CA1242923A - Process for decaffeinating roasted coffee - Google Patents
Process for decaffeinating roasted coffeeInfo
- Publication number
- CA1242923A CA1242923A CA000461696A CA461696A CA1242923A CA 1242923 A CA1242923 A CA 1242923A CA 000461696 A CA000461696 A CA 000461696A CA 461696 A CA461696 A CA 461696A CA 1242923 A CA1242923 A CA 1242923A
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- Prior art keywords
- process according
- roasted coffee
- caffeine
- decaffeination
- flavoring substances
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
ABSTRACT
The invention relates to a process for extracting caffeine from roasted, ground coffee by means of CO2 at a pressure of from 50 to 200 bar and at a temperature of from 5 to 31°C., and the caffeine-loaded CO2 is passed through an acidic ion exchanger to remove the caffeine. The process offers the advantage that in short decaffeination periods high degrees of decaffeina-tion can be achieved.
The invention relates to a process for extracting caffeine from roasted, ground coffee by means of CO2 at a pressure of from 50 to 200 bar and at a temperature of from 5 to 31°C., and the caffeine-loaded CO2 is passed through an acidic ion exchanger to remove the caffeine. The process offers the advantage that in short decaffeination periods high degrees of decaffeina-tion can be achieved.
Description
Case 3049 PROCESS EOR DECAFFEINATING ROASTED COFFEE
DESCRIPTION
_ _ 05 The invention relates to a process for extract-ing caffeine from roasted, ground coffee by means of carbon dioxide.
The use of carbon dioxide for removing caffeine from coffee has been known. Numerous processes for decaffeination have been described in the literature.
German Patent No. 2,005,293 describes decaffeina-tion of moistened green coffee beans ~y means of supercritical CO2, i.e. at temperatures above 31C.
in a pressure range of 120 to 180 bar. Decaffein-ation carried out in this way takes from 5 to 15hours, and the subsequent drying takes from 2 to 5 hours.
German Patent No. 2,212,281 describes decaffeina-tion of green coffee with li~uid, i.e. subcritical, CO2 at temperatures below 31C. within a pressure range of about 80 to 400 bar. The minirnum decaffeina-tion period in this process is 14 hours.
Besides decaffeination of greerl coffee, a-ttempts have been made to deca~feinate also roasted coffee.
Thus, German Patent No. 2,119,67~ describes the decaffeination of roasted, ground coffee with super--critical CO2 by removing in a first step flavoring oil and, in a second step, the caffeine, after the f~ 3~
roasted coffee has been moistened. This mode of operation prevents flavoring substances from being extracted, too. This two-step process takes 10 hours on the average, i.e. 5 hours for each step.
05 German OS 2,638,383 describes decaffeination of green or roasted coffee extracts by means of liquid or supercritical CO2. Decaffeination of roasted coffee is accomplished in that the coffee firs-t is treated with water at elevated temperature, then the flavoring substances are removed from the aqueous solution, whereafter caffeine is extracted from aqueous solution at 15C. with liquid carbon dioxide or with supercritical carbon dioxide and is recovered from the carbon dioxide solution.
The two last-named processes dealing with the decaffeination of roasted coffee have the disadvant age in common that they are carried out in two steps, i.e. that first the flavoring substances must be removed and only thereafter the decaffeination proper can take place. Consequently, the time required for the entire process is considerable.
All the known decaffeination processes operat-ing with the use of carbon dioxide have in common that the decaffeina-tion step -takes at leas-t 4 to 5 hours, in many cases substantially longer.
Moreover, in cases where supercritical CO2 is employed -the temperatures normally range from 40 to - 80C. In order to preserve the flavor characteristics of the product it would be more favorable to operate at lower temperatures.
It is the object of the invention to provide a process for decaffeinating roasted coffee with which it is possible.
1. to remove the caffeine from the roasted coffee in a mild way;
DESCRIPTION
_ _ 05 The invention relates to a process for extract-ing caffeine from roasted, ground coffee by means of carbon dioxide.
The use of carbon dioxide for removing caffeine from coffee has been known. Numerous processes for decaffeination have been described in the literature.
