GB1596587A - Processor for preparing decaffeinated coffee - Google Patents

Abstract

To produce a decaffeinated instant coffee with an improved flavour and aroma, an aqueous extract of ground roast coffee is decaffeinated by treatment with an organic solvent for caffeine which is not miscible with water and removal of the decaffeinated aqueous coffee extract from the caffeine-containing organic solvent which is not miscible with water; flavour and aroma of the coffee extract are improved by readmixing certain flavourings, by displacing the caffeine from the organic solvent by means of a treatment with water, introducing the resulting organic solvent, which contains flavourings, into the coffee extract, and freeing the coffee extract from solvent. The extract which has been freed from solvent can now be dried to give instant coffee powder.

Description

(54) PROCESS FOR PREPARING DECAFFEINATED COFFEE (71) We. THE THE PROCTER & GAM BLE COMPANY, a company organised under the laws of State of Ohio, United States of America, of 301 East Sixth Street, Cincinnati, Ohio 45202. United States of America, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:- This invention relates to a process for preparing a decaffeinated extract. More particularly, it relates to a process for the preparation of a decaffeinated coffee extract of the soluble or instant type.

Numerous methods for the decaffeination of coffee have been described in the art. For example. U.S. Reissue Patent 13,261, issued September 1, 1908 to Meyer et al., describes a process involving direct contact between green coffee and a solvent for caffeine.

Moistened green coffee beans are contacted with an organic solvent, residual solvent is removed from the green beans, and the decaffeinated beans are roasted for preparation of a coffee extract and product therefrom. Another approach to decaffeination of coffee has involved the formation of an aqueous extract of green coffee solubles followed by a liquid/liquid decaffeination operation utilizing an organic solvent. This method is described in detail in U.S. Patent 2.309.092. issued January 26, 1943 to Berry et al.

Green bean decaffeination methods, while effective to remove caffeine from the coffee beans, involve the handling of large amounts of coffee and solvent materials and require the utilization of expensive equipment and facilities. Moreover, the decaffeination and desolventizing steps employed in green bean decaffeination methods are slow operations tending to reduce process efficiency.

Certain of the economic considerations and processing inefficiencies of green bean decaffeination methods have been overcome by resort to liquid/liquid decaffeination of roast and ground coffee extract. Extract decaffeination methods are relatively fast in operation and require less capital equipment and expense than green bean decaffeination methods. Examples of extract decaffeination methods are described in U.S. Patent 2,472,121 (issued June 7, 1949 to Ornfelt); U.S. Patent 2,472,881 (issued June 14, 1949 to Bender); and U.S. Patent 2,933,395 (issued April 19, 1060 to Adler et al.). In general, these methods involve the preparation of an extract of roast and ground coffee and decaffeination of the extract by utilization of a water-immiscible organic solvent for caffeine.The resulting decaffeinated extract, separated from the caffeine-laden organic solvent, can be utilized in the preparation of a soluble coffee in conventional manner.

While extract decaffeination methods permit certain economic and practical limitations of green bean decaffeination methods to be overcome, extract decaffeination methods are attended by the same problems of flavor quality as exist in the case of decaffeination methods in general. Thus, it has been generally appreciated that decaffeinated coffee products tend to lack the flavor and aroma qualities of their non-decaffeinated counterparts. The tendency of decaffeinated coffee products to be diminished with respect to flavor and aroma principles that contribute materially to cup aroma and flavor has been attributed for the most part to the tendency of caffeine solvents to remove certain desirable non-caffeine constituents of coffee.

SUMMARY OF THE INVENTION The present invention is based in part upon the discovery that important noncaffeine flavor and aroma constituents normally removed from an aqueous coffee extract in the course of liquid/liquid decaffe ination can be efficiently recovered and restored to the coffee extract with the result that an extract having improved flavor and aroma characteristics is obtained. Thus, the recovery and restoration to a coffee extract of these important coffee and aroma principles can be effectively utilized in extract decaffeination methods. These methods generally comprise the steps of forming an aqueous extract of roast and ground coffee, decaffeinating the extract by contact with a waterimmiscible organic solvent for caffeine, and separating the decaffeinated aqueous coffee extract from the caffeine-containing waterimmiscible organic solvent.It has been found that desirable flavor and aroma principles can be effectively recovered by partitioning the caffeine content of the water-immiscible organic solvent into water. The resulting organic solvent and its content of flavor and aroma principles is thereafter be restored to the coffee extract. The extract can then be desolventized and dried in a conventional manner to a soluble coffee product having improved flavor and aroma characteristics.

