载吸附剂粒子的香味产生介质中的香料保持材料由于香烟主流烟中的极性成分,特别是水分,而溶解,吸附能逐渐增大。当然,贮藏中香料几乎不会从香料产生介质释放。
本发明的第二方面的香烟过滤嘴具备含有本发明的香料担载吸附剂粒子的过滤部。而且,本发明的第三方面的带过滤嘴的香烟提供一种具备香烟杆、和与上述香烟杆的一端连接的本发明的过滤嘴的带过滤嘴的香烟。
本发明的香烟过滤嘴可含有在通常的过滤嘴原料例如醋酸纤维素纤维丝束(通过三醋酸甘油酯等增塑剂粘结)中分散有本发明的香料担载吸附剂粒子的过滤部。可在该过滤部的一端连接所谓的普通过滤部(由利用三醋酸甘油酯等增塑剂粘结的醋酸纤维素丝束构成)。或者,本发明的香烟过滤嘴可含有分开配置的两个普通过滤部、和填充在这两个普通过滤部间的空间的本发明的香料担载吸附剂粒子。
图2为具备本发明的一个实施方式的香烟用过滤嘴的香烟(带过滤嘴的香烟)50的概略剖面图。带过滤嘴的香烟50具备将烟丝等烟草填充材料521用香烟卷纸522卷装而成的香烟杆52。香烟杆52与通常的香烟相同。
在香烟杆52的一端附设有过滤嘴54。过滤嘴54具备与香烟杆52的一端直接相接而设置的装有香料担载吸附剂粒子的过滤部541、和相对于主流烟的流动方向设置于过滤部541的下游侧端的普通过滤部542。
装有香料担载吸附剂粒子的过滤部541以过滤嘴卷绕纸541b卷装分散有香料担载吸附剂粒子FCA的例如醋酸纤维素纤维541a,可以通过与通常的木炭过滤嘴相同的方法制作。
普通过滤部542以过滤嘴卷绕纸542b卷装例如醋酸纤维素纤维542a的丝束。
由过滤部541及542构成的过滤嘴54与通常的带过滤嘴的香烟一样,利用接装纸56安装于香烟杆52。
图3为具备本发明的另一实施方式的香烟用过滤嘴的香烟(带过滤嘴的香烟)60的概略剖面图。在该带过滤嘴的香烟60中,利用接装纸56安装于香烟杆52的过滤嘴62具备:直接安装于香烟杆52的一端的第一普通过滤部621、和与该第一普通过滤部621空开间隔而设置的第二普通过滤部622,其整体利用过滤嘴卷绕纸66卷装。第一及第二普通过滤部621及622具有与图2所示的普通过滤部相同的结构。在第一普通过滤部621和第二普通过滤部622之间的空间(空腔)64中填充有本发明的香料担载吸附剂粒子FCA。
实施例
<液态的香味释放组合物的制备>
将以表1所示比例含有的下述表1所示成分的混合物利用乳化机(Primix公司制ROBOMICSMARKII)以7500rpm乳化15分钟。此时,以混合物的温度不会超过45℃的方式用水冷却乳化机的周围。如上得到液态的香味释放组合物A~D。
另外,作为中链脂肪酸三甘油酯,使用花王公司制的CoconardMT,作为卵磷脂,使用日清Oillio公司制的LP-20E,作为糖酯,使用三菱化学食品公司制的P-1570。
[表1]
<香料担载吸附剂粒子的制备>
实施例1
在此,使用大川原制作所制圆锥型螺条式混合机/干燥机RiboconeRM-50-SR(参照图1)。将活性炭(KurarayChemical公司制KuraraycoalGGS-H28/70;平均粒径:0.4mm、BET比表面积:1700m2/g)15kg和5重量%支链淀粉水溶液6kg投入于上述混合/干燥机,在夹套内于200kPa的压力下使温度120℃的蒸汽循环,将混合/干燥机内的压力设定为12.3kPa,搅拌活性炭。进行5分钟搅拌后,将7.5kg液态香味释放组合物A经60分钟从喷嘴喷雾于混合/干燥机内后,进一步进行搅拌干燥5分。将香料担载吸附剂粒子从混合/干燥机中取出,迅速地放入连续流动造粒干燥装置(大川原制作所制Mixgrade0.5型),进行3分钟的活性炭粒子中的显热交换及除湿,得到香料担载吸附剂粒子制品。