German Patent No. 2,005,293 describes decaffeina-tion of moistened green coffee beans ~y means of supercritical CO2, i.e. at temperatures above 31C.
in a pressure range of 120 to 180 bar. Decaffein-ation carried out in this way takes from 5 to 15hours, and the subsequent drying takes from 2 to 5 hours.
German Patent No. 2,212,281 describes decaffeina-tion of green coffee with li~uid, i.e. subcritical, CO2 at temperatures below 31C. within a pressure range of about 80 to 400 bar. The minirnum decaffeina-tion period in this process is 14 hours.
Besides decaffeination of greerl coffee, a-ttempts have been made to deca~feinate also roasted coffee.
Thus, German Patent No. 2,119,67~ describes the decaffeination of roasted, ground coffee with super--critical CO2 by removing in a first step flavoring oil and, in a second step, the caffeine, after the f~ 3~
roasted coffee has been moistened. This mode of operation prevents flavoring substances from being extracted, too. This two-step process takes 10 hours on the average, i.e. 5 hours for each step.
05 German OS 2,638,383 describes decaffeination of green or roasted coffee extracts by means of liquid or supercritical CO2. Decaffeination of roasted coffee is accomplished in that the coffee firs-t is treated with water at elevated temperature, then the flavoring substances are removed from the aqueous solution, whereafter caffeine is extracted from aqueous solution at 15C. with liquid carbon dioxide or with supercritical carbon dioxide and is recovered from the carbon dioxide solution.
The two last-named processes dealing with the decaffeination of roasted coffee have the disadvant age in common that they are carried out in two steps, i.e. that first the flavoring substances must be removed and only thereafter the decaffeination proper can take place. Consequently, the time required for the entire process is considerable.
All the known decaffeination processes operat-ing with the use of carbon dioxide have in common that the decaffeina-tion step -takes at leas-t 4 to 5 hours, in many cases substantially longer.
Moreover, in cases where supercritical CO2 is employed -the temperatures normally range from 40 to - 80C. In order to preserve the flavor characteristics of the product it would be more favorable to operate at lower temperatures.
It is the object of the invention to provide a process for decaffeinating roasted coffee with which it is possible.
1. to remove the caffeine from the roasted coffee in a mild way;
2. to achieve a high degree of decaffeination;
3. to carry out the decaffeination in a 05single step; and
4. to carry out the decaffeination in as short a time as possible.
This object is accomplished with a process of the initially defined type which is characterized in that the ex-traction is carried out with liquid CO2 at a pressure of from 50 to 200 bar, preferably 80 to 150 bar, and at a temperature of from 5 to 31C., preferably 15 to 31C., and the caffeine-loaded CO2 is passed through an acidic ion exchanger to remove the caffeine.
It has been surprisingly found that with the presently proposed process it is possible to carry out the decaffeination in a relatively very short time, i.e. in less than 4 hours, in most cases in less than 3 hours, and at the same time to achieve an unusually high degree of decaffeination. This result is all the more surprising since with the use of the otherwise conventional decaffeination periods no improvement but a deterioration of the results is obtained.
The efficiency of a decaffeination process may be determined by means of the following relationship between the decaffeination degree and the decaffein ation period:
Ct (CO) X ~e kt) so that k is k = _ ln Ct/co Therein ct is the caffeine content in per cent after -the time t; cO is the initial caffeine content in per cent; and t is the decaffeination period in hours. The efficiency of the decaffeination is reflected by the decaffeination factor k.
While for all the known decaffeination process operating with the use of supercritical or li~uid CO2 only k-values of less than 1, partially even values substantially below 1, have been reached, it is possible with the process of the invention to attain k-values that are markedly higher than 1.
Surprisingly the process of the invention is the most efficient decaffeination process hitherto found, no matter whether it is carried out wi-th supercritical or subcritical Co2 to enhance the efficiency, as described, for example, in Gerrnan oS 2,737,793.
