【発明の詳細な説明】
〔産業上の利用分野〕
本発明は特定の条件における減圧蒸留にて留出して得ら
れる香料の低沸点成分と揮発性溶媒を含有してなる室内
散布用香料組或物に関し、更に詳しくは、噴霧使用を繰
り返しても残香性がなく、常にフレッシュな本来の芳香
を得ることができる室内散布用香料組或物に関する．
〔従来の技術及び発明が解決しようとする課題〕従来の
室内芳香剤は、溶液状やゲル状のものが多く、これらは
、一般には溶媒の自然蒸散によって香りを漂よわすもの
でありその匂い立ちを強調する目的から拡散力の強い香
料が使用される事が多く、さわやかな好ましい香りを創
ることが難かしかった．又、ハンドスプレーやエアゾー
ル形式の室内芳香剤にあっては広い空間に瞬時に、香り
を漂よわす事が可能であるが、しかしながら、散布回数
の増加に伴い床や壁に香−りが付着累積してしみになっ
たり、本来目的とする芳香と異なる重い香りが残存し、
これが、室内芳香剤としてのさわやかさやフレッシュ感
を損ねてしまう欠点がある．
〔課題を解決するための手段〕
本発明者らは上記課題を鑑み、鋭意研究した結果、後記
特定の条件における減圧蒸留にて留出して得られる香料
の低沸点成分と揮発性溶媒を含有してなる室内散布用香
料＆！！戒物は残香性がなく、常にフレンシュな本来の
芳香を提供し、また室内に香りやしみが付着しないこと
を見出し、本発明を完戒するに至った．
本発明は、０． ２ ｍ ｍ Ｈ ｇ − ０． ５
ｍ ｍ Ｈ Ｈの減圧下に於いて、３０℃〜１１０℃の
昇温により留出して得られる香料の低沸点成分と揮発性
溶媒を含有してなる室内散布用香料組戒物である．本発
明でいう室内散布用香料組戒物とは、室内芳香剤などの
ように人体以外、特に大気中に噴霧させるための香料で
あり、噴霧タイプ（スプレータイプ）でもコロンやオー
ドトワレなどのように直接人体に用いる香料はこの限り
ではない．本発明に用いられる香料は通常汎用されてい
るものであればよく、例えば、ジャスミンオイル，ロー
ズオイル．カーネーションオイル．バイオレットオイル
，ヒアシンスオイル，ボアドローズオイル，ベチバーオ
イル．ナツメグオイル．ネロリオイル．ラベンダーオイ
ル．オレンジオイル，レモンオイル，ベルガモットオイ
ル，ナルシサスオイル．イランイランオイル．サンダル
ウッドオイル等の天然香料、ビネン．リモネン，ヘキサ
ノール，エチルアセテート，オシメン，リナリルアセテ
ート．リナロール．ゲラニオール，シトラール，シネオ
ール，ベンズアルデヒド，アニスアルデヒド，バニリン
．カルボン，イオノン，ダマセノン，インドール，ジャ
スミンラクトン，ゲラニルアセテート．ボルニルアセテ
ート等の本発明の蒸留条件に適合する沸点を有する合戒
香料、およびこれらの香料を組み立ててなる調合香料な
どがあげられる．
本発明に於いては、これらの香料を通常の方法で減圧蒸
留して得られた低沸点或分を用いるのであるが、その蒸
留条件は０． ２ ｍ ｍ Ｈ ｇ〜０．５ｍｍＨｇの
減圧下に於いて３０℃〜１１０゜Ｃの昇温により留出し
たものを用いることができる．また、本発明に於いて二
種以上の香料の低沸点戒分を用いる場合は、各々を減圧
蒸留して低沸点成分を得てからこれらを組み合わせる方
法、組みあわせた後に減圧蒸留して低沸点或分を得る方
法などいずれの方法でもよい．
本発明に用いられる揮発性溶媒は、沸点１００゜Ｃ以下
の溶媒が用いられ、例えば水、エタノール，イソプロビ
ルアルコール等の低級アルコール、ＬＰＧガス（液化石
油ガス），フレオンガス及びこれらの類似物等が挙げら
れ、これらの一種以上を用いる．
本発明に於いて香料の低沸点成分と揮発性溶媒を組み合
わせる方法は次の通りである．上記香料の少なくとも一
種以上を、合計して大略０． ５〜５重量％（以下ｗｔ
％と略記する）を上記揮発性溶媒に溶解させる．揮発性
溶媒としてＬＰＧガス，フレオンガス及びこれらの類似
物を用いる場合には、これらが噴射剤も兼ねているので
