Method for recovering caffeine
专利摘要:
Decaffeination of green coffee beans with an aqueous medium, whereby caffeine is removed from the aqueous medium which also contains non-caffeine green coffee solids, by adsorption with substantially neutral active carbon. Thereafter the medium may be recycled to extract further amounts of caffeine from the same or another batch of green coffee beans. 公开号:SU1056875A3 申请号:SU813276096 申请日:1981-04-09 公开日:1983-11-23 发明作者:Греен Давид;Бланк Морис 申请人:Сосьете Де Продюи Нестле С.А. (Фирма); IPC主号:
专利说明:
ate O5 00 A1 The invention relates to methods for extracting caffeine from an aqueous solution containing caffeine extracted from green coffee beans. Lime is a method of extracting caffeine, involving direct contact between the grains and the caffeine solvent, followed by separation of the latter. The disadvantage of this method is the difficulty of releasing caffeine. The closest in technical essence and the achieved result to the invention is a method of extracting caffeine from an aqueous solution containing caffeine extracted from green grains, which involves treating the solution with activated carbon. Among the various solid adsorbents, activated carbon has certain advantages over other substances, such as polymer resins, due to its availability and easy iZ regeneration. However, it has been observed that contact between the aqueous extract and activated carbon leads to an increase in p which is associated with a deterioration in the color and taste of the coffee beans. The aim of the invention is to improve the taste and aroma of coffee. This goal is achieved in that, according to the method for extracting caffeine from an aqueous solution, caffeine extracted from green 1 ........,. "..... ..., .-." ...,. ... grains, which involve treating the solution with activated carbon, before treating the aqueous solution with activated carbon, the latter is neutralized with hydrochloric acid in the case of using thermally activated carbon or sodium hydroxide in the case of using phosphoric activated carbon, followed by washing with deionized water until pH is reached etc washwater equals 6.0. The essence of the method is as follows. An aqueous solution of caffeine is obtained according to standard procedures involving contacting green coffee beans with water for the time required to reduce the caffeine content of the beans to the desired level. Contacting can be carried out in a countercurrent system using equipment similar to that used in the process of preparing coffee extract by extracting roasted coffee, or periodic contacting can be used in which a fixed amount of water is continuously recycled through a fixed portion of coffee beans, and in each cycle caffeine is removed from extract before the next feed it to the grain. In a countercurrent system, an aqueous extracting medium, containing caffeine and solid, caffeine-free coffee, moves towards the raw coffee, with a significantly higher caffeine content .. When leaving the system, the caffeine-enriched extract passes the adsorbent, preferably again in the countercurrent column . The main factors affecting the process are the following: temperature, the ratio of solvent (extractant) to coffee, the ratio of carbon to coffee, time and speed of movement of the liquid, each of these factors can affect the desired degree of decaffeination. When carrying out the process in accordance with the invention, the neutral activated carbon of the south will be used either in a batch apparatus or in a continuous apparatus with a countercurrent system. In both cases, for the continuous process, it is usually envisaged that the adsorbent layers are doubled, so that one or several n / ™ ir ciU-f a-g 3i / I H PM pm LJA Lff can be replaced, while the rest are and work. Decaffeination of green coffee beans is carried out with deionized water; The ratio of water to coffee is by no means a decisive parameter; however, to some extent it is determined, from practical considerations, an industrial process. For these reasons, excess volumes are excluded, as well as the ratio of water to 1 ;; oe, which do not provide sufficient extraction of caffeine. It has been found that a generally weight ratio of water to green coffee, constituting at least about three parts of water to one part of green coffee, gives satisfactory results. In one preferred embodiment, green coffee beans are in contact on a fixed bed aide in a column or in a suitable rotary drum, or in an apparatus, like an extractor. In both cases, the weight of water and coffee is constant, the water enriched with caffeine, after leaving the column or extractor, is decaffeinated with neutral activated carbon before it is recycled. The weight of the coal is 20-30% by weight of green decaffeinated coffee. The cumulative contact time depends, among other things, on the water / coffee ratio, temperature and the desired degree of decaffeination. In most cases, it is 3-50 hours. The preferred temperature range is from 60 to. Lower temperatures are excluded, especially for long contact times, due to the increased growth of microbiological activity, which leads to the fermentation of sucrose present in the extract. In addition, the diffusion rate of caffeine from beans decreases with temperature. Above, with a long contact time, the aroma (taste) may deteriorate, and in practice such temperatures are difficult to maintain without resorting to leak-proof equipment. In another preferred embodiment, the continuous extraction and decaffeination process of green coffee beans uses a counter system. For processing green coffee, equipment similar to the equipment used to extract roasted coffee is used. Fresh water entering the extractor usually has a temperature of 90-120 C. It is preferable to use deionized water. The ratio of water to coffee is not decisive, but the ratio in the range from 3: 1 to 15: 1 by weight is mainly used. The number of extractors and the cycle time are chosen such as to obtain the desired degree of decaffeination. Up to eight serially connected extractors with cycle times from 15 to 120 minutes can be used. WATER extract