In the process of the invention the roasted coffee is first moistened with water, typically to a moisture conten-t of from 20 to 50% by weight. Then the liquid carbon dioxide is circula-ted through the con-tainer charged with the roasted coffee. The -temperature ranges between 5 or 15 and 30C., respec-tively; preferably the~process is carried out at ambient -temperature. The pressure is at least equal to the equilibrium pressure of the liguid CO2 at the prevailing temperature, i.e. it ranges between 50 :. .
~2~ 3 and ~0 bar. The upper limit is about 200 bar;
preferably 150 bar should not be exceeded. Under these conditions the density of the liquid C02 is about 0.7 to 0.85.
05 In the circulation system an ion exchanger is interposed which selectively removes the caffeine from the liquid C02. Since also flavoring substances can be extracted from the roasted coffee b~ means of the liquid C02, it is necessary that the ion e~changer operates selectively with respect to the caffeine.
Acidic ion exchanges, especially highly acidic ion exchangers, may be employed. Thus, for instance, the following ion exchangers may be used for the contemplated purpose:
- polystyrene resin with sulfonic acid as anchoring group;
- polycondensation resin with phenol sulfonic acid as anchoring group.
. Since increasingly more flavoring substances are extracted from the product at pressures abo~e 150 and particularly above 200 bar, it is more favorable to operate below a pressure of 150 bar.
Normally the extraction is terminated after 2 to 3 hours. The degree of decaffeination cannot be increased by longer extraction periods. Rather does the degree of decaffeination surprisingly decrease, as will be shown further below.
After termination of the decaffeination the quantities of flavoring substances contained in the C2 are isolated by simple evaporation of the C02 and are recombined with the roasted coffee. The C02 is recovered. The ion exchangers can be cleaned and the caffeine can be recovered by treatment of the ion exchangers with liquid carbon dioxide at elevated pressures, i.e. at pressures above 200 bar.
In a preferred embodiment of the process the liguid C02 employed is pre-loaded with the flavoring 05 substances of the product that tend to be co-extracted - to a certain extent during decaffeination so tat pre-loading markedly reduces this tendency. Pre-load-ing is accomplished by passing dry liquid CO2 over roasted coffee and extracting the flavoring substances.
The preferably saturated CO2 thus pre loaded with roasted coffee flavoring substances - after having been moistened - will extract the ca~feine more selectively from a new roasted coffee charge.
According to another embodiment of this inven-tion, the roasted coffee may be stripped or otherwisedepleted of the flavoring substances before being decaffeinated by means of the li~uid C02. Flavoring substances may be removed by means of steam stripping or extraction with a non-toxic, selective solvent such as dry liquid CO2 or dry supercritical CO2.
Desriably any flavoring material removed from the roasted coffee prior to deca~feination is added back to an aqueous extract obtained form the decaffeinated roasted coffee~ The aromatized, decaffeinated extract would then be dried.
The fi~ure shows schematically an apparatus by means of which the process of the invention can be carried out. The figure illustrates an extraction vessel l and an adsorber 2 which, through a heat exchanger 3 and a circulating pump 4, are connected to form a circulation system. By means of the booster pump 5 to CO2 is introduced into the circu-lation system from a tank (not shown). ~he heat exchanger 3 serves for adaption to the operating temperature. In the extraction vessel l there is the roasted, ground coffee, while in the adsorber 2 the ion exchanger is accomodated. The circulating pump 4 takes care of the circulation.
The invention will now be further explained by 05 the folowing examples.
Example l 1.5 kg of roasted ground coffee having an average particle size of lmm was moistened with 0.5 kg water. In the extraction vessel 1 it was extracted at 29C. for 2.5 hours with liquid carbon dioxide at a pressure of 85 bar (density of CO2 = 0.703). A
highly acidic ion exchanger was employed as adsorbent.
The initial caffeine content of the coffee was 1.74%. After extraction the flavoring substances contained in the CO2 were removed by evaporation of the C02 and recombined with the coffee. The final coffee product had a residual caffeine content of 0.028%. Hence, the decaffeination factor k = 1.65.
The final roasted coffee was a perfect product which did not differ sensorially from -the starting coffee product.