他の噴射剤は必要ないが、これらの揮発性溶媒を用いな
い場合には、空気．窒素．炭酸ガス等の圧縮ガスによる
噴射剤を含有させて室内散布用香料組成物を得る．
本発明の室内散布用香料組底物は、ハンドスプレーやエ
アゾール形式の形態，オートタイマー等により適当な間
隔を設定して室内に噴霧させる形態などの様々な形態に
適用可能である．〔実施例〕
以下実施例及び比較例によって本発明を詳述する．
尚、実施例中で用いた残香性及び香り試験方法＾，Ｂは
下記の通りである．
（残香性及び香り試験方法Ａ〜同一の香りによるテスト
）
圧縮空気圧をタイマーで適当にコントロールし、１５分
間隔で５秒間噴霧するように電磁弁を開閉調節したボン
ベを用い、これに各試料を入れ、このボンベを同じ広さ
の空室に置き、１０日連続（１日につき６時間）で噴霧
させた．
噴霧中の香りの評価と毎日の噴霧終了後２時間後の残香
性の比較を１０人の専門パネラーによって１日各１回計
ｌθ回繰り返して判定した．｛残香試験方法Ｂ〜異なる
香りによるテスト｝上記試験方法Ａで用いたものと同一
に調節されたボンベを用いた。香りの異なる試料を別々
のボンベ１．２に入れ同室に設置した．まずボンベｌを
３時間作動させ、その後ボンベ２を１時間作動させるよ
うに制御した．
ボンベ２の作動終了３０分後の残香性の評価を１０人の
専門パネラーによって１０回繰り返して判定した．
実施例１，比較例ｌ
（ｉ）香料の低沸点成分の調製
丸型フラスコにラベンダーオイル１． ０ ｋ ｇを入
れ、減圧蒸留装置を取り付けた＊０，２ｍｍｌｇ〜０．
５ ｍ ｍ Ｈ Ｈの範囲で減圧し、オイルバス中で
温度３０℃から１１０℃まで昇温させ、その間毎分約２
〜３ｍｌの留出速度で初留分を採取した。最終的には７
２０ｇのラベンダーオイル低沸点或分が採取された．
（ ｉｉ ）室内散布用香料組或物の調製及び試験上記
で得られたラベンダーオイル低沸点成分及び未蒸留のラ
ベンダーオイルを用いて下記の組或にて試料をｔＪ４製
し、前記『残香性及び香り試験方（ｗｔ ％）
第１表から明らかな如く、本発明の香料組或物は常にフ
レッシュな香りが保たれ、使用後も残香が少ない優れた
ものであった．一方、比較用の香料組成物は重い香りが
残り、ラベンダーオイルが持つ本来のさわやかな香りを
随時得ることができ第 １ 表 評価結果
（表中数値は延べ人数−１００人を示す）実施例２〜３
（ｉ）香料の低沸点戒分の調製
丸型フラスコにジャスミンオイル１． ０ ｋ ｇを入
れ、減圧蒸留装置を取り付ける＊ Ｏ− ２ ｍ ｍ
Ｈ ｇ〜０． ５ ｍ ｍ Ｈ ｇ″ｉ？減圧し、オイ
ルバス中で温度３０゜Ｃ〜１１０゜Ｃまで昇温させ、そ
の間毎分２〜３Ｎ１の留出速度で留分を採取した．最終
的には４９０ｇのジャスミンオイル低沸点成分が採取さ
れた．上記で得られたジャスミンオイル低沸点戒分とリ
モネンを１二〇で組み合わせてシトラス系香料の低沸点
戒分をｉＪ製した（実施例２）．また、同様に、ジャス
ξンオイル低沸点成分とリナロールを２：８で組み合わ
せてフローラル系香料の低沸点成分を調製した（実施例
３）．
（１１）室内散布用香料Ａｌｌ戒物の調製及び試験上記
で得られた香料を用い下記の組成にて試料を調製し、ボ
ンベ１に実施例２を、ボンベ２に実施例３を入れ、前記
ｒ残香性及び香り試験方法ＢＪを行った．その結果を第
２表に示した．第２表から明らかな如く、本発明の香料
組底物は残香が少なく、続けて異なる香りに切り替えて
も前の香りと混ざらずに新たな香りを得ることができる
優れたものであった．
第 ２ 表 評価結果
（表中数値は延べ人数＝１００人を示す）実施例４ エ
アゾール形弐の室内芳香剤（ｉ）香料の低沸点成分の調
製
丸型フラスコに下記組或で組み立てた香料１．０ｋｇを
入れ、減圧蒸留装置を取り付けた．０．２ｍ ｍ Ｈ
ｇ 〜０． ５ ｍ ｍ Ｈ ｇの範囲で減圧し、オイ
ルバス中で温度３０゜Ｃから１１０℃まで昇温させ、こ