DETAILED DESCRIPTION OF THE IN VENTION By the process of the present invention, an aqueous extract of roast and ground coffee is subjected to a liquid/liquid extraction with an organic water-immiscible caffeine solvent.

A resulting caffeine-laden solvent is separated from the decaffeinated coffee extract and is subjected to a recovery process whereby certain desirable flavor and aroma principles in the organic solvent are retained after partitioning of a caffeine content of the organic solvent into water.

The aqueous coffee extract can be prepared in conventional manner from roast and ground coffee beans. Coffee beans are roasted and ground to a suitable state of subdivision for extraction by any of a number of known methods. Countercurrent extraction methods can conveniently be employed, and examples of such methods are described in, for example, U.S. Patent 3,700,463 (issued October 24, 1972 to Bolt et al.), and U.S. Patent 3,700,466 (issued October 24, 1972 to Bergeron et al.). The extract will normally have a concentration of soluble coffee solids in the range of from 15% to 35%, although extracts having a lesser or greater concentration of such coffee solids can be employed.

The coffee extract can be devolatilized prior to the liquid/liquid extraction operation. For example, the coffee extract can be devolatilized by flashing-off volatiles at subatmospheric pressure or by passing an inert gas such as carbon dioxide, nitrogen, or steam through the coffee extract. The coffee volatiles are condensed for later addition to the coffee extract, known as the add-back process. The employment of a devolatilization step, whereby the volatiles are condensed in a suitably chilled condenser for add-back to the coffee extract, constitutes a preferred practice from the standpoint of optimizing flavor of the ultimate coffee product and minimizing the possibly adverse affect of operating conditions upon the volatile components of the coffee extract. A preferred devolatilization step involves the stripping of volatiles from the coffee extract with the aid of steam.

If desired, the coffee extract can be concentrated prior to the liquid/liquid decaffeination operation. For example, the extract can be concentrated into the range of 309 to 45% coffee solids prior to the decaffeination step.

The roast and ground coffee extract can be decaffeinated by a number of methods. The decaffeination operation involves a liquid/liquid extraction whereby contact of the aqueous extract with a liquid water-immiscible organic solvent effects substantial removal of the caffeine content of the coffee extract.

Any of a variety of water-immiscible organic caffeine solvents can be employed. Examples include hydrocarbon solvents such as benzene and toluene, halogenated hydrocarbons, such as chloroform, methylene chloride, dichloroethylene, trichloroethylene, difluoromonochloromethane, and 1,1,1 -trichloro- ethane. Other suitable water-immiscible organic solvents for caffeine include ethyl acetate and benzyl alcohol. It will be appreciated that preferred solvents will include those which are effective to remove caffeine from the extract while removing as small an amount of non-caffeine coffee solids as practicable and leaving as little residue of solvent in the ultimate coffee product.

The liquid/liquid extraction is preferably performed while using as low a solvent to extract ratio as is practicable. The employment of low solvent to extract ratios permits removal of the caffeine content from the coffee extract while minimizing the amount of non-caffeine solids removed from the extract. Thus, by controlling the amount of organic solvent contacted with the coffee extract, the extraction of coffee solids having a solvent-to-water distribution coefficients smaller than caffeine is minimized. Employment of high ratios of solvent to extract results in the increased removal along with caffeine of coffee solids having solvent to water distribution coefficients smaller than caffeine. When the caffeine-laden solvent is thereafter contacted with water to partition the caffeine content from the organic solvent, such coffee solids tend to partition along with the caffeine with the result that such solids do not remain with the organic solvent for restoration to the coffee extract. A ratio of water-immiscible organic solvent to coffee extract in the range of from 0.3:1 to 10:1 can be employed. The particular ratio employed will depend upon the particular solvent selected for the extract decaffeination. For example, where the solvent is methylene chloride, a preferred ratio will be from 0.5:1 to 1:1.