Examples 2 to 6 Example 1 was repeated at different pressures and in different decaffeination periods. The decaffeinati.on temperature was 29C. in all instances.
The resulks are compiled in the following Table I.
TABLE I
Example Pres- Decaffeina- Initial Final Decaffeina- Decaffeina-sure tion Period Caffeine Caffeine tion Degree tion Factor 05 (bar) (hrs) c~(%) ct(%) (%) K
2 300 4.3 1.74 0.17 90.2 0.54 3 200 ~.3 1.74 0.17 90.2 0.54 lO 4 200 2.0 1.74 0.059 96.6 1.35 ~5 2.5 1.74 0.030 98.3 1.62 6 ~5 2.5 1.74 0.032 98.2 1.60 15 Table I shows that optimum results are obtained at about equilibrium pressure and in a decaffeination period of about 2.5 hours. Furthermore, the Table shows that inferior decaffeination degrees are ob-tained at excessively high pressure and in excessively long decaffeination periods. This might be due to t~e fact that at higher pressures and especially after decaffeination periods longer than 4 hours the caffeine is desorbed from the exchanger column.
~ence, surprisingly -the optimum results are obtained in rela-tively very short decaffeination perlods. In the examples 4 to 6 of the inven-tion the value of the decaffeination factor is markedly above the value 1Ø By way of comparison the following Table II shows tha-t in known decaffeination processes using carbon dioxide k-values invariably lower than 1.0, partially substantially below 1.0, are reached.
TAB~E II
Patent Tempera- Pres- Decaffeina- Final Initial Decaffeina-ture sure tion Period Caf:Eeine Caffeine tion Factor 05 (C) (bar)(hrs.) ct (%) cO (%) K
German 2,005,293 70 160 5 - 30 0.01 1.2 0.95 - 0.15 German lO2,119,678 50 280 4 0.03 1.2 0.922 German 2,212,281 20 350 14 0.05 1.04 0.22 German 2,727,191 70 250 8 0.08 1.02 0.322
This object is accomplished with a process of the initially defined type which is characterized in that the ex-traction is carried out with liquid CO2 at a pressure of from 50 to 200 bar, preferably 80 to 150 bar, and at a temperature of from 5 to 31C., preferably 15 to 31C., and the caffeine-loaded CO2 is passed through an acidic ion exchanger to remove the caffeine.
It has been surprisingly found that with the presently proposed process it is possible to carry out the decaffeination in a relatively very short time, i.e. in less than 4 hours, in most cases in less than 3 hours, and at the same time to achieve an unusually high degree of decaffeination. This result is all the more surprising since with the use of the otherwise conventional decaffeination periods no improvement but a deterioration of the results is obtained.
The efficiency of a decaffeination process may be determined by means of the following relationship between the decaffeination degree and the decaffein ation period:
Ct (CO) X ~e kt) so that k is k = _ ln Ct/co Therein ct is the caffeine content in per cent after -the time t; cO is the initial caffeine content in per cent; and t is the decaffeination period in hours. The efficiency of the decaffeination is reflected by the decaffeination factor k.
While for all the known decaffeination process operating with the use of supercritical or li~uid CO2 only k-values of less than 1, partially even values substantially below 1, have been reached, it is possible with the process of the invention to attain k-values that are markedly higher than 1.
Surprisingly the process of the invention is the most efficient decaffeination process hitherto found, no matter whether it is carried out wi-th supercritical or subcritical Co2 to enhance the efficiency, as described, for example, in Gerrnan oS 2,737,793.
In the process of the invention the roasted coffee is first moistened with water, typically to a moisture conten-t of from 20 to 50% by weight. Then the liquid carbon dioxide is circula-ted through the con-tainer charged with the roasted coffee. The -temperature ranges between 5 or 15 and 30C., respec-tively; preferably the~process is carried out at ambient -temperature. The pressure is at least equal to the equilibrium pressure of the liguid CO2 at the prevailing temperature, i.e. it ranges between 50 :. .
~2~ 3 and ~0 bar. The upper limit is about 200 bar;
preferably 150 bar should not be exceeded. Under these conditions the density of the liquid C02 is about 0.7 to 0.85.