containing caffeine and solid, caffeine-free green coffee can be concentrated, for example, in a countercurrent system, before removing caffeine by contacting with neutral activated carbon. In this system, coal is contained in several columns, and the extract passes successively through these columns. Periodically, the most saturated column is shut off from the system and replaced with a column containing syzhey coal. In the columns: the preferred temperature is from 60 to 90 ° C. The number of columns, the cycle time for each column and the residence time of the extract are chosen so as to achieve the desired degree of decaffeination and to minimize the amount of coal used. The weight of the coal is usually 10-20% by weight of decaffeinated green coffee. The contact temperature between the coal and the extract is desirable at least about 60 ° C to eliminate microbiological problems, while for the same reasons, the temperature in the receiving device of the column must be slightly higher. Since activated carbon adsorbs acids as well as caffeine, the pH of the aqueous extract increases, reaching a maximum of 6.0 to 7.5 However, as the process progresses, the pH drops again so that, for example, at 97% decaffeinization, the pH is less than one. above the natural pH of the aqueous extract of green grains. Conversely, the pH of the green grain extract in contact with non-neutralized activated carbon is above 9.0, which apparently also explains the deterioration in color and flavor. When decafining is complete, it is usually desirable to avoid excessive loss of the solid residue present in the aqueous extract to decaffeinated green grains. Grains can be dried usually to wt.% Moisture and combine directly with the extract. Alternatively, pre-concentrate extract; for example, by evaporation, to 15-55% by weight of the solid residue before contact with the grains. A satisfactory re-consolidation of the solid residue is achieved in C-8 hours at a temperature of preferably 60-80 ° C. It is desirable that the total amount of water present is such that the final moisture content in the beans does not exceed about 55 wt.%. The total water is composed of residual moisture of pre-dried grains and water, present in the aqueous extract. After re-combining the solid residue, the coffee is dried so that the moisture content before frying is 5-12% by weight. The amount of solid caffeine residue in contact with the coffee beans can be less than the amount extracted during decaffeination. Periodically activated carbon should be regenerated, usually by heating or by solvent extraction. Example 1. Neutralized activated carbon is obtained by washing commercial thermally activated carbon with hydrochloric acid and then washing with deionized water (pH 6.0) until the pH of the wash water is equal to 6.0, 2000 hours of green coffee beans are loaded into rotary extractor drum along with 7000 parts of deionized water. The temperature is raised and maintained at 80 ° C. The solution after the extractor at a rate of 15,000 hours passes through a column containing 230 hours of neutralized activated carbon before returning to the extractor. After one hour, the second is connected in series. a column also containing 230 parts of neutralized activated Peep After 5 hours of total process the recirculation is stopped, and the extract, having a pH of 6.2, is separated from the coffee beans, dried to a moisture content of 2%, and mixed with the extract, which was previously concentrated to 20 solid residue. Mixing is carried out for 6 hours at. After this, the coffee with 5 humidity is dried to a moisture content of 8.5. Coffee Decaffeinated Up to 97% He has a good appearance, similar to the original non-decanelised grains, but partly darker in color. The coffee drink obtained from the roasted beans, according to tasters, has good taste quality and color. When milk is added to a cup, the color of the coffee takes on a reddish-brown tint without admixture of gray. Examples 2-k. The decaffeination procedure described in Example 1 was repeated with various material modifications and process parameter variations. Results are summarized in the table. Measured in distilled water-at. After decaffeination, the non-caffeine solids are combined with decaffeinated beans. Example S- Green coffee beans are decaffeinated with an aqueous solution; continuously by countercurrent extraction. Used 6 series-connected extractors, each of which contains 60 kg of green coffee. Extraction is carried out with deionized water, the temperature of which is at the entrance to the most exhausted extractor equals. The aqueous pactor, which contains caffeine and decaffeinated solid green beans, is removed from the extractor with the least spent coffee. The last extractor containing decaffeinated coffee is removed once per hour from the system and replaced with an extractor with fresh green coffee beans. The ratio of water to green coffee beans is 10: 1, so that the flow rate of water entering the system is equal to OHL l / h. one The extract coming out of the apparatus with the least spent green coffee in countercurrent is directed through three columns connected in series, each of which contains 35 kg of neutralized activated carbon obtained by a method similar to that described in Example I, the temperature of the columns is maintained at 75 ° C. hours the most saturated coal column with fresh coal. . Decaffeinated green beans are dried to 20% moisture content and mixed with the appropriate amount of decaffeinated extract, which is pre-concentrated to 20% solids. 568758 Mixing is carried out for 6 hours. Bri 75s After this, the coffee with 5% moisture content is dried to 9 moisture content. 5 Example6.1kg phosphorus activated carbon (Norit, the Netherlands) was suspended in distilled water. The pH of the suspension is 2.5. Then, 23 g of sodium hydroxide, dissolved in a small amount of distilled water, was added, and the suspension was vigorously stirred. Then the coal was filtered and washed until neutral wash water. The proposed method allows to obtain a decaffeinated product with improved taste and aroma.