实施例2
使用液态的香味释放组合物B代替液态的香味释放组合物A,除此以外,通过与实施例1同样的步骤得到香料担载吸附剂粒子制品。
实施例3
使用液态的香味释放组合物C代替液态的香味释放组合物A,除此以外,通过与实施例1同样的步骤得到香料担载吸附剂粒子制品。
实施例4
使用液态的香味释放组合物D代替液态的香味释放组合物A,除此以外,通过与实施例1同样的步骤得到香料担载吸附剂粒子制品。
<带过滤嘴的香烟的制作>
制作图3所示结构的带过滤嘴的香烟。具体而言,用镊子从具备具有醋酸纤维素纤维丝束作为过滤嘴原料的过滤嘴的市售的带过滤嘴的香烟制品“WinstonLight”除去作为过滤嘴原料的醋酸纤维素纤维丝束后,在该空腔部填充醋酸纤维素纤维丝束(长度10mm;2.5Y/35000(即,单纤度2.5旦尼尔;单纤维剖面Y型;总纤度35000旦尼尔)),填充实施例1~4中得到的香料担载吸附剂粒子30mg(香烟杆的轴方向的空间部64的长度2mm),最后填充醋酸纤维素纤维丝束(长度10mm;2.5Y/35000),制作图3所示结构的带过滤嘴的香烟。另外,直接使用不担载香料的活性炭(KurarayChemical公司制KuraraycoalGGS-H28/70)30mg代替实施例1~4中得到的香料担载吸附剂粒子,除此以外,与上述同样地制作带过滤嘴的香烟(以下,称为对照香烟)。
确认在吸这4种本发明的带过滤嘴的香烟时,主流烟中源自香料的香味被释放,并且与对照的带过滤嘴的香烟相比,香味增强。这些结果显示根据本发明的方法,能够以短时间的处理将大量的香料担载于吸附剂核粒子。
比较例
除了对活性炭只喷雾5重量%l-薄荷醇的乙醇溶液以外,与实施例1同样地制备香料担载吸附剂粒子。使用该香料担载吸附剂粒子,与上述同样地制作带过滤嘴的香烟。吸该带过滤嘴的香烟,但未确认到源自香料的香味。
实验例
吸实施例4中制作的带过滤嘴的香烟,考察主流烟中的丙酮吸附能。
在该实验中,为了捕捉香烟主流烟中成分,使用图4所示的装置70。该装置70具有粒状物质的捕捉器71,所述粒状物质的捕捉器71具备剑桥过滤嘴711(直径47mm)、保持香烟CIG的烟草主流烟流入口71a及烟草主流烟流出口71b。进而,装置70具备采样器72。采样器72内收纳有捕捉烟草主流烟中的气相成分的药液TA。在本实验中,放入含有茴香脑200ppm作为内标物质的甲醇10mL作为药液TA。采样器72收纳于收纳有用于将捕捉药液TA保持为低温的制冷剂RM的杜瓦瓶73内。在本实验中,使用干冰和异丙醇的混合物作为制冷剂RM,在实验中,将捕捉药液TA保持为-70℃以下的温度。粒状物质捕捉器71的流出口71b连接有延伸至采样器72内的药液TA中的导管74。而且,在自动吸烟器76的抽吸口76a连接有采样器72内的延伸至捕捉药液TA上部空间内的导管75。若点燃香烟并驱动自动吸烟器76,则通过经由导管75的抽吸将采样器72内减压,随之使烟草主流烟通过捕捉器71内的剑桥过滤嘴711。此时,烟草主流烟中的粒状物质被剑桥过滤嘴711捕捉,除去了粒状物质的主流烟经由导管74导入于采样器72内的捕捉药液TA内,起泡,并将主流烟中的气相成分捕捉于捕捉药液TA。
在本实验中,将实施例4中制作的香烟安装于捕捉器71,利用自动吸烟器76以ISO的标准吸烟条件(1喷烟:2秒钟吸烟35mL、喷烟间隔:58秒)吸烟。吸烟结束后,将采样器72内的药液移至血清瓶,在其中放入捕捉了粒状物质的剑桥过滤嘴711,以250次/分钟振荡萃取30分钟。将该萃取液1mL放入GC/MS分析用玻璃瓶,在以下的条件下分析主流烟中成分。
主流烟中成分的分析条件:
·GC/MS:Hewlett-Packard制HP7890/5975