05 In the circulation system an ion exchanger is interposed which selectively removes the caffeine from the liquid C02. Since also flavoring substances can be extracted from the roasted coffee b~ means of the liquid C02, it is necessary that the ion e~changer operates selectively with respect to the caffeine.
Acidic ion exchanges, especially highly acidic ion exchangers, may be employed. Thus, for instance, the following ion exchangers may be used for the contemplated purpose:
- polystyrene resin with sulfonic acid as anchoring group;
- polycondensation resin with phenol sulfonic acid as anchoring group.
. Since increasingly more flavoring substances are extracted from the product at pressures abo~e 150 and particularly above 200 bar, it is more favorable to operate below a pressure of 150 bar.
Normally the extraction is terminated after 2 to 3 hours. The degree of decaffeination cannot be increased by longer extraction periods. Rather does the degree of decaffeination surprisingly decrease, as will be shown further below.
After termination of the decaffeination the quantities of flavoring substances contained in the C2 are isolated by simple evaporation of the C02 and are recombined with the roasted coffee. The C02 is recovered. The ion exchangers can be cleaned and the caffeine can be recovered by treatment of the ion exchangers with liquid carbon dioxide at elevated pressures, i.e. at pressures above 200 bar.
In a preferred embodiment of the process the liguid C02 employed is pre-loaded with the flavoring 05 substances of the product that tend to be co-extracted - to a certain extent during decaffeination so tat pre-loading markedly reduces this tendency. Pre-load-ing is accomplished by passing dry liquid CO2 over roasted coffee and extracting the flavoring substances.
The preferably saturated CO2 thus pre loaded with roasted coffee flavoring substances - after having been moistened - will extract the ca~feine more selectively from a new roasted coffee charge.
According to another embodiment of this inven-tion, the roasted coffee may be stripped or otherwisedepleted of the flavoring substances before being decaffeinated by means of the li~uid C02. Flavoring substances may be removed by means of steam stripping or extraction with a non-toxic, selective solvent such as dry liquid CO2 or dry supercritical CO2.
Desriably any flavoring material removed from the roasted coffee prior to deca~feination is added back to an aqueous extract obtained form the decaffeinated roasted coffee~ The aromatized, decaffeinated extract would then be dried.
The fi~ure shows schematically an apparatus by means of which the process of the invention can be carried out. The figure illustrates an extraction vessel l and an adsorber 2 which, through a heat exchanger 3 and a circulating pump 4, are connected to form a circulation system. By means of the booster pump 5 to CO2 is introduced into the circu-lation system from a tank (not shown). ~he heat exchanger 3 serves for adaption to the operating temperature. In the extraction vessel l there is the roasted, ground coffee, while in the adsorber 2 the ion exchanger is accomodated. The circulating pump 4 takes care of the circulation.
The invention will now be further explained by 05 the folowing examples.
Example l 1.5 kg of roasted ground coffee having an average particle size of lmm was moistened with 0.5 kg water. In the extraction vessel 1 it was extracted at 29C. for 2.5 hours with liquid carbon dioxide at a pressure of 85 bar (density of CO2 = 0.703). A
highly acidic ion exchanger was employed as adsorbent.
The initial caffeine content of the coffee was 1.74%. After extraction the flavoring substances contained in the CO2 were removed by evaporation of the C02 and recombined with the coffee. The final coffee product had a residual caffeine content of 0.028%. Hence, the decaffeination factor k = 1.65.
The final roasted coffee was a perfect product which did not differ sensorially from -the starting coffee product.
Examples 2 to 6 Example 1 was repeated at different pressures and in different decaffeination periods. The decaffeinati.on temperature was 29C. in all instances.
The resulks are compiled in the following Table I.