权利要求:
Claims (1) [1] METHOD FOR REMOVING CAFFEINE from an aqueous solution containing caffeine extracted from green beans, comprising treating the solution with activated carbon, characterized in that, in order to improve the taste and aroma of coffee, before processing the aqueous solution with activated carbon, the latter is neutralized with hydrochloric acid in the case of using thermally activated carbon or sodium hydroxide in the case of using coal activated with phosphoric acid, followed by washing with deionized water until the pH is washed waters equal to 6.0. Οι smiling 00 Joint venture
类似技术:
公开号 | 公开日 | 专利标题 SU1056875A3|1983-11-23|Method for recovering caffeine US4160042A|1979-07-03|Process for treating an aqueous extract of a vegetable material US4317841A|1982-03-02|Process for the deacidification of a coffee extract US4031251A|1977-06-21|Decaffeination of vegetable material US4976983A|1990-12-11|Coffee product with reduced malic acid content US4444798A|1984-04-24|Process for removing stimulating compounds from cocoa US5208056A|1993-05-04|Process for decaffeinating raw coffee US3790689A|1974-02-05|Extraction of roasted and ground coffee US4390698A|1983-06-28|Detheobromination of cocoa CA2028643A1|1991-04-29|Process for improving the quality of robusta coffee AU650924B2|1994-07-07|Decaffeinated coffee products with reduced potassium content GB2029688A|1980-03-26|Process for deacidifying a coffee extract and the deacidified extract obtained CA1196811A|1985-11-19|Recovery of xanthine stimulants from aqueous media US4508743A|1985-04-02|Caffeine adsorption CA1203111A|1986-04-15|Process for restoring virtually caffeine-free coffeebean extract substances into coffee beans which havebeen extracted with an aqueous liquid and havethereby been decaffeinated US4204004A|1980-05-20|Infusing bag containing combination of dried extract and ligneous adsorbent and process of preparing same Katz1987|Decaffeination of coffee ES8602363A1|1985-12-01|A process for removing chlorogenic acid compounds and caffeine from coffee, and roasted coffee obtainable by this process. US5288511A|1994-02-22|Supercritical carbon dioxide decaffeination of acidified coffee US4237288A|1980-12-02|Decaffeination of fatty materials EP0111375B1|1986-10-01|A process for decaffeinating green coffee beans with active carbon US5266342A|1993-11-30|Method for decaffeinating coffee materials including a reverse osmosis permeate recycle US4087562A|1978-05-02|Decaffeination of green coffee EP0050482B1|1984-07-11|A method for the production of decaffeinated tea CA1123656A|1982-05-18|Process for decaffeinating raw coffee
同族专利:
公开号 | 公开日 AT388487B|1989-06-26| EP0040712A1|1981-12-02| NZ197009A|1983-05-10| GB2076626B|1984-10-03| GB2076626A|1981-12-09| DE3119277C2|1991-04-25| DD158736A5|1983-02-02| AU7017381A|1981-12-03| ES8207415A1|1982-10-01| EP0040712B1|1984-04-18| IT8148226D0|1981-04-08| IL62789D0|1981-07-31| PL127869B1|1983-12-31| GR75660B|1984-08-02| US4495210A|1985-01-22| MX158675A|1989-02-27| CA1162436A|1984-02-21| AU542970B2|1985-03-28| PL231342A1|1982-02-15| IT8148557D0|1981-05-27| KE3527A|1985-06-07| DE3119277A1|1982-04-15| ZA812953B|1982-05-26| JPH0145345B2|1989-10-03| PT72782B|1982-03-22| IL62789A|1983-10-31| ES502543A0|1982-10-01| JPS5712952A|1982-01-22| EP0040712B2|1989-04-19| IT1171255B|1987-06-10| ATA218281A|1983-08-15| PH16963A|1984-04-27| PT72782A|1981-04-01|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 RU2746120C2|2016-05-19|2021-04-07|Декафино, Инк.