DE1492753A1 - Process for the recovery and concentration of oxidation-sensitive aromatic substances - Google Patents

Description

INtUiI UlMi £ PATENT ADVOCATE DR. HANS-GUNTHER EGGERT ₁ DIPLOMA CHEMIST

5 KDLN-LINDINTHAL PETEK-KINTQEN-STKASSB 3

Cologne, May 21, 1968

H92753 ^{S1 / ho}

Salada Foods Ltd., Toronto, Ontario, Canada

Process for extracting and concentrating oxidations sensitive flavorings

The invention relates to the production and concentration of natural aromas from easily oxidizable extracts. she is particularly used in the production and concentration of natural aromas from volatile extracts, like tea or coffee extracts, the aroma of which is quick is subject to oxidative degradation and cannot be successfully isolated as a natural aroma using conventional methods.

It is known to be used in the manufacture of tea and coffee concentrates to distill and fractionate the flavorings from the extracts. However, it has become well-known Process proved to be very problematic to maintain the aroma of the freshly poured beverage and unchanged one has therefore tried constantly while maintaining the process principle of the distillation by changing the individual process steps to arrive at concentrates with an improved natural aroma.

Thus, according to German patent specification 267 196, the fired and ground coffee added sugar and that with

Mixture mixed with water at a temperature not

distilled over 100 ^{° C.} Bad-tasting essential oils and bitter substances as well as tar products should be retained by the sugar and its charred products.

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In the process of the Swiss patent for the production of tea extracts in powder form, tea leaves are used extracted with hot water and the volatile aromatic substances separated from the extract by simple evaporation and condensed. The extract freed from the aromatic substances is concentrated on its own and then again flavored and spray-dried. This process does not use or contain fractional distillation Measures to avoid a change in the flavoring substances during the process.

According to the process of US Pat. No. 2,927,860, an aqueous tea extract is first prepared and then a flash distillation is carried out in vacuo, 5 to 50% of the extract being drawn off in vapor form. The vapor containing the diluted flavor is separated and condensed and then introduced into the middle part of a fractionating column where e ^ is concentrated at a pressure of at least one atmosphere. The concentrated aromas are then fed back into the tea extract. To carry out this known method, a complicated device for separating and concentrating the aroma is required, which consists of a flash evaporator, a heat exchanger for condensing the vapor-aroma mixture, a preheater for the diluted aroma and an aroma fractionation column. In contrast to the process of the invention, however, in this known process the fractionation is not carried out under an inert gas.

From the German patents 899 01 and 1 31095 is the use of inert gas in the production of soluble coffee extracts is known. The inert gas will be yes, however used in other process steps than according to the invention. For example, the German patent specification 89 901 describes the production of solid soluble coffee extracts, the Extract is evaporated in the absence of air. A fractional distillation of the aroma substances with exclusion of air is possible However, this known patent cannot be found. at

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the method of the German patent IJl 095 is a stream of inert gas is used as a carrier for the extraction of aromas from tea and coffee. These Flavorings are not removed by distillation, but rather by passing the stream of inert gas through the dry coffee powder or tea at a low temperature and later adsorption of the aromas on sugar won. The teaching that a fractional distillation of the Aroma substances "should be carried out under an inert gas atmosphere; on the contrary, it means that the aroma is also decomposed by the action of water vapor under an inert gas atmosphere.

The prior art therefore includes the use of Inert gas only to protect the coffee extract, but not known to protect the aroma during a fractional distillation.

The invention differs therefrom essentially in that the aroma substances are fractionated under an inert gas atmosphere. This process produces tea concentrates that have the aroma of freshly poured tea own. The method of the invention enables economical production and concentration without that expensive or complicated equipment would be required.

The invention accordingly provides a method for recovering and concentrating oxidation-sensitive Flavors from a liquid extract by volatilization and fractionation, which is characterized by that the aroma components of the extract are volatilized by fractional distillation in an inert gas atmosphere and concentrated.

According to the invention, the natural aroma is obtained by a special method of fractional distillation under an inert gas atmosphere to protect against oxidative degradation

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won. According to the invention, such a fractionated Distillation can be carried out under atmospheric pressure. According to the invention, the natural aroma can be concentrated and then, if necessary, store under an inert gas atmosphere that protects against oxidative degradation.

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The invention is described below on the basis of an apeiielleo an » application Ib connection old of the illustration «who do the work- »• ie ·« obeoetlaoA veranaohaulicht, described, ί

In the drawing, 1 represents an alembic which is "the for" in "be stiemte itsnge 2 a tea extract or another oxidative extract," le coffee, be * me sowing contains another inert gas * such as carbon dioxide or a mixture of nitrogen and carbon dioxide * is already a porSaen. Plug k connected » and through the oil line 5 generally flasks, deflected or raised herds denote» whereby 5 a pressure regulator 6, «Inen flow control 7 and suitable Abaperrventile, 8« nthftlt «EIa Mesager & t 9 let sur beetiamung the fuel content · in the flask 1 closedea"

The piston I can be "grounded" by means of a wood device 10, x.B "an electrical apparatus, an Oaabrenner o.g."

On the flask I let * a column 11 gaeetst »the preferably old, braided, rustproof Stehlapirelen (indicated at 12) is filled» Ea is however sä beaertoen * des «any other suitable • FQllkSrper» dl «old the resulting DSapfea does not react *> · Β · Berls & ttel and Besehlgrlnge «are used tcuonon · ·.

The column 11 leads to a "KChltr 1?", The obsr the BUck-1λufkanal 14 leads back into the column.

An outflow line 5 for the product branches off from the return channel 14 and is controlled by the valve 16. The line 15 leads through a water outlet 1? The ends of the cooler IJ and the gate layer 18 connect "the connection was established, the" Soar 20 is old "Inen T-approach 2J and a ·· valve 24 s & sgestattst, upper dl · inert gas au · de» Systea ebxlebea can «The Template 18

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can be connected via «in control valve 21 with a» supply vessel 22 « the «earth.

the execution fell dea process for the preparation and concentration of flavor, the batch is 2 "contains the tea or other Ausgangamaterial, preferably first freed of oxygen, however, is inert to displace dissolved oxygen gas duroh the liquid passes" These VorspOlung can before introduction aea Extract can be made in the flask 1 or expediently by lowering the porous stopper 4 into the liquid na oh dea introducing the extract 2 into the flask 1 and passing the inert gas from the bottle 3 through the liquid

The pre-cleaning of the liquid 2 is not an essential feature of the invention, but represents a means of rapidly reducing the oxygen content of the system Bottle 3 passed into the flask for so long «bi; the oxygen content in the flask according to the indication that the measuring device 9 is less than 0.2 % , with the help of the Halzgerfite 10, the flask is heated to a boiling point of the liquid. The flow rate of the inert gas is then reduced to a value that is sufficient to keep the atmosphere in the flask 1 essentially free of oxygen.

As the temperature of the liquid extract 2 rises to the boiling point, the aroma components of the extract become evaporated. These volatilized aronia components become borne by the vapors generated during boiling and rise in the column 11 to the top.

The bowl and aroma retention area of the extract condense 1 «cooler 13 and flow through the return flow duct 14 into the Column 11 back, where they meet with other ascending, aroma-laden fluid bodies »The packing

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12 provide effective contact of liquid and Sip up and ensure an axleaic condensation de «Aroaas in the flowing liquid ·

When thermal equilibrium is reached, d * h * nom the bottle temperature is constant »the valve 16 becomes open and set to a high flow rate « The condensation tray DSapfo »in which the aroma is concentrated "Ground through there" valve 16 in the heat exchanger drained "where it is cooled down in the template 18 prior to cooling. As soon as a desired amount of the concentrated aroma has" sat in the template 18 " the aroma is transferred to a storage column 22 which has been pre-purged by inert gas.

Of course, the concentration of the aroma can be changed by changing the oil flow ratio "d * h" of the amount of product added to the column in the "Relation to the amount of product collected and by changing the weight of the pack" whereby the concentration "it increases" the reflux ratio and increasing deposit height increases. The type of packing also has an influence on the aroma concentration "since the concentration of the aroma increases with the old assumption that the contact between the liquid and the pot" increases "

example 1

500 tablespoons of extract are prepared by adding a Sohwarstee · »Bisehung (Orange Pekoe) Bit Uasser at 92 ⁰ C and put into the still 1» Nitrogen (2.2 liters min.) Was passed through the apparatus until the oxygen content Above the liquid was 0.0 % , the flow rate of nitrogen was reduced to 0.5 liters / rin. The liquid was heated to boiling. The fractionating column 11 was operated using a Röokfluaeverhiltnia of 14 ι 1. Braided packing was used stainless steel coils · The column was diameter

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■■ '· ■■ ^Λ ; · ■■; ° t ■

■■■■■■■■ - ι ■■■. ■. · '' <'Γ - ..!.!

from 25 m and mr 122 co high · Di «Bestlllatteoegftsehwlfidlg · cold of the column lay ** i 64.7 e / h.oe ² · 1 $ en? Aroea were for half an hour · in the template »18 work · Sa« Aroma i was used for Inetant-TeepuXver * At an · Itst (blind i, a © up teat) s & rtHobe Veraoehaperaonen declared »daes

the powder and a drink made from it aroMatiaierten Verßleichaprobe Oberlecen is ·

Example g . *

Using 1500 al extract and with a «ROekflusa · In relation to 20 ι 1 the In Belaplel 1 beaetir level Verauob repeated. The DogtlXlatlonggegehwlndlgkelt cheated 66 * 5 g / a «en · 35 ad aroita concentrate were obtained in 1 * 5 hours caught »ßleaea Arooa was baked in tae powder« daa judged significantly beaaer with an anal reading ttoat was al «daa nleht> araoated comparing powder.

fis iat noted below, DAEs not only the Baratellung and centering, but also the capture and storage of Aroaas, carried out in an inert AtsoaphBre the absence of oxygen, so that the final product no oxidative degradation erflhrt and aueh after attv storage a fresh nator "llcbea flavor maintains.

Although the process was observed as a batch process, However, it can also be carried out continuously

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Claims (4)

U92753 PATENT CLAIMS 1. Method for extracting and concentrating oxidation-sensitive Flavorings from a liquid extract by volatilization and fractionation, thereby characterized in that the aroma components of the extract by fractional distillation in volatilized and concentrated in an inert gas atmosphere. 2. The method according to claim 1, characterized in that the fractional distillation is essentially at Atmospheric pressure is carried out. j5. Method according to claim 1 or 2, characterized in that a tea extract is used as the liquid extract. 4. The method according to claims 1 to 3 *, characterized in that that the extract prior to fractional distillation to remove oxygen with inert gas is stripped. New documents (Art. 7 | 1 Abe. 2 No. I Sett a des Anderuhoeges. V. 4.9. 9 098 0 3/0770