The liquid/liquid decaffeination operation can be conducted in a batch or continuous operation, although a continuous countercurrent liquid/liquid extraction of caffeine will be preferred. Liquid/liquid extraction techniques are well known and generally involve continuous contacting of extract with the water-immiscible organic caffeine solvent. The contact can be suitably conducted in an elongated column. For example, where a solvent heavier than the aqueous extract is employed, the aqueous extract can be sprayed into the lower end of an elongated column containing the caffeine solvent. The coffee extract is allowed to travel upwardly in a manner countercurrent to the solvent and the decaffeinated extract is removed continuously from the top of the decaffeination column. Such a method is described in detail in U.S. Patent 2,933,395 (issued April 19, 1960 to Adler et al.).Other methods for effecting the liquid/liquid extraction can be employed. For example, the coffee extract can be contacted with the caffeine solvent by passing the extract and the organic solvent in countercurrent fashion into a packed columnar bed comprising an elongated tower fitted with Pall rings. Raschig rings or the like.

Preferred apparatus for conducting the liquid/liquid decaffeination comprises such liquid/liquid contacting devices as the Rotary-disk Contactor, the Oldshue-Rushton column, or the York-Scheibel column. It will be appreciated that the feasibility of the employment of low ratios of solvent to extract will depend in part upon the nature of the solvent employed, the concentration of the coffee extract, and the efficiency or mass transfer capability of the liquid/liquid contacting equipment. Thus, it will be preferred to employ a liquid/liquid contacting device which provides the mechanical agitation and turbulence necessary for maximization of mass transfer. For this reason, a preferred type of liquid/liquid contactor is the Rotarydisk Contactor. It has been found that such a device will permit efficient decaffeination at low solvent-to-extract ratios, e.g., less than 1:1.The Rotary-disk Contactor and other suitable liquid/liquid contacting devices are described in detail in Perry's Chemical Engineers' Handbook, McGraw-Hill Book Company. 4th Edition, Section 21, pp. 2335.

The decaffeinated extract is separated from the caffeine-laden solvent in known manner. Normally the separation will be the result of continuous removal of countercurrent coffee extract and solvent streams from the liquid/liquid contactor. The separated caffeine-laden solvent is thereafter treated for recovery of flavor and aroma principles.

The water-immiscible organic caffeineladen solvent is treated for separation of the caffeine therefrom. This is accomplished by contacting the caffeine-laden solvent with an amount of water sufficient to remove or partition the caffeine from the organic phase into the aqueous phase. Substantially complete removal or partition of caffeine from the organic solvent is realized. The amount of water employed will vary with the particular nature of the solvent. Generally, an amount of water providing a ratio of water to caffeine-laden solvent of from 0.5:1 to 10:1 will be sufficient to effect the partitioning of caffeine into an aqueous phase. A preferred ratio in the case of methylene chloride solvent is from 5:1 to 6:1.Preferably, the caffeine-laden solvent will be concentrated prior to caffeine removal so as to minimize the amount of caffeine-laden solvent which must be handled and contacted with water for the caffeine removal. In addition, concentration of the caffeine-laden solvent permits maximization of mass transfer and reduces capital equipment requirements. Concentration can be effected by flashing of the organic solvent, by the use of conventional thin-film evaporators or the like. For economy of operation, evaporated solvent will be condensed for re-use in further liquid/liquid decaffeination. The concentrated caffeineladen solvent will preferably be concentrated such that the solids content comprises from 1% to 10% by weight of the caffeine-laden solvent.

The partitioning of caffeine from the caffeine-laden solvent can be achieved by any effective contact of water with the caffeine-laden solvent. The caffeine-laden solvent can be introduced in a countercurrent manner into a column containing water.

As in the case of the liquid/liquid decaffeination operation, the separation of caffeine from the caffeine-laden solvent can be facilitated by the use of other conventional liquid/liquid contacting devices. A preferred device is a continuous countercurrent extractor such as a Rotary-disk Contactor. This device permits intimate contact between water and the caffeine-laden solvent and efficient recovery of aqueous and organic phases.

The amount of aroma and flavor principles restored to the coffee extract will depend upon the amount present in the organic solvent as the result of the extract decaffeination operation. It will be appreciated that the advantages achieved by restoration to a coffee extract of such principles will depend upon the nature of the coffee extract and the selectivity of the caffeine solvent used in the decaffeination operation. For example, ethyl acetate will remove from a coffee extract, in addition to caffeine, an appreciable content of aroma and flavor principles, relative to a more selective solvent such as methylene chloride. Accordingly, the benefits of the process of the invention will be most advantageous and the greatest contribution realized where relatively non-selective solvents are employed.The process of the invention, thus, makes more feasible the use of such solvents for the decaffeination of coffee.

The removal of caffeine from the caffeineladen solvent results in the recovery in the solvent of certain flavor and aroma principles. These principles, when restored to the decaffeinated coffee extract, permit the preparation of a decaffeinated coffee extract having as much of the aroma and flavor principles as is practicable. Thus, the extract when dried in a conventional manner to a soluble or instant coffee product, provides a product having improved flavor and aroma properties. While the precise chemical nature of the recovered flavor and aroma principles is not entirely understood, they are comprised of numerous flavorful and aromatic principles resulting from roasting and extraction or hydrolysis of coffee.The flavor and aroma principles, although water-soluble, have a greater affinity than caffeine for the organic solvent as is apparent from the recovery of such principles in the organic phase and recovery of caffeine in the aqueous phase.

The flavor and aroma principles recovered by the process of the invention are incorporated into the decaffeinated coffee extract prior to conventional drying thereof. The production of a soluble coffee powder from a decaffeinated coffee extract will be preceded by a solvent-stripping operation whereby residual solvent can be removed from the coffee extract. The flavor and aroma principles in the organic solvent can be added to the decaffeinated extract prior to the removal of residual solvent therefrom. Thus, the decaffeinated aqueous extract and the added solvent with flavor and aroma principles can be treated for simultaneous removal of solvent. Preferably, the solvent will be stripped from the decaffeinated extract by passing the extract over a heated evaporating surface under reduced pressure or by stripping with steam.Conventional thin-film evaporation devices can be used for this purpose. Other methods for volatilizing and recovering residual solvent can, however, be employed.

After stripping of residual solvent, condensed volatiles from the coffee extract obtained prior to the decaffeination thereof, if any. can be added to the extract. The resulting extract is then dried to a soluble coffee powder, e.g., by spray-drying or freeze-drying, with or without a prior concentration step.

The invention is illustrated in the following specific examples which are given by way of example only and not as limiting the invention. All percentages and ratios expressed in the specification and claims are bv weight.

EXAMPLE I An aqueous coffee extract having a solubles content of 20% is prepared by conventional countercurrent extraction of roast and ground coffee. The coffee extract is subjected to a devolatilization step by contacting the extract with steam (0.1 Ib. of steam/lb. of extract) in a packed column maintained at a vacuum of 21 inches of mercury. The steamstripped volatiles are condensed, and the condensate is stored at less than 50'F for subsequent reincorporation into the coffee extract.

The stripped, i.e., devolatilized, coffee extract is introduced as the dispersed phase into the bottom of a continuous countercurrent extractor (a Rotary-disk Contactor). The decaffeination solvent, methylene chloride, is introduced at the top of the extractor as the continuous phase. A solvent ratio of 1.0 lb. of solvent/lb. of coffee extract is used at a temperature of 90OF, and caffeine removal of 98% is achieved. The decaffeinated extract containing dissolved and entrained solvent is withdrawn from the top of the extractor. The decaffeination solvent containing caffeine and flavor and aroma constituents is withdrawn from the bottom of the extractor.

The decaffeination solvent containing caffeine and flavor and aroma constituents is evaporated to a solids concentration of about 5% by weight. The concentrated solvent is then introduced as the dispersed phase into the top of a second continuous countercurrent extractor (another Rotary-disk Contactor) with water as the continuous phase. A water-to-solvent ratio of 5.0 is used at a temperature of 70'F and a caffeine removal of 99% is achieved. The decaffeinated concentrated solvent stream containing the flavor and aroma constituents is withdrawn from the bottom of the extractor and added to the decaffeinated coffee extract. The resulting extract is then desolventized by steam-stripping in another packed column maintained at a vacuum of 21 inches mercury and using 0.1 lb. of steam/lb. of extract.

The residual solvent level in the decaffeinated coffee extract is reduced to less than 1 ppm on a solids basis. The decaffeinated coffee extract is then concentrated to 63% solubles by vacuum evaporation. The condensate of steam-stripped volatiles is added to the coffee extract, and the extract is spraydried to a 97% decaffeinated soluble coffee powder.

The resulting product is significantly stronger and has a more flavorful, balanced flavor than would a corresponding product made without recovery of flavor and aroma constituents from the caffeine-laden solvent and restoration thereof to the decaffeinated coffee extract.

EXAMPLE II An aqueous coffee extract having a solubles content of 20% is prepared by conventional countercurrent extraction of roast and ground coffee. The coffee extract is subjected to a devolatilization step by contacting the extract with steam (0.1 Ib. of steam/lb. of extract) in a packed column maintained at a vacuum of21 inches of mercury. The steamstripped volatiles are condensed, and the condensate is stored at less than 50"F for subsequent reincorporation into the coffee extract.

The stripped, i.e.. devolatilized, coffee extract is introduced as the dispersed phase into the top of a continuous countercurrent extractor (a Rotary-disk Contactor). The decaffeination solvent, ethyl acetate, is introduced at the bottom of the extractor as the continuous phase. A solvent ratio of 1.3 Ibs.

of solvent/lb. of coffee extract is used at a temperature of 140 F. and caffeine removal of 98% is achieved. The decaffeinated extract containing dissolved and entrained solvent is withdrawn from the bottom of the extractor.

The decaffeination solvent containing caffeine and flavor and aroma constituents is withdrawn from the top of the extractor.

The decaffeination solvent containing caffeine and flavor and aroma constituents is evaporated to a solids concentration of about 1.556 by weight. The concentrated solvent is then introduced as the dispersed phase into the bottom of a second continuous countercurrent extractor (another Rotary-disk Contractor) with water as the continuous phase.

A water-to-solvent ratio of 0.7 is used at a temperature of 70 F. and a caffeine removal of 99'S is achieved. The decaffeinated concentrated solvent stream containing the flavor and aroma constitutions is withdrawn from the top of the extractor and added to the decaffeinated coffee extract. The resulting extract is then desolventized by steamstripping in another packed column maintained at a vacuum of21 inches mercury and using 0.1 lb. of steam/lb. of extract. The residual solvent level in the decaffeinated coffee extract is reduced to less than I ppm on a solids basis. The decaffeinated coffee extract is then concentrated to 63% solubles by vacuum evaporation.The condensate of steam-stripped volatiles is added to the coffee extract. and the extract is spray-dried to a 97 decaffeinated soluble coffee powder.

The resulting product is significantly stronger and has a more flavorful. balanced flavor than would a corresponding product made without recovery of flavor and aroma constituents from the caffeine-laden solvent and restoration thereof to the decaffeinated coffee extract.

We are aware of the Solvents in Food Regulations 1582/1967 and no claim is made to the use of the present invention contrary to the law.

WHAT WE CLAIM IS:- 1. In the process of preparing a decaffeinated coffee, which comprises the steps of forming an aqueous extract of roast and ground coffee, decaffeinating said extract by contact with a water-immiscible organic solvent for caffeine, and separating the decaffeinated aqueous coffee extract from the caffeine-containing water-immiscible organic solvent, the improvement which comprises contacting the caffeine-containing water-immiscible organic solvent with an amount of water sufficient to partition caffeine into an aqueous phase, recovering the water-immiscible organic solvent containing flavor and aroma constituents and incorporating said water-immiscible organic solvent and flavor and aroma constituents into the decaffeinated roast and ground coffee extract.

2. The process of Claim 1 wherein caffeine is partitioned from said caffeine-containing water-immiscible organic solvent by contacting water and said solvent at a ratio of water to caffeine-containing solvent of 0.5:1 to 10:1.

3. The process of Claim 2 wherein the water-immiscible organic solvent is methylene chloride and the ratio is from 5:1 to 6:1.

4. The process of Claim 1 wherein subse- quent to said incorporation of water-immiscible organic solvent and flavor and aroma constituents into the decaffeinated roast and ground coffee extract the extract is desolventized.

5. The process of Claim 4 wherein the desolventized extract is dried to a soluble coffee powder.

6. The process of Claim 1 wherein the caffeine-containing water-immiscible solvent is concentrated prior to caffeine removal to a solids content of 1% to 10%.

7. The process of Claim 1 wherein the water-immiscible organic solvent is ethyl acetate.

8. The process of Claim 1, when carried out substantially as described in either of the Examples.

9. Decaffeinated coffee when produced by the process of any of the foregoing claims.

**WARNING** end of DESC field may overlap start of CLMS **.

Claims (9)

**WARNING** start of CLMS field may overlap end of DESC **. stronger and has a more flavorful, balanced flavor than would a corresponding product made without recovery of flavor and aroma constituents from the caffeine-laden solvent and restoration thereof to the decaffeinated coffee extract. EXAMPLE II An aqueous coffee extract having a solubles content of 20% is prepared by conventional countercurrent extraction of roast and ground coffee. The coffee extract is subjected to a devolatilization step by contacting the extract with steam (0.1 Ib. of steam/lb. of extract) in a packed column maintained at a vacuum of21 inches of mercury. The steamstripped volatiles are condensed, and the condensate is stored at less than 50"F for subsequent reincorporation into the coffee extract. The stripped, i.e.. devolatilized, coffee extract is introduced as the dispersed phase into the top of a continuous countercurrent extractor (a Rotary-disk Contactor). The decaffeination solvent, ethyl acetate, is introduced at the bottom of the extractor as the continuous phase. A solvent ratio of 1.3 Ibs. of solvent/lb. of coffee extract is used at a temperature of 140 F. and caffeine removal of 98% is achieved. The decaffeinated extract containing dissolved and entrained solvent is withdrawn from the bottom of the extractor. The decaffeination solvent containing caffeine and flavor and aroma constituents is withdrawn from the top of the extractor. The decaffeination solvent containing caffeine and flavor and aroma constituents is evaporated to a solids concentration of about 1.556 by weight. The concentrated solvent is then introduced as the dispersed phase into the bottom of a second continuous countercurrent extractor (another Rotary-disk Contractor) with water as the continuous phase. A water-to-solvent ratio of 0.7 is used at a temperature of 70 F. and a caffeine removal of 99'S is achieved. The decaffeinated concentrated solvent stream containing the flavor and aroma constitutions is withdrawn from the top of the extractor and added to the decaffeinated coffee extract. The resulting extract is then desolventized by steamstripping in another packed column maintained at a vacuum of21 inches mercury and using 0.1 lb. of steam/lb. of extract. The residual solvent level in the decaffeinated coffee extract is reduced to less than I ppm on a solids basis. The decaffeinated coffee extract is then concentrated to 63% solubles by vacuum evaporation.The condensate of steam-stripped volatiles is added to the coffee extract. and the extract is spray-dried to a 97 decaffeinated soluble coffee powder. The resulting product is significantly stronger and has a more flavorful. balanced flavor than would a corresponding product made without recovery of flavor and aroma constituents from the caffeine-laden solvent and restoration thereof to the decaffeinated coffee extract. We are aware of the Solvents in Food Regulations 1582/1967 and no claim is made to the use of the present invention contrary to the law. WHAT WE CLAIM IS:-

1. In the process of preparing a decaffeinated coffee, which comprises the steps of forming an aqueous extract of roast and ground coffee, decaffeinating said extract by contact with a water-immiscible organic solvent for caffeine, and separating the decaffeinated aqueous coffee extract from the caffeine-containing water-immiscible organic solvent, the improvement which comprises contacting the caffeine-containing water-immiscible organic solvent with an amount of water sufficient to partition caffeine into an aqueous phase, recovering the water-immiscible organic solvent containing flavor and aroma constituents and incorporating said water-immiscible organic solvent and flavor and aroma constituents into the decaffeinated roast and ground coffee extract.

2. The process of Claim 1 wherein caffeine is partitioned from said caffeine-containing water-immiscible organic solvent by contacting water and said solvent at a ratio of water to caffeine-containing solvent of 0.5:1 to 10:1.

3. The process of Claim 2 wherein the water-immiscible organic solvent is methylene chloride and the ratio is from 5:1 to 6:1.

4. The process of Claim 1 wherein subse- quent to said incorporation of water-immiscible organic solvent and flavor and aroma constituents into the decaffeinated roast and ground coffee extract the extract is desolventized.

5. The process of Claim 4 wherein the desolventized extract is dried to a soluble coffee powder.

6. The process of Claim 1 wherein the caffeine-containing water-immiscible solvent is concentrated prior to caffeine removal to a solids content of 1% to 10%.

7. The process of Claim 1 wherein the water-immiscible organic solvent is ethyl acetate.

8. The process of Claim 1, when carried out substantially as described in either of the Examples.

9. Decaffeinated coffee when produced by the process of any of the foregoing claims.