• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The method relates to the food industry, in particular decaffeinated tea. The goal is to reduce energy costs. The method of decaffeinating tea involves extracting from 15 to 50 wt.% Water from tea with moist carbon dioxide at a pressure of 255-350 bar and a temperature of 50 to 80 ° C, the subsequent separation of caffeine from carbon dioxide using an adsorbent and recycling of the caffeine-free carbon dioxide through already extracted tea. The method consists in that an adsorbent, in particular activated carbon, is dispersed in an amount of from 5 to 40% in the extraction material, calculated on the weight of dry tea. At the same time, it is possible to mix activated carbon with tea, use activated carbon with a grain size from 0.1 to 10 mm, separate tea from activated carbon in a cyclone or on a sieve, or by air separation, or by electrofiltration, and also conduct extraction 1-4 hours. In addition, carbon dioxide can be taken in an amount of 0.1-3 kg per 1 g of extractable caffeine. 5 hp f-ly.
    公开号:SU1523042A3
    申请号:SU864027377
    申请日:1986-04-30
    公开日:1989-11-15
    发明作者:Клима Хубертус；Шютц Эрвин；Фолльбрехт З.Хайнц-Рюдигер
    申请人:Скв Тростберг, Аг (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to a process for the purification of tea using supercritical gas, in particular carbon dioxide.
    The aim of the invention is to reduce energy costs.
    The method consists in that the adsorbent, in particular activated carbon, is dispersed in the extraction material in an amount of 5-40% by weight, calculated on the weight of dry tea.
    It is established that using this method, the extraction time to
    a certain degree of decaffeination can be significantly reduced, respectively, the amount of carbon dioxide used can be significantly reduced. In addition, the tea obtained by the proposed method is almost the same in taste and aroma as tea, in which case the extraction of caffeine and the separation of caffeine with help. The adsorbent is produced separately. When using the adsorbent in an amount of less than 5 wt.%, Coffee adsorption cm
    Yin in the adsorbent is insufficient, and the extracted tea as a result of this is characterized by an undesirably high final caffeine content. The use of an adsorbent in an amount of more than 40 is economically disadvantageous. Since in this case only slightly higher is achieved: degree of adsorption, on the other hand, an excess amount of adsorbent is a ballast material that takes place in an extraction autoclave.
    Activated carbon is preferably used as an adsorbent, however, other adsorbing agents, such as ion exchangers, kieselguhr, zeolites, or activated alumina, can also be used.
    Uniform dispersion of the adsorbent in the extraction material can be produced in various ways. For example, before loading into an autoclave, tea is mixed with an adsorbent until a homogeneous mixture is obtained, and conventional technical devices can be used for this purpose. In addition, it is possible to fill the autoclave with layers, in which case the autoclave is alternately charged with tea and an adsorbent. In both embodiments of the process, it is advantageous that the carbon dioxide current, before leaving the autoclave, passes through the loading of the pure adsorbent once more, with the result that the remaining caffeine is removed from the gas stream.
    In these embodiments of the method after extraction, the adsorbent must be separated from the decaffected tea. This operation can be carried out using such conventional separation methods as cyclone separation, air separation, sieve separation or electrofiltration. In order to achieve an optimal separation, it is most preferable that the grain size of the adsorbent is significantly different from the particle size of the tea. This position is usually observed when the adsorbent grains have a relatively large diameter. On the other hand, as the particle size increases, the specific surface area decreases, which is negative.
    0
    is related to adsorption activity. Therefore, preferably the average grain size should be 0.1-10 mm. In order to facilitate the subsequent separation of the adsorbent, it is also possible to limit the particles of the adsorbent to such materials that cannot prevent the transfer of carbon dioxide current, but prevent the adsorbent from entering the extraction space.
    The adsorbent can be placed, for example, in a container that can be flushed with carbon dioxide through a suitable sieve or hole. This capacity may be. rigidly fixed in an autoclave and, using an appropriate device, can be filled before and after extraction, respectively, emptied, or when filled with an autoclave, such containers can be dug evenly distributed in the packed material.
    In accordance with another embodiment of the process, the adsorbent is enclosed in a textile material. The adsorbent is placed in bags, bags or sleeves, which are then evenly distributed inside the extraction material or arranged in layers therein. It is necessary that the size of the holes of the fabric be large enough for unhindered entry and exit of the current of carbon dioxide, yo be less than the diameter of the particles of the adsorbent and prevent the exit of these particles.