TABLE I
Example Pres- Decaffeina- Initial Final Decaffeina- Decaffeina-sure tion Period Caffeine Caffeine tion Degree tion Factor 05 (bar) (hrs) c~(%) ct(%) (%) K
2 300 4.3 1.74 0.17 90.2 0.54 3 200 ~.3 1.74 0.17 90.2 0.54 lO 4 200 2.0 1.74 0.059 96.6 1.35 ~5 2.5 1.74 0.030 98.3 1.62 6 ~5 2.5 1.74 0.032 98.2 1.60 15 Table I shows that optimum results are obtained at about equilibrium pressure and in a decaffeination period of about 2.5 hours. Furthermore, the Table shows that inferior decaffeination degrees are ob-tained at excessively high pressure and in excessively long decaffeination periods. This might be due to t~e fact that at higher pressures and especially after decaffeination periods longer than 4 hours the caffeine is desorbed from the exchanger column.
~ence, surprisingly -the optimum results are obtained in rela-tively very short decaffeination perlods. In the examples 4 to 6 of the inven-tion the value of the decaffeination factor is markedly above the value 1Ø By way of comparison the following Table II shows tha-t in known decaffeination processes using carbon dioxide k-values invariably lower than 1.0, partially substantially below 1.0, are reached.
TAB~E II
Patent Tempera- Pres- Decaffeina- Final Initial Decaffeina-ture sure tion Period Caf:Eeine Caffeine tion Factor 05 (C) (bar)(hrs.) ct (%) cO (%) K
German 2,005,293 70 160 5 - 30 0.01 1.2 0.95 - 0.15 German lO2,119,678 50 280 4 0.03 1.2 0.922 German 2,212,281 20 350 14 0.05 1.04 0.22 German 2,727,191 70 250 8 0.08 1.02 0.322
Claims (15)
1. A process for extracting caffeine from roasted, ground coffee by means of CO2 characterized in that the extraction is carried out with liquid CO2 at a pressure of from 50 to 200 bar and at a temperature of from 5 to 31°C., and the caffeine-loaded CO2 is passed through an acidic ion exchanger to remove the caffeine.
2. Process according to claim 1 characterized in that the pressure ranges from 80 to 150 bar.
3. Process according to claim 1 wherein the pressure is at least about the equilibrium pressure of the liquid CO2 at the prevailing temperature.
4. Process according to claim 1 wherein the density of the liquid CO2 is about 0.7 to 0.85.
5. Process according to claim 1 wherein the temperature ranges from about 15 to about 31°C.
6. Process according to claim 1 wherein the extraction is carried out for a period of time of less than 4 hours.
7. Process according to claim 1 wherein the roasted coffee is first moistened with water to a moisture content of from about 20 to about 50% by weight.
8. Process according to claim 1 wherein the extraction is carried out at ambient temperature.
9. Process according to claim 1 wherein said acidic ion exchanger is selected from the group consisting of polystyrene resin with sulfonic acid as anchoring group and polycondensation resin with phenol sulfonic acid as anchoring group.
10. Process according to claim 6 wherein said period of time is between 2 and 3 hours.
11. Process according to claim 1 including the further steps of isolating quantities of flavoring substances contained in the CO2 by evaporation of the CO2, and then recombining said flavoring substances with the roasted coffee.
12. Process according to claim 1 wherein said CO2 is first pre-loaded with flavoring substances of the roasted coffee.
13. Process according to claim 12 wherein said pre-loading comprises the steps of passing dry liquid CO2 over roasted coffee and extracting the flavoring substances.
14. Process according to claim 1 wherein said roasted coffee is initially stripped of flavoring substances before being decaffeinated.
15. Process according to claim 14 wherein said stripping step comprises steam stripping, or extraction with a non-toxic, selective solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000461696A CA1242923A (en) | 1984-08-23 | 1984-08-23 | Process for decaffeinating roasted coffee |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000461696A CA1242923A (en) | 1984-08-23 | 1984-08-23 | Process for decaffeinating roasted coffee |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1242923A true CA1242923A (en) | 1988-10-11 |
Family
ID=4128579
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000461696A Expired CA1242923A (en) | 1984-08-23 | 1984-08-23 | Process for decaffeinating roasted coffee |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA1242923A (en) |
-
1984
- 1984-08-23 CA CA000461696A patent/CA1242923A/en not_active Expired
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MKEX | Expiry | ||
| MKEX | Expiry |
Effective date: 20051011 |