·柱:DB-1701
·柱流量:1.2mL/分钟
·升温条件:在60℃保持5分钟后,以5℃/分钟升温至160℃,以10℃/分钟升温至250℃,保持30分钟。
·注射:分流比10:1;注入口220℃;流量12mL/分钟;总流量16.2mL/分钟
·MS条件:扫描参数33.0~200.0;阈值50;MS离子源230℃;MS四极150℃。
对带普通过滤嘴的香烟(具有市售的带过滤嘴的香烟制品“WinstonLight”的香烟杆,并在其一端连接有由醋酸纤维素纤维丝束(长度20mm;2.5Y/70000)构成的普通过滤嘴;以下,称为基准香烟)及上述对照香烟也进行同样的分析。
由实施例4的带过滤嘴的香烟、对照香烟及基准香烟的分析结果分别算出丙酮的峰面积值,将实施例4的带过滤嘴的香烟及对照香烟的丙酮峰面积值分别除以基准香烟的丙酮峰面积值,并将该值乘100倍而求出丙酮降低率(%),从100%中减去其丙酮降低率(%)而算出丙酮吸附率。其结果,对照香烟的丙酮吸附率为48%,实施例4的带过滤嘴的香烟的丙酮吸附率为45%。该结果表示:实施例4的香料担载粒子具有相当于吸附剂核粒子的固有吸附能的约94%的吸附能。即,实施例4的带过滤嘴的香烟与含有不担载香料的活性炭的对照香烟相比,虽然吸附能偏低,但发挥大致相同的吸附能。
实施例1~3中制作的过滤嘴香烟也发挥与实施例4的带过滤嘴的香烟相同的吸附能。
参考例
除了将活性炭置换成比表面积为700m2/g及1000m2/g的活性炭30mg以外,制作与上述对照香烟同样的2种带过滤嘴的香烟。对于这些香烟,与上述同样地考察丙酮吸附率,前者的香烟为23%,后者的香烟为34%。由此可知,如果比表面积为700m2/g以上,则对香烟主流烟中的成分的吸附具有效果。
<担载的香料及香料保持材料的量的测定>
对实施例1~4中得到的香料担载粒子测定担载的香料的量及香料保持材料的量。
依据现有技术文献(WO2008/072627)的例1~3制备比较例的香料担载粒子,对于所制备的香料担载粒子,同样地测定所担载的香料的量及香料保持材料的量。
比较例的香料担载粒子如下制备。
比较例1(现有技术文献的例1)
在预先制备的支链淀粉10重量%的支链淀粉水分散液中添加咖啡油2重量%。将该混合液在乳化机中进行强搅拌(乳化机转速2500rpm),制备香料分散液。另一方面,将平均粒径250μm的碳酸钙粒子100g放入流动造粒干燥机,以0.6m/秒的流速鼓入75℃的暖风,迅速地间歇喷雾上述香料分散液(喷雾1分钟后停止喷雾30分钟,重复该循环),将合计10g的香料分散液喷雾于碳酸钙粒子表面并干燥。然后,迅速地将流动层内冷却至室温,得到期望的香料珠。
比较例2(现有技术文献的例2)
将平均粒径250μm的碳酸钙粒子100g放入流动造粒干燥机,一边以1.0m/秒的流速鼓入30℃的暖风一边连续地喷雾含有添加了香草醛的烟草用香料1重量%和支链淀粉9重量%的香料混合水溶液,将合计5g的混合水溶液喷雾于碳酸钙粒子表面并干燥。然后,迅速地将暖风温度降低至室温,以0.4m/秒的流速冷却,得到期望的香料珠。
比较例3(现有技术文献的例3)
在预先制备的支链淀粉10重量%的支链淀粉水分散液中添加咖啡油1重量%及卵磷脂0.5重量%。将该混合液在乳化机中进行强搅拌(乳化机转速7500rpm、15分钟),制备香料分散液。另一方面,将平均粒径250μm~1.4mm的粉碎咖啡豆粒子300g放入旋转流动造粒干燥机(Preund产业(株)制SFC-MINI),将底部旋转多孔板以约500rpm、造粒防止用搅拌桨以约400rpm旋转,以0.6m/秒的流速鼓入75℃的暖风,形成粉碎咖啡豆粒子的流动层。一边将上述香料分散液保温为40℃,一边连续地对该流动层进行喷雾,由此,将合计90g的香料分散液喷雾于咖啡豆粒子表面并干燥。然后,迅速地将暖风温度降低至室温,以0.4m/秒的秒速冷却,得到期望的香料珠。