の間毎分約２〜３ｍｌの留出速度で留分を採取した．最
終的には８７０ｇの低沸点が採取された．（組或）
（ｗｔ％）シネオール
２ベンズアルデヒド
１オシ，７７
αビネン ３オレンジオ
イル ２レモンオイル
８ベルガモットオイル
５ベンジルアセテート
１５インドール１０％溶液 ５ジャス
ミンオイル １０リナロール
４ミュゲベース
３５イランイランオイル
３（１１）室内散布用香料組成物の調製
上記で得られた香料の低沸点成分を用い下記の＆ＩＩ威
にてエアゾール形式の室内芳香剤を調製した．（組成）
（ｗｔ％）前記香料の
低沸点戊分 ２．０９５％未変性エタ
ノール ４５．０ＬＰＧガス
５０．０蒸留水
３． ０（！！法）
エタノールを攪拌し、これに香料の低沸点或分を添加し
て均一に溶解した後、所要量の水を加えた．これをエア
ゾール容器に収容した後、ＬＰＧガスをエアゾール容器
内の上記溶液の中に吹き込み（充填して）、室内芳香剤
を調製した．実施例５ エアゾール形式の室内芳香剤（
ｉ）香料の低沸点成分の調製
丸型フラスコに下記組或で組み立てた香料１．０ｋｇを
入れ、減圧蒸留装置を取り付けた．０．２ｍ ｍ Ｈ
ｇ 〜０． ５ ｍ ｍ Ｈ ｇの範囲で減圧し、オイ
ルバス中で温度３０“Ｃから１１０℃まで昇温させ、そ
の間毎分約２〜３ｍｆｆｉの留出速度で留分を採取した
。最終的には７００ｇの低沸点成分が採取された。[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a fragrance composition for indoor spraying containing a volatile solvent and a low boiling point component of a fragrance obtained by distillation under reduced pressure under specific conditions. More specifically, the present invention relates to a fragrance composition for indoor spraying that does not leave a residual scent even after repeated spraying and can always provide a fresh original fragrance. [Prior art and problems to be solved by the invention] Conventional room air fresheners are often in the form of solutions or gels, and these generally emit a scent due to the natural evaporation of a solvent. Fragrances with strong diffusive power are often used to emphasize standing, making it difficult to create a pleasant, refreshing scent. In addition, hand spray and aerosol type indoor air fresheners can instantly diffuse a scent into a large space, but as the number of sprays increases, the scent accumulates and accumulates on floors and walls. It may cause stains, or a heavy scent that differs from the original fragrance may remain.
This has the disadvantage of impairing the refreshing and fresh feeling of a room air freshener. [Means for Solving the Problems] In view of the above problems, the present inventors have conducted extensive research and have found that a fragrance containing low boiling point components and volatile solvents obtained by distillation under reduced pressure under the specific conditions described below. Fragrance for indoor spraying &! ! We discovered that the precepts do not have a lingering scent, always provide a fresh natural fragrance, and do not leave scents or stains in the room, leading to the completion of the present invention. The present invention provides 0. 2 mm Hg - 0. 5
This is a fragrance compound for indoor spraying containing a volatile solvent and a low boiling point component of a fragrance obtained by distillation by raising the temperature from 30°C to 110°C under a reduced pressure of m m H H. In the present invention, a fragrance compound for indoor spraying is a fragrance that is intended to be sprayed into the atmosphere other than the human body, such as an indoor air freshener, and even if it is a spray type, it can be sprayed into a spray type such as cologne or eau de toilette. This does not apply to fragrances used directly on the human body. The fragrance used in the present invention may be any commonly used fragrance, such as jasmine oil, rose oil, etc. Carnation oil. Violet oil, hyacinth oil, bore rose oil, vetiver oil. Nutmeg oil. Neroli oil. Lavender oil. Orange oil, lemon oil, bergamot oil, narcissus oil. Ylang ylang oil. Natural fragrances such as sandalwood oil, vinegar. Limonene, hexanol, ethyl acetate, ocimene, linalyl acetate. Linalool. Geraniol, citral, cineol, benzaldehyde, anisaldehyde, vanillin. Carvone, ionone, damascenone, indole, jasmine lactone, geranyl acetate. Examples include synthetic fragrances having a boiling point compatible with the distillation conditions of the present invention, such as bornyl acetate, and blended fragrances made by assembling these fragrances. In the present invention, a low-boiling point fraction obtained by distilling these fragrances under reduced pressure using a conventional method is used, and the distillation conditions are 0. It is possible to use a product distilled by raising the temperature to 30° C. to 110° C. under a reduced pressure of 2 mm Hg to 0.5 mm Hg. In addition, in the case of using two or more types of low boiling point components of fragrances in the present invention, it is possible to distill each of them under reduced pressure to obtain low boiling point components and then combine them, or to combine them and then distill them under reduced pressure to obtain low boiling point components. Any method of obtaining a certain amount is fine. The volatile solvent used in the present invention is a solvent with a boiling point of 100°C or less, such as water, ethanol, lower alcohols such as isopropyl alcohol, LPG gas (liquefied petroleum gas), Freon gas, and similar substances thereof. Use one or more of these. In the present invention, the method of combining the low boiling point component of the fragrance and the volatile solvent is as follows. The total amount of at least one of the above fragrances is approximately 0. 5 to 5% by weight (hereinafter wt
(abbreviated as %) in the above volatile solvent. When using LPG gas, Freon gas, and similar substances as volatile solvents, no other propellant is necessary as these also serve as propellants, but when these volatile solvents are not used, air ．． nitrogen. A fragrance composition for indoor spraying is obtained by containing a propellant using compressed gas such as carbon dioxide gas. The fragrance composition for indoor spraying of the present invention can be applied in various forms, such as hand spray, aerosol format, and spraying indoors at appropriate intervals using an automatic timer or the like. [Examples] The present invention will be explained in detail below using Examples and Comparative Examples. Incidentally, the fragrance lingering property and fragrance test method ^,B used in the examples are as follows. (Fragrance lingering and fragrance test method A - Test using the same scent) Using a cylinder with a solenoid valve controlled to open and close so that the compressed air pressure was appropriately controlled with a timer and sprayed for 5 seconds at 15 minute intervals, each sample was placed in the cylinder. The cylinder was placed in an empty room of the same size and sprayed for 10 consecutive days (6 hours per day). The evaluation of the scent during spraying and the comparison of the residual scent 2 hours after the end of daily spraying were conducted by 10 expert panelists, once a day for a total of 1θ times. {Fragrance Residual Test Method B ~ Test with Different Smells} A bomb regulated identically to that used in Test Method A above was used. Samples with different scents were placed in separate cylinders 1.2 and placed in the same room. First, cylinder 1 was operated for 3 hours, and then cylinder 2 was operated for 1 hour. The residual fragrance of cylinder 2 was evaluated 30 minutes after completion of operation by 10 expert panelists who repeated the evaluation 10 times. Example 1, Comparative Example 1 (i) Preparation of low boiling point components of fragrance In a round flask, add 1.5 oz of lavender oil. *0.2 mmlg to 0.0 kg and attached a vacuum distillation device.
The pressure was reduced in the range of 5 mm H H, and the temperature was raised from 30°C to 110°C in an oil bath, during which time the temperature was approximately 2 m/min.
The first fraction was collected at a distillation rate of ~3 ml. In the end 7
20g of low boiling lavender oil was collected. (ii) Preparation and testing of a fragrance composition for indoor spraying Using the lavender oil low boiling point component obtained above and undistilled lavender oil, a sample was prepared using the following composition, and the above-mentioned "persistence and fragrance composition" were prepared. Fragrance test method (wt %) As is clear from Table 1, the fragrance composition of the present invention always maintained a fresh fragrance and was excellent with little residual fragrance even after use. On the other hand, the comparative fragrance composition had a heavy scent, and the original refreshing scent of lavender oil could be obtained at any time. ~3 (i) Preparation of low-boiling point ingredients for fragrance Place 1. Insert 0 kg and attach vacuum distillation equipment* O-2 mm
Hg~0. The pressure was reduced to 5 mm H g''i?, and the temperature was raised to 30°C to 110°C in an oil bath, during which time a fraction was collected at a distillation rate of 2 to 3 N1 per minute.Finally, 490 g A low boiling point component of jasmine oil was collected.The low boiling point component of the jasmine oil obtained above was combined with limonene at a ratio of 120 to produce a low boiling point component of a citrus fragrance (Example 2). Similarly, a low boiling point component of a floral fragrance was prepared by combining the low boiling point component of Jasmine oil and linalool at a ratio of 2:8 (Example 3). (11) Preparation and testing of indoor spray fragrance All precepts Samples were prepared with the following composition using the fragrance obtained in step 1, Example 2 was placed in cylinder 1, and Example 3 was placed in cylinder 2, and the above-mentioned r scent persistence and fragrance test method BJ was conducted. It is shown in Table 2. As is clear from Table 2, the fragrance composition of the present invention has little residual scent, and even when switching to a different scent in succession, a new scent can be obtained without mixing with the previous scent. Table 2: Evaluation results (the numbers in the table indicate the total number of people = 100 people) Example 4 Aerosol type 2 room air freshener (i) Preparation of low boiling point component of fragrance The following was placed in a round flask. 1.0 kg of the assembled fragrance was put into the container, and a vacuum distillation device was attached.0.2 mm H
g ~0. The pressure was reduced to 5 mm Hg, and the temperature was raised from 30°C to 110°C in an oil bath, during which time fractions were collected at a distillation rate of about 2 to 3 ml per minute. In the end, 870g of low boiling point material was collected. (group)
(wt%) Cineole
2 Benzaldehyde
1 Oshi, 77 α-vinene 3 Orange oil 2 Lemon oil
8 bergamot oil
5 Benzyl acetate
15 Indole 10% solution 5 Jasmine oil 10 Linalool
4 Myuge base
35 ylang ylang oil
3 (11) Preparation of fragrance composition for indoor spraying Using the low boiling point component of the fragrance obtained above, an aerosol-type indoor fragrance was prepared according to the following process. (composition)
(wt%) Low boiling point fraction of the above fragrance 2.095% undenatured ethanol 45.0 LPG gas
50.0 distilled water
3. 0 (!! method) Ethanol was stirred, a certain amount of the low boiling point fragrance was added thereto, and after uniformly dissolving, the required amount of water was added. After storing this in an aerosol container, LPG gas was blown into (filled with) the solution in the aerosol container to prepare a room air freshener. Example 5 Aerosol type room air freshener (
i) Preparation of low boiling point components of fragrance 1.0 kg of the fragrance assembled as shown below was placed in a round flask, and a vacuum distillation apparatus was attached. 0.2mmH
g ~0. The pressure was reduced in the range of 5 mm H g and the temperature was raised from 30"C to 110°C in an oil bath, during which time the fraction was collected at a distillation rate of about 2-3 mffi per minute. The final fraction was 700 g. Low boiling point components were collected.
（＆ｌｌ威） （ｗｔ％
）ベルガモットオイル ２５レモンオ
イル ２０ラベンダーオイル
２５ネロリオイル
ｌ０ナツメグオイル
６ボアドローズオイル ６サ
ンダルウッドオイル ３ベチバーオイ
ル ３イランイランオイル
２（１１）室内散布用香料組或物の調
製
上記で得られた香料の低沸点或分を用い下記の＆Ｉｌ威
にてエアゾール形式の室内芳香剤を調製した。(&llwei) (wt%
) Bergamot oil 25 Lemon oil 20 Lavender oil 25 Neroli oil
l0 nutmeg oil
6 bore rose oil 6 sandalwood oil 3 vetiver oil 3 ylang ylang oil
2 (11) Preparation of a fragrance composition for indoor spraying Using the low-boiling point part of the fragrance obtained above, an aerosol-type indoor fragrance was prepared according to the following procedure.
（組戒） （ｗｔ％）前記
香料の低沸点成分 １． ０９５％未変
性エタノール ９３．０蒸留水
５．０窒素ガス
１．０（製法）
エタノールを攪拌し、これに香料の低沸点或分を添加し
て均一に溶解した後、所要量の水を加えた．これをエア
ゾール容器に収容した後、ＬＰＣ，ガスをエアゾール容
器内の上記溶液の中に吹き込み室内芳香剤を調製した．
〔発明の効果〕
０． ２ ｍ ｍ Ｈ ｇ 〜０． ５ ｍ ｍ Ｈ
ｇの減圧下に於いて、３ ０ ’Ｃ〜１１０゜Ｃの昇温
により留出して得られる香料の低沸点或分と揮発性溶媒
を含有してなる室内散布用香料＆１戒物は、噴霧使用を
繰り返しても残香性がなく、常にフレンシュな本来の芳
香を得ることができ、また、異なる香りに切り換えても
前の香りと混じることなく新たな香りを得られる優れた
室内散布用香料組威物であることは明らかである。(Kumikai) (wt%) Low boiling point component of the above fragrance 1. 095% undenatured ethanol 93.0 Distilled water
5.0 nitrogen gas
1.0 (Manufacturing method) Ethanol was stirred, a certain amount of a low boiling point fragrance was added thereto and dissolved uniformly, and then the required amount of water was added. After placing this in an aerosol container, LPC and gas were blown into the solution in the aerosol container to prepare a room air freshener. [Effect of the invention] 0. 2 mm Hg ~0. 5 mm H
A fragrance for indoor dispersion and a precept containing a volatile solvent and a low-boiling point fraction of the fragrance obtained by distillation by raising the temperature from 30'C to 110°C under a reduced pressure of An excellent fragrance set for indoor spraying that does not leave a scent behind even after repeated use, allowing you to always obtain a fresh original fragrance, and even when switching to a different scent, you can obtain a new scent without mixing with the previous scent. It is clear that it is a prestigious item.