|Caffeine-absorbing material, caffeine-absorbing system, decaffeination system, and related methods for removing caffeine from solutions|FR741904A|1933-02-23| FR741903A|1933-02-23| DD78586A| FR503796A|1917-07-26|1920-06-17|Johan Nicolaas Adolf Sauer|Process for the treatment of liquids by the substance known as: "decolorizing carbon"| GB285386A|1927-02-14|1928-10-11|Ver Chemische & Metallurgische|Process for eliminating the acidity of acid activated charcoal| DE685367C|1933-09-08|1939-12-16|Coffex A G|Procedure for decaffeinating coffee| FR779451A|1933-09-08|1935-04-05|Coffex A G Soc|Method and apparatus for decaffeinating and improving green coffee| US2198859A|1938-05-18|1940-04-30|Max Brunner & Co|Process for decaffeinating coffee| CH211646A|1938-05-18|1940-10-15|Max Brunner & Co|Procedure for decaffeinating coffee.| CH623205A5|1977-07-29|1981-05-29|Nestle Sa| CH635485A5|1978-08-22|1983-04-15|Coffex Ag|METHOD FOR DECOFFINATING RAW COFFEE.|US4407834A|1981-05-21|1983-10-04|Societe D'assistance Technique Pour Produits Nestle S.A.|Recovery of xanthine stimulants from aqueous media| CH661409A5|1982-10-01|1987-07-31|Haco Ag|METHOD FOR RECYCLING PRACTICALLY COFFEIN-FREE BEAN COFFEE EXTRACTS IN COFFEE BEANS EXTRACTED WITH AN AQUEOUS LIQUID, AND THEREFORE DECANCIFIED BY THEM.| NL188074C|1982-12-10|1992-04-01|Douwe Egberts Tabaksfab|METHOD FOR DECAFFINING GREEN COFFEE BEANS WITH ACTIVE COBOL.| WO1987004598A1|1986-02-06|1987-08-13|Code Kaffee-Handelsgesellschaft Mbh|Coffee and process for its production| CA1301754C|1986-05-30|1992-05-26|Louris Kaper|Process for recovering caffeine absorbed in activated carbon, and a process for decaffeinating coffee| US4939518A|1987-09-24|1990-07-03|Hitachi, Ltd.|Analog to digital converter| DE3736322A1|1987-10-27|1989-05-11|Jacobs Suchard Gmbh|METHOD FOR CAREFULLY DECAFFINATING RAW COFFEE| DE3806372C2|1988-02-24|1990-02-01|Code Kaffee-Handelsgesellschaft Mbh, 2000 Hamburg, De| JPH0775593B2|1988-06-13|1995-08-16|松下電器産業株式会社|coffee maker| DE4019559C2|1989-10-13|1992-08-27|Mannesmann Ag, 4000 Duesseldorf, De| US5021253A|1989-12-13|1991-06-04|The Dow Chemical Company|Decaffeination of liquid medium| DE4010826A1|1990-04-04|1991-10-17|Jacobs Suchard Ag|Decaffeinating process, esp. for liq. raw coffee extract| AU2003275679A1|2002-10-28|2004-05-13|Kao Corporation|Method of removing caffeine from caffeine-containing catechin compound composition| JP4181863B2|2002-11-29|2008-11-19|花王株式会社|Caffeine-containing catechin composition decaffeination method| US8680301B2|2004-02-17|2014-03-25|Suntory Holdings Limited|Lipase activity inhibitors containing high-molecular weight polyphenol fractions, tea extracts, and processes for producing the same| US7799553B2|2004-06-01|2010-09-21|The Regents Of The University Of California|Microfabricated integrated DNA analysis system| JP4842680B2|2006-03-28|2011-12-21|花王株式会社|Method for producing chlorogenic acid-containing material| CN105658074A|2013-10-21|2016-06-08|德穆斯股份公司|Process for removing caffeine from green coffee and plant for implementing the process| GB201405488D0|2014-03-26|2014-05-07|Infre S A|Decaffeination methods and systems|
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申请号 | 申请日 | 专利标题 US06/153,904|US4495210A|1980-05-28|1980-05-28|Caffeine adsorption| 相关专利
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