香料的量及香料保持材料的量如下测定。
香料的测定:
用精制水、甲醇混合液对香料担载粒子进行振荡萃取。将萃取液供于气相色谱图质量分析仪(GC/MS)并测定香料。
香料保持材料的测定:
称量香料担载粒子(重量A),以除去粒子内水分为目的进行加热干燥(干燥后的重量B)。对干燥后的粒子加入精制水进行振荡萃取,使香料保持材料溶出。将萃取后的粒子进一步进行加热干燥(干燥后的重量C)。将重量C和重量A的差值作为香料保持材料量。
将测定结果示于图5。图5以香料担载粒子相对于总重量的比例(重量%)表示所担载的香料的量及香料保持材料的量。图5显示本发明的香料担载粒子比比较例的香料担载粒子担载更大量的香料。
另外,本发明的香料担载粒子可以比比较例的香料担载粒子以更短时间的处理制备。
Claims (5)
1.一种香料担载吸附剂粒子的制造方法,该方法包括:一边在减压条件下对具有700m2/g以上的BET比表面积的吸附剂核粒子进行搅拌,一边将含有香料和葡聚糖的液态的香味释放组合物喷雾在所述吸附剂核粒子上。
2.如权利要求1所述的香料担载吸附剂粒子的制造方法,其中,所述液态的香味释放组合物以所述香料担载吸附剂粒子总重量的5~20%的量含有所述葡聚糖,以所述葡聚糖重量的10~50%的量含有上述香料。
3.如权利要求1或2所述的香料担载吸附剂粒子的制造方法,其中,所述减压条件为12.3kPa以下的压力。
4.如权利要求1或2所述的香料担载吸附剂粒子的制造方法,其中,在所述喷雾中,将所述吸附剂核粒子保持为60℃以下的温度。
5.如权利要求3所述的香料担载吸附剂粒子的制造方法,其中,在所述喷雾中,将所述吸附剂核粒子保持为60℃以下的温度。
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PCT/JP2012/067724 WO2013011898A1 (ja) | 2011-07-15 | 2012-07-11 | 香料担持吸着剤粒子、シガレット用フィルタ、フィルタ付きシガレットおよび香料担持吸着剤粒子の製造方法 |
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CN105011361B (zh) * | 2015-07-17 | 2018-11-09 | 云南中烟工业有限责任公司 | 一种液体分子嵌入式非燃烧加香材料的制备方法 |
CN105001988B (zh) * | 2015-07-17 | 2018-07-24 | 云南中烟工业有限责任公司 | 一种三层夹心结构香料缓释滤嘴添加剂的制备装置及其应用方法 |
TW201703657A (zh) | 2015-07-17 | 2017-02-01 | 菲利浦莫里斯製品股份有限公司 | 用於吸菸製品的活性碳珠 |
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CN112790425A (zh) * | 2019-11-13 | 2021-05-14 | 湖南中烟工业有限责任公司 | 一种香味缓释层状材料及其制备和在加热不燃烧烟草制品中的应用 |
CN111916656A (zh) * | 2020-07-21 | 2020-11-10 | 合肥通用机械研究院有限公司 | 一种用于三元材料的集成式生产系统 |
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