    0
    Another embodiment of the construction is that the adsorbent is surrounded by a porous inorganic carrier, for example, porous clay or POROUS; graphite, which makes it possible for gas to come in contact with activated carbon, but prevents it from contacting activated carbon. The method can be applied both with axial and radial passage of supercritical gas in an autoclave. In this case, it is necessary that the containers filled with the adsorbent should be optimally located in the loaded material,
    5 In the process of decaffeinating tea, it is sufficient to extract within 1-4 hours.
    0
    five
    five
    0
    By applying the proposed method, the amount of carbon dioxide can be significantly reduced. Essentially, from 0.1 to 3 kg of carbon dioxide per gram of caffeine removed from tea is used for extraction.
    Using this extraction method, it is possible to organize the decaffeination process much more economically. Due to the short extraction time (1-4 hours) and the use of a relatively small amount of carbon dioxide, significantly higher productivity can be achieved. In addition, the cost of instrumentation is very small, since the extraction and addendum of caffeine can be produced by the device,
    The method is illustrated by the following winners. .
    Example 1. D kg of a conventional mixture of black tea with a caffeine content of 2.9% is mixed with 10% by weight of activated carbon (grain diameter 1–3 mm) 5 after which the mixture is moistened with 40% by weight of water. Then, the mixture is loaded into a cylindrical extraction autoclave and immediately after this, extraction is carried out for 2-h with moist synthetic carbon dioxide at 260 bar and 63 ° C (flow rate of gaseous carbon dioxide 200 kg / h). After the tea is separated from the activated carbon by air separation, the tea is dried. The caffeine content in tea is 05.48% 51, which corresponds to an extraction degree of 83.5%.
    Example 2-8 kg of the same tea blend is mixed with 25 of the same grains of activated carbon, after which the mixture is moistened with 40% by weight of water. Extraction is carried out by analogy with that described in Example 1, however, carbon dioxide consumption is halved and extraction time is 1 hour. After separating the mixture and drying tea, the caffeine content in tea is 0.21% (extraction degree 92.8 %).
    Thus, by increasing the amount of activated carbon by half, the extraction time can be reduced while obtaining the best result, and
    her
    s

    ten
    15
    20
    25
    5230426
    at the same time, the specific consumption of carbon dioxide is reduced by 1/8 (calculated on the weight of tea).
    Example 3. A standard mixture of black tea under the conditions of Example 1 is moistened, mixed with activated charcoal and extracted. The tea is separated from the activated carbon by air separation. The mixture is loaded into a cylindrical glass tube and air is blown from below. The air flow is controlled so that the tea is carried out of the glass tube and precipitated in the cyclone, and the activated bead pops up no higher than half the glass tube. After separation, the tea is free of activated carbon as well. The content of particles in the activated carbon as a result of sorting is 8%.
    Example 4. A standard mixture of black tea with a caffeine content of 3.1% is mixed with 30% fine-grained activated carbon and moistened with 40% water. The mixture is loaded into a loading box with a perforated wall. In the middle of the loading box, a vertical perforated tube, additionally sheathed with a sieve cloth, is installed so that its upper end can be connected to the sleeve with the gas outlet of the extraction vessel. During extraction, carbon dioxide under a pressure of 30 MPa: and at 60 ° C passes out through the mixture of tea with activated carbon and leaves it through a centrally installed tube. Extraction is stopped after 1.5 h. The mixture is dried and the activated carbon is sieved through a sieve with a cell diameter of 0.8 mm. The tea contains 0.29% caffeine and is free from activated carbon, and the activated carbon contains 13% of fine fractions, which are by air separation method.
    Example 5-6 kg of a standard mixture of black tea with a caffeine content of 2.9% is moistened with 40% water and divided into three equal portions. Three times 700 g of granular charcoal is loaded into a bag of filter cloth and six fractions starting, loaded into a loading box, and the bags with activated carbon are placed tightly against the wall. Filled with 30
    35
    40
    45
    50
    55
    but the loading box is placed in an autoclave and extracted for 2j5 h with carbon dioxide at 28 MPa and 65 ° С (consumption of CO 200 kg / h) ,.
    The carbon dioxide gas passing through the autoclave passes through a separation stage, in which, after the test, there is 4.2 g of caffeine, i.e.
    2.6%
    in terms of
    extracted amount of caffeine “After the experiment, the layers of tea are mixed and dried. The caffeine content is 0.17%,
    An example of a bobkg standard black tea mixture with a caffeine content of 2.9% is moistened with 40% water and divided into three equal portions. Three times 700 grams of crushed activated carbon are poured into a bag of filter cloth HJ starting from six lobes, loaded with tea into the loading box5, and bags containing activated carbon must lie against the walls. - The loaded loading box is placed in an autoclave and using CO at 280 bar and 65 ° C, extraction is carried out for 2.5 hours (CO consumption 200 kg / h). CO entering from the autoclave is directed through a precipitating cascade S in which, after the experiment, caffeine was detected in an amount of 4.2 g, i.e. 25.6% based on the amount of caffeine extracted. The layers of tea after the experiment are cleaned and you | are narrowed down. The caffeine content is 0517%.
    Example 7. The process is carried out analogously to example 5, but 1.1 kg of activated carbon is placed in the uppermost bag. The results for tea are almost identical, while 0.8 kg of caffeine was found in the precipitating cascade, that is, 0.5% in terms of caffeine extracted.
    Example 8 A mixture of activated carbon and tea is dried and sieved through a sieve with cells of 0.25 mm. The separated activated carbon contains about 10% of the fine fractions of tea, and the tea is practically free from impurities.
    Example 9. A mixture of balls
    ten
    15
    20
    25
    thirty
    35
    40
    45
    50
    The mixture of tea and activated carbon in accordance with Example 1. After extraction with help, the air flow is directed through two cyclones of various sizes connected in series. Since the particle density is not the same, almost exclusively tea is separated in one cyclone, and in the other cyclone, activated carbon with a content of ca 4.7% is released from the mainstream.
    Example P. Separation of tea and activated carbon with an electrostatic precipitator.
    The mixture of tea and activated carbon in accordance with example D after extraction and suge is directed with using an upward flow of air through an electrostatic precipitator. After a surge voltage of 6 kV / cm between the discharge electrode and the precipitating electrode, the tea is completely retained on the precipitation electrode and can be diverted downwards periodically and the activated carbon is directed by air flow through an electrostatic precipitator and then separated from the air in the cyclone.
    Example 12 7 kg of a conventional mixture of black tea with a caffeine content of 2.9% is mixed with 40% by weight of activated carbon (grain diameter 1-3 mm) and moistened with 40% weight by weight of water. The mixture is placed in a cylindrical extrusion autoclave and immediately after that extracted. wet supercritical CO at 28 MPa and 60 C for 3 h with a total of 25 kg COg. (throughput of COg. 8.33 kg / h), and CO gas, continuously flows from bottom to top in the axial direction and continuously. It is fed into the cycle, so that it is recycled through the already extracted tea. At the end of the extraction, the extraction tank is emptied and the extracted tea is separated by winding from activated carbon and dried immediately after that. The content of cofglin and tea is separated by vibration. -55 Hi-ia in tea is 0.08%. what. corresponds to the degree of extraction of 97.2%,
    COg gas consumption. 0.13 kg / g extracted caffeine.
    .on sieve with cells of 5 mm in size and then dried.
    0
    five
    0
    five
    0
    five
    0
    45
    50
    Example 10, Separation of tea and activated carbon using a cyclone.
    The mixture of tea and activated carbon in accordance with Example 1. After extraction with help, the air flow is directed through two cyclones of various sizes connected in series. Since the particle density is not the same, almost exclusively tea is separated in one cyclone, and in the other cyclone, activated carbon with a content of ca 4.7% is released from the mainstream.
    Example P. Separation of tea and activated carbon with an electrostatic precipitator.
    The mixture of tea and activated carbon in accordance with example D after extraction and suge is directed with using an upward flow of air through an electrostatic precipitator. After a surge voltage of 6 kV / cm between the discharge electrode and the precipitating electrode, the tea is completely retained on the precipitation electrode and can be diverted downwards periodically and the activated carbon is directed by air flow through an electrostatic precipitator and then separated from the air in the cyclone.
    Example 12 7 kg of a conventional mixture of black tea with a caffeine content of 2.9% is mixed with 40% by weight of activated carbon (grain diameter 1-3 mm) and moistened with 40% weight by weight of water. The mixture is placed in a cylindrical extrusion autoclave and immediately after that extracted. wet supercritical CO at 28 MPa and 60 C for 3 h with a total of 25 kg COg. (throughput of COg. 8.33 kg / h), and CO gas, continuously flows from bottom to top in the axial direction and continuously. It is fed into the cycle, so that it is recycled through the already extracted tea. At the end of the extraction, the extraction tank is emptied and the extracted tea is separated by winding from activated carbon and dried immediately after that. The coffee content is 55 Hi-ia in tea is 0.08% ,. what. corresponds to the degree of extraction of 97.2%,
    Example 13. 7 kg of the usual mixture of black tea with a caffeine content of 2.9% is mixed with 40% by weight of activated tea. coal (grain diameter 1-3 mm) and moistened with 40 wt.% water.
    The mixture was filled with a cylindrical extraction autoclave in accordance with Example 12 and then continuously extracted with moist supercritical CO at 28 MPa and for 3 hours (total of 560 CO, throughput of CO gas 186.7 kg / h) This gaseous CO continuously passes extraction capacity from the bottom up (the flow of gas in the axial direction). Carbon dioxide during extraction is continuously fed into the cycle, so that it passes through recycled tea through recycled tea. At the end of the extraction and separation of the extracted tea, the activated carbon is separated from the tea by spinning. The caffeine content in tea is 0.06%, which corresponds to an extraction degree of 97.9%.
    The amount of CO gas is thus 2.82 kg / g. extracted caffeine.
    权利要求:
    Claims (6)
    [1]
    1. A method for decaffeinating tea involving the extraction of a moisturizing tea containing 15 ... 50 wt.%
    ,
    Q 5. 0 5
    0
    five
    water, carbon dioxide at a pressure of 25.5-35 MPa and a temperature of 50 ... 80 ° C, the separation of caffeine from carbon dioxide by means of activated carbon and the recirculation of caffeine-free carbon dioxide through the already extracted tea, characterized in that In order to reduce energy costs, before extraction, activated carbon is introduced into the mass of tea in an amount of 5 ... 40% based on the weight of dry tea, and after extraction, tea is separated from the activated carbon.
    [2]
    2. The method according to claim 1, characterized by the fact that activated carbon is mixed with tea,
    [3]
    3. The method according to claim 1, about tl to h..a - y i and with the fact that activated carbon is taken with a grain size of 0.1 ...
    10 mm.
    [4]
    4. Method of pop, 1, characterized in that the separation of tea from activated carbon is carried out in a cyclone, either on a sieve, or by air separation, or by electrofiltering.
    [5]
    5. The method according to claim 1, characterized in that the extraction is carried out for 1-4 hours.
    [6]
    6. The method according to p. I, characterized in that carbon dioxide is taken in an amount of 0.1-3 kg per
    1 g of extractable caffeine.
    类似技术:
    公开号 | 公开日 | 专利标题
    SU1523042A3|1989-11-15|Method of decaffeinating tea
    US4247570A|1981-01-27|Process for the decaffeination of coffee
    US4006066A|1977-02-01|Method of and apparatus for the treatment of exhaust-gases in the electrolytic production of aluminum
    CA1052291A|1979-04-10|Method and apparatus for the purification of waste gas containing gaseous pollutants
    US1825707A|1931-10-06|Method of adsorbing a gas in a solid adsorbent
    US3907971A|1975-09-23|Method of removing HF from gases
    US3879569A|1975-04-22|Process for the decaffeination of raw coffee
    KR960007092B1|1996-05-27|Method for decaffeinated coffee with a supercritical fluid
    US1997125A|1935-04-09|Separation of foreign bodies from powdered materials
    US4259094A|1981-03-31|Apparatus for continuous recovery of solvent
    US2780310A|1957-02-05|Purification of gases with shaped purifying materials
    US4065271A|1977-12-27|Process of separating hydrogen fluoride from gases
    US5199185A|1993-04-06|Process and equipment for gaseous desiccation of organic particles
    CZ278777B6|1994-06-15|Process for removing particles of bentonite and particles containing carbonaceous compounds from dust, obtained when recovering return sand by mechanical way
    US3527026A|1970-09-08|Apparatus for treating a gas to remove impurities therefrom
    US2106869A|1938-02-01|Drier for granular and like materials
    SU1602385A3|1990-10-23|Method and installation for decaffeinization
    US3910849A|1975-10-07|Method for manufacture of activated carbon and apparatus therefor
    US4201695A|1980-05-06|Arrangement for regenerating particulate adsorbents
    US3216843A|1965-11-09|Treatment of carbon black
    US4061477A|1977-12-06|Method and apparatus for the purification of waste gas containing gaseous pollutants
    US3823487A|1974-07-16|Method for drying moisture from wet spent coffee grounds
    US4745096A|1988-05-17|Bagasse residue filter materials and activated carbon products and methods of manufacturing the same
    US2206337A|1940-07-02|Method of decolorizing liquids
    RU2062951C1|1996-06-27|Method of processing coal to powder and apparatus for performing the same
    同族专利:
    公开号 | 公开日
    CN86103112A|1986-10-29|
    IN164998B|1989-07-22|
    DE3667900D1|1990-02-08|
    CN1008507B|1990-06-27|
    JPH0736743B2|1995-04-26|
    CA1279221C|1991-01-22|
    EP0200150A3|1988-01-20|
    EP0200150B1|1990-01-03|
    AT49104T|1990-01-15|
    DE3515740A1|1986-11-06|
    US4976979A|1990-12-11|
    DE3515740C2|1993-07-29|
    JPS61254144A|1986-11-11|
    EP0200150A2|1986-11-05|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2198859A|1938-05-18|1940-04-30|Max Brunner & Co|Process for decaffeinating coffee|
    DE2127642C3|1971-06-03|1975-10-16|Studiengesellschaft Kohle Mbh, 4330 Muelheim|Process for making caffeine-free, full-flavored black tea|
    US4247570A|1976-08-04|1981-01-27|Studiengesellschaft Kohle Mbh|Process for the decaffeination of coffee|
    DE2637197C2|1976-08-18|1983-01-27|Hag Ag, 2800 Bremen|Process for the removal of caffeine from natural substances containing caffeine with a supercritical extractant|
    NL7712503A|1977-11-14|1979-05-16|D E J Int Research|PROCEDURE FOR DECAFFINING GREEN COFFEE BEANS.|
    DE3339181A1|1983-10-28|1985-05-09|Uhde Gmbh, 4600 Dortmund|METHOD AND DEVICE FOR DECAFFINATING TEA LEAVES|
    DE3413869C2|1984-04-12|1989-08-31|Hopfenextraktion Hvg Barth, Raiser & Co, 8069 Wolnzach, De|
    DE3415844C2|1984-04-27|1994-02-03|Sueddeutsche Kalkstickstoff|Process for the production of decaffeinated tea|DE3838952C2|1988-11-17|1993-08-19|Hopfenextraktion Hvg Barth, Raiser & Co, 8069 Wolnzach, De|
    US5151188A|1990-06-12|1992-09-29|The Government Of The United States Of America, As Represented By The Secretary Of The Department Of Health And Human Services|Supercritical fluid extraction enhancer|
    JPH08225793A|1994-12-22|1996-09-03|Showa Shell Sekiyu Kk|Lubricating additive and lubricating grease composition containing the same|
    US5614096A|1995-05-24|1997-03-25|Kimberly-Clark Corporation|Compressed adsorbent filter cake|
    JPH11505716A|1995-05-24|1999-05-25|キンバリークラークワールドワイドインコーポレイテッド|Filter with absorbent clay minerals attached to individual exposed surfaces of fiber matrix|
    US5906743A|1995-05-24|1999-05-25|Kimberly Clark Worldwide, Inc.|Filter with zeolitic adsorbent attached to individual exposed surfaces of an electret-treated fibrous matrix|
    US5603830A|1995-05-24|1997-02-18|Kimberly-Clark Corporation|Caffeine adsorbent liquid filter with integrated adsorbent|
    USD383036S|1995-11-16|1997-09-02|Kimberly-Clark Corporation|Filter cake holder|
    US6063428A|1996-02-26|2000-05-16|The Procter & Gamble Company|Green tea extract subjected to cation exchange treatment and nanofiltration to improve clarity and color|
    CN1072446C|1996-05-24|2001-10-10|王振锟|Overcritical multiple fluid tea-processing method and product thereof|
    CN1044616C|1996-06-28|1999-08-11|中国石油化工总公司|Coupled succimide lubricant additive|
    EP2253223A1|2003-12-02|2010-11-24|Kao Corporation|Package drink|
    CA2572995C|2004-07-09|2010-12-07|Nateco2 Gmbh + Co. