JP3772080B2 - Method for preparing gas phase aroma components - Google Patents

Method for preparing gas phase aroma components Download PDF

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JP3772080B2
JP3772080B2 JP2000308611A JP2000308611A JP3772080B2 JP 3772080 B2 JP3772080 B2 JP 3772080B2 JP 2000308611 A JP2000308611 A JP 2000308611A JP 2000308611 A JP2000308611 A JP 2000308611A JP 3772080 B2 JP3772080 B2 JP 3772080B2
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gas phase
gas
inert gas
mass flow
mixing
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JP2002113339A (en
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純一 井手
幸彦 中村
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T Hasegawa Co Ltd
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T Hasegawa Co Ltd
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Description

【０００１】
【発明の属する技術分野】
本発明は気相香気成分の混合による香料の調合装置及び調合方法に関する。さらに詳しくは、複数個の試料瓶内に注入された液体香料の気相部に平衡状態で存在する気相香気成分の混合による香料の調合装置及び調合方法に関する。
【０００２】
【従来の技術】
従来、香料の調合は多くの液体試料の混合によってなされてきた。液体試料の蒸気圧、即ち揮発性は各香気成分により異なり、このため新しい香料の調合、即ち液体としての処方値の決定には多くの時間を必要とするものであった。
【０００３】
米国特許明細書第４、５２０、６５１号は、無臭ガスと共に数種の揮発性物質の蒸気を個別に混合し、混合室で該混合ガスを混合することにより、芳香を得る装置を開示している。この装置は、窒素タンクと、その分配室と、分配室からの窒素ガスの流量調整バルブと、揮発性物質入り容器と、該容器と連結した混合室とを備えている。この装置では、揮発性の少ない物質の場合には長時間にわたり無臭ガスを通気しなければ嗅覚部に到達せず、また長時間の通気は容器内の気液平衡バランスを乱し、揮発性物質と気液平衡状態にある香気成分の混合ガスについての芳香を感知することができない。また、この装置では無臭ガスの流量が必ずしも正確でなく、感得した芳香の香料としての処方を明確にするためには、なお多くの手間を必要とする。また、混合室内等には、測定した揮発性成分のメモリー効果が生じるため、次回の測定までには時間を要することとなる。
【０００４】
【発明が解決しようとする課題】
本発明は、各種気相香気成分を気相状態で任意に、かつ定量的に混合できる、調合作業の簡易迅速化を図りうる香料用気相香気成分の調合装置及び調合方法の提供を目的とする。
【０００６】
【課題を解決するための手段】
本発明は、不活性ガス供給槽からマスフローコントローラ及び電磁バルブを経て所定量の不活性ガスを試料瓶中の気相部に突出している不活性ガス注入管を経て複数個の試料瓶の気相部に供給する工程と、試料瓶の気相部からマスフローコントローラにより制御定量された不活性ガスと気相香気成分との混合ガスを試料瓶中の気相部に突出している送出管及び電磁バルブを経て混合室に供給する複数個の供給工程と、マスフローコントローラにより制御定量された不活性ガスを該混合ガスと同時に混合室に供給する供給工程と、不活性ガスと気相香気成分を撹拌混合用部材を備えた混合室で撹拌混合する混合工程と、混合後の混合ガスの芳香に応じて不活性ガスの流量をマスフローコントローラにより制御定量する工程とからなることを特徴とする気相香気成分の調合方法を提供する。
【０００７】
【発明の実施の形態】
以下本発明を図１に基づいて説明する。不活性ガス供給槽１から流路２、分岐流路３を経て不活性ガスはマスフローコントローラ４、５、６、７に供給される。不活性ガスは、香気成分と反応しないものであればよく、例えば、空気、窒素ガス等が挙げられる。マスフローコントローラは、質量流量を測定するものであり、体積流量計とは異なり、圧力、温度、ガス密度等に関係なく流量を計測することができるので、必ずしも開放系とはいえない本発明の装置、方法での使用に適している。マスフローコントローラ７で流量を計測された所定流量の不活性ガスは、電磁バルブV7を経て混合室１１に供給される。マスフローコントローラ４、５、６により流量を計測された所定量の不活性ガスはそれぞれ流路８、９、１０、電磁バルブV1、V3、V5を経て試料瓶１２、１３、１４に不活性ガス注入管１５、１６、１７を経て供給される。図を含め本説明において、説明の便宜上マスフローコントローラ及び試料瓶をそれぞれ３個としているが、試料瓶等の数は必要に応じさらに多数設けることができる。
【０００８】
不活性ガス注入管は、試料瓶中に注入された液体の上部、即ち気相部に開口している。注入された不活性ガスは気相部で気液平衡状態にある気相香気成分を、試料瓶に設けられた送出管１８、１９、２０及び電磁バルブV2、V4、V6、流路２１、２２、２３を経て混合室１１に移送する。不活性ガスの通気量は、試料瓶内の気液平衡状態を損なわない範囲内とすることにより、再現性の良い各気相香気成分の混合ガスを取得することができる。電磁バルブは、不活性ガス及び気相香気成分の流れ遮断及び逆流防止用に設置されている。
【０００９】
混合室１１は、内部にガスの撹拌混合用の部材（図示せず）を備えたものが使用される。ガスの撹拌混合用の部材としては、例えばスタティックミキサー、分溜管等が挙げられる。分溜管としてはビグローカラム、回転バンド型分溜管、充填塔等が挙げられる。混合室１１には、マスフローコントローラ７、流路２４を経て不活性ガスが供給される。この供給された不活性ガスは、混合室１１から排出される混合ガスの量を大きくし、気相香気成分の鼻即ち嗅覚部、あるいは分析装置に達し易くする。さらにこの不活性ガスは、混合室内でのガス流量を大きくすることにより、乱流化を促進し、各気相香気成分の混合を進める働きがある。
【００１０】
電子制御装置２５によりマスフローコントローラ４、５、６、７の流量を制御し、各気相香気成分の量を適宜の範囲に制御し、嗅覚等によりその是非を判断された混合ガスの各マスフローコントローラ流量値、即ち各気相香気成分の流量値を、これに接続された電子制御装置２５により、液相における割合に換算することができる。これにより、気相香気成分の混合により創出した興味ある香料を、その香料の処方値（各気相香気成分の液相における割合）に迅速に変換することができる。図中、記号２６はリレーボードを、２７は通信ケーブルを示す。
【００１１】
試料瓶の上流側及び下流側にある電磁バルブは、逆流防止用としても機能するものであり、さらには混合室内に流路２４を経た不活性ガスを通すことにより、いわゆるメモリー効果を払拭し、次回の測定を迅速に実施することができる。
【００１２】
実施例１：
実験試料として、ジャスミン調合香料を用い、マスフローコントローラによる不活性ガス流量と処方値（重量部表示）との関係を調べた。
【００１３】
【表１】

Figure 0003772080
【００１４】
図１に示す装置を用い、Benzyl acetate、2-Hexylcinnamic aldehyde及びYlang Ylang をそれぞれ試料瓶にいれ、マスフローコントローラにより空気の流量を処方値と同じに設定した。即ちBenzyl acetate：2-Hexylcinnamic aldehyde：Ylang Ylang 1st comoro＝１８０：９０：３０ml/min.と設定し、そして流路２４の空気流量を１２０ml/min.と設定した。撹拌混合部材としてビグローカラムを使用した混合室から得られた混合ガスを液体窒素に浸せきしたU字管で５分間トラップした後、ガスクロマトグラフィで分析した。
【００１５】
【表２】
Figure 0003772080
【００１６】
注：(A):Benzyl acetate：2-Hexylcinnamic aldehyde：Ylang Ylang ＝１８０：９０：３０ml/min.に空気流量をマスフローコントローラで設定し、ガスクロマトグラフィで各成分を分析したときのピーク面積百分率。
：(B)：表１に示したジャスミン調合香料を試料瓶に入れ、気相部の香気成分をガスクロマトグラフィで分析したときのピーク面積百分率。
：(C）：（A）の気相香気成分量を蒸気圧を基に液相香気成分量に変換したデータ（重量％）。
:（D）： (B)の気相香気成分量を蒸気圧を基に液相香気成分量に変換したデータ（重量％）。
【００１７】
【表３】
Figure 0003772080
注：Ylang Ylang中にはBenzyl acetateが含まれているので、p-cresyl methyl ether量からYlang Ylang量を求めた。表中数値は重量部で示した。
マスフローコントローラで流量を設定することにより、望む芳香を有する香料としての組成を容易に決定することができる。
【００１８】
【発明の効果】
本発明によれば、マスフローコントローラにより不活性ガスの流量を適宜調整することにより気相香気成分を容易に調整できると共に、望む芳香を有する香料としての処方を容易に決定できる調合装置及び調合方法が提供される。本発明によれば、さらに、流量の設定された不活性ガスを混合室に供給することにより、さらに撹拌混合に適した部材を備えた混合室を使用することにより、気相香気成分の混合を容易ならしめることができる。
【図面の簡単な説明】
【図１】本発明の気相香気成分の調合装置を示す説明図である。
【符号の説明】
１ 不活性ガス供給槽
４ マスフローコントローラ
５ マスフローコントローラ
６ マスフローコントローラ
７ マスフローコントローラ
１１ 混合室
１２ 試料瓶
１３ 試料瓶
１４ 試料瓶
２５ 電子制御装置[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a fragrance blending apparatus and blending method by mixing gas phase aroma components. More specifically, the present invention relates to a fragrance blending apparatus and a blending method by mixing gas phase fragrance components present in an equilibrium state in a gas phase portion of liquid fragrance injected into a plurality of sample bottles.
[0002]
[Prior art]
Traditionally, fragrances have been formulated by mixing many liquid samples. The vapor pressure, i.e. volatility, of the liquid sample is different for each aroma component, and therefore it takes a lot of time to formulate a new fragrance, i.e. to determine the prescription value as a liquid.
[0003]
U.S. Pat. No. 4,520,651 discloses an apparatus for obtaining a fragrance by individually mixing vapors of several volatile substances together with an odorless gas and mixing the mixed gas in a mixing chamber. Yes. This apparatus includes a nitrogen tank, its distribution chamber, a flow rate adjusting valve for nitrogen gas from the distribution chamber, a container containing volatile substances, and a mixing chamber connected to the container. In this device, in the case of a substance with low volatility, it does not reach the olfactory part unless odorless gas is vented for a long time, and long-term ventilation disturbs the vapor-liquid equilibrium balance in the container, and the volatile substance It is impossible to sense the fragrance of the mixed gas of fragrance components in a gas-liquid equilibrium state. Further, in this apparatus, the flow rate of the odorless gas is not always accurate, and much labor is required to clarify the prescription as a perfumed fragrance. In addition, since the memory effect of the measured volatile component occurs in the mixing chamber or the like, it takes time until the next measurement.
[0004]
[Problems to be solved by the invention]
It is an object of the present invention to provide a preparation device and a preparation method for a gas phase aroma component for a fragrance capable of mixing various gas phase aroma components arbitrarily and quantitatively in a gas phase state, and capable of simplifying and speeding up a mixing operation. To do.
[0006]
[Means for Solving the Problems]
The present invention provides a gas phase of a plurality of sample bottles through an inert gas injection pipe projecting a predetermined amount of an inert gas from an inert gas supply tank through a mass flow controller and an electromagnetic valve to a gas phase part in the sample bottle. A feeding pipe and an electromagnetic valve projecting into the gas phase part in the sample bottle, the step of supplying to the part, and the mixed gas of the inert gas and the gas phase aroma component controlled and quantified by the mass flow controller from the gas phase part of the sample bottle A plurality of supply steps to be supplied to the mixing chamber through the process, a supply step to supply the inert gas controlled and quantified by the mass flow controller to the mixing chamber simultaneously with the mixed gas, and stirring and mixing the inert gas and the gas phase aroma components wherein a mixing step of stirring and mixing in a mixing chamber having a use member, in that it consists of a step of controlling quantified by the mass flow controller flow rate of the inert gas in accordance with the fragrance of the mixed gas after mixing It provides a method for the preparation a gas phase aroma components.
[0007]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be described with reference to FIG. The inert gas is supplied from the inert gas supply tank 1 to the mass flow controllers 4, 5, 6, 7 through the flow path 2 and the branch flow path 3. The inert gas should just be a thing which does not react with an aromatic component, for example, air, nitrogen gas, etc. are mentioned. The mass flow controller measures the mass flow rate, and unlike the volume flow meter, the mass flow controller can measure the flow rate regardless of the pressure, temperature, gas density, etc., so the device of the present invention is not necessarily an open system. Suitable for use in the method. A predetermined flow rate of the inert gas whose flow rate is measured by the mass flow controller 7 is supplied to the mixing chamber 11 via the electromagnetic valve V7. A predetermined amount of inert gas whose flow rate is measured by the mass flow controllers 4, 5, 6 passes through the flow paths 8, 9, 10 and electromagnetic valves V 1 , V 3 , V 5 to the sample bottles 12, 13, 14. It is supplied through active gas injection pipes 15, 16, 17. In the present description including the drawings, for convenience of explanation, three mass flow controllers and three sample bottles are provided, but a larger number of sample bottles and the like can be provided if necessary.
[0008]
The inert gas injection pipe opens to the upper part of the liquid injected into the sample bottle, that is, the gas phase part. The injected inert gas is a gas phase aroma component in a gas-liquid equilibrium state in the gas phase portion, and the delivery pipes 18, 19, and 20 provided in the sample bottle and the electromagnetic valves V 2 , V 4 , V 6 , flow path Transfer to the mixing chamber 11 through 21, 22, and 23. By setting the aeration amount of the inert gas within a range that does not impair the vapor-liquid equilibrium state in the sample bottle, it is possible to obtain a mixed gas of each gas phase aroma component with good reproducibility. The electromagnetic valve is installed for blocking the flow of inert gas and gas phase aroma components and preventing backflow.
[0009]
The mixing chamber 11 is provided with a gas stirring / mixing member (not shown). Examples of the gas stirring and mixing member include a static mixer and a fractionating pipe. Examples of the fractionating pipe include a Vigreux column, a rotating band type fractionating pipe, and a packed tower. An inert gas is supplied to the mixing chamber 11 via the mass flow controller 7 and the flow path 24. The supplied inert gas increases the amount of the mixed gas discharged from the mixing chamber 11 and easily reaches the nose of the gas phase aromatic component, that is, the olfactory part or the analyzer. Further, this inert gas has a function of promoting turbulence by increasing the gas flow rate in the mixing chamber and promoting the mixing of the respective gas phase aromatic components.
[0010]
The mass flow controllers 4, 5, 6, and 7 are controlled by the electronic control device 25, the amounts of the respective gas phase aroma components are controlled within an appropriate range, and the mass flow controllers of the mixed gas determined by the sense of smell etc. The flow rate value, that is, the flow rate value of each gas phase aroma component can be converted into the ratio in the liquid phase by the electronic control unit 25 connected thereto. Thereby, the interesting fragrance created by mixing the gas phase fragrance components can be quickly converted into the prescription value of the fragrance (the ratio of each gas phase fragrance component in the liquid phase). In the figure, symbol 26 indicates a relay board, and 27 indicates a communication cable.
[0011]
The electromagnetic valves on the upstream side and downstream side of the sample bottle function also for backflow prevention, and further wipe out the so-called memory effect by passing an inert gas through the flow path 24 into the mixing chamber. The next measurement can be carried out quickly.
[0012]
Example 1:
As a test sample, jasmine blended fragrance was used, and the relationship between the inert gas flow rate by the mass flow controller and the prescribed value (in parts by weight) was examined.
[0013]
[Table 1]
Figure 0003772080
[0014]
Using the apparatus shown in FIG. 1, Benzyl acetate, 2-Hexylcinnamic aldehyde, and Ylang Ylang were each placed in a sample bottle, and the air flow rate was set to the same as the prescription value by a mass flow controller. That is, Benzyl acetate: 2-Hexylcinnamic aldehyde: Ylang Ylang 1st comoro = 180: 90: 30 ml / min. And the air flow rate in the flow path 24 was set to 120 ml / min. The mixed gas obtained from the mixing chamber using the Vigreux column as the stirring and mixing member was trapped for 5 minutes with a U-shaped tube immersed in liquid nitrogen, and then analyzed by gas chromatography.
[0015]
[Table 2]
Figure 0003772080
[0016]
Note: (A): Benzyl acetate: 2-Hexylcinnamic aldehyde: Ylang Ylang = The peak area percentage when each component was analyzed by gas chromatography with an air flow rate set at 180: 90: 30 ml / min.
: (B): Percentage of peak area when the jasmine blended fragrance shown in Table 1 was placed in a sample bottle and the aroma components in the gas phase were analyzed by gas chromatography.
: (C): Data (% by weight) obtained by converting the gas phase aroma component amount of (A) into the liquid phase aroma component amount based on the vapor pressure.
: (D): Data (weight%) obtained by converting the gas phase aroma component amount of (B) into the liquid phase aroma component amount based on the vapor pressure.
[0017]
[Table 3]
Figure 0003772080
Note: Since Ylang Ylang contains Benzyl acetate, the amount of Ylang Ylang was determined from the amount of p-cresyl methyl ether. The numerical values in the table are expressed in parts by weight.
By setting the flow rate with a mass flow controller, the composition as a fragrance having a desired fragrance can be easily determined.
[0018]
【The invention's effect】
ADVANTAGE OF THE INVENTION According to this invention, while adjusting the flow volume of an inert gas suitably by a massflow controller, while being able to adjust a gaseous-phase aroma component easily, the preparation apparatus and the preparation method which can determine easily prescription as a fragrance | flavor which has a desired fragrance are provided. Provided. According to the present invention, by further supplying an inert gas having a set flow rate to the mixing chamber, and further using a mixing chamber equipped with a member suitable for stirring and mixing, mixing of gas phase aroma components can be performed. It can be easily adjusted.
[Brief description of the drawings]
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is an explanatory view showing a gas phase aroma component preparation device of the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Inert gas supply tank 4 Mass flow controller 5 Mass flow controller 6 Mass flow controller 7 Mass flow controller 11 Mixing chamber 12 Sample bottle 13 Sample bottle 14 Sample bottle 25 Electronic controller

Claims (5)

不活性ガス供給槽からマスフローコントローラ及び電磁バルブを経て所定量の不活性ガスを試料瓶中の気相部に突出している不活性ガス注入管を経て複数個の試料瓶の気相部に供給する工程と、試料瓶の気相部からマスフローコントローラにより制御定量された不活性ガスと気相香気成分との混合ガスを試料瓶中の気相部に突出している送出管及び電磁バルブを経て混合室に供給する複数個の供給工程と、マスフローコントローラにより制御定量された不活性ガスを該混合ガスと同時に混合室に供給する供給工程と、不活性ガスと各気相香気成分を撹拌混合用部材を備えた混合室で撹拌混合する混合工程と、混合後の混合ガスの芳香に応じて不活性ガスの流量をマスフローコントローラにより制御定量する工程とからなることを特徴とする気相香気成分の調合方法。 A predetermined amount of inert gas is supplied from an inert gas supply tank to a gas phase portion of a plurality of sample bottles via an inert gas injection pipe protruding into the gas phase portion of the sample bottle via a mass flow controller and an electromagnetic valve. process and, delivery tube and the mixing chamber through the solenoid valve a mixed gas of an inert gas and gaseous aroma components controlled quantified by the mass flow controller from the gas phase of the sample bottle protrudes into the gas phase portion in the sample bottle A plurality of supply steps for supplying to the mixture, a supply step for supplying the inert gas controlled and quantified by the mass flow controller to the mixing chamber simultaneously with the mixed gas, and a member for stirring and mixing the inert gas and each gas phase aroma component. feel characterized a mixing step of stirring and mixing in a mixing chamber having, in that it consists of a step of controlling quantified by the mass flow controller flow rate of the inert gas in accordance with the fragrance of the mixed gas after mixing Formulation method of aroma components. 不活性ガスの流量制御が、電子制御装置により制御されたマスフローコントローラにより実施されることを特徴とする請求項１記載の気相香気成分の調合方法。  The method for preparing a gas phase aroma component according to claim 1, wherein the flow rate control of the inert gas is performed by a mass flow controller controlled by an electronic control unit. マスフローコントローラにより制御定量された不活性ガスにより混合室に供給された気相香気成分の量を電子制御装置により液相香気成分量に換算することを特徴とする請求項１記載の気相香気成分の調合方法。  2. The gas phase aroma component according to claim 1, wherein the amount of the gas phase aroma component supplied to the mixing chamber by the inert gas controlled and quantified by the mass flow controller is converted into a liquid phase aroma component amount by the electronic control unit. The preparation method. 混合室が、スタティックミキサー又はビグローカラムを備えていることを特徴とする請求項１記載の気相香気成分の調合方法。  The method for preparing a gas phase aroma component according to claim 1, wherein the mixing chamber comprises a static mixer or a big glow column. 不活性ガス注入管の気相部中の突出長さが、送出管の気相部中の突出長さよりも大きいことを特徴とする請求項１記載の気相香気成分の調合方法。The method for preparing a gas phase aroma component according to claim 1, wherein the protruding length in the gas phase portion of the inert gas injection pipe is larger than the protruding length in the gas phase portion of the delivery pipe.
JP2000308611A 2000-10-10 2000-10-10 Method for preparing gas phase aroma components Expired - Lifetime JP3772080B2 (en)

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Publication number Priority date Publication date Assignee Title
CN106237877A (en) * 2016-09-28 2016-12-21 北京明尼特环保设备有限公司 A kind of dynamically gas-liquid mixed distributing instrument

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JP4621375B2 (en) * 2001-04-03 2011-01-26 長谷川香料株式会社 Deodorant search method
JP2009189411A (en) * 2008-02-12 2009-08-27 Mizunami Seiki Kk Aroma container and aroma generator having the same
JP6086677B2 (en) * 2012-09-03 2017-03-01 静岡県 Method and apparatus for measuring volatile components
CN103341330A (en) * 2013-06-27 2013-10-09 江苏物联网研究发展中心 Standard gas distribution device for gas testing system

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US4520651A (en) * 1982-04-19 1985-06-04 Ira Litman Method and apparatus for obtaining the combined aroma of several substances
JPH08153685A (en) * 1994-11-25 1996-06-11 Mitsubishi Corp Special material gas supply device for semiconductor
BR9801758A (en) * 1997-06-05 2000-02-22 Givaudan Roure Int Olfactometer

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106237877A (en) * 2016-09-28 2016-12-21 北京明尼特环保设备有限公司 A kind of dynamically gas-liquid mixed distributing instrument
CN106237877B (en) * 2016-09-28 2019-05-17 北京明尼特环保设备有限公司 A kind of dynamic gas-liquid mixed distributing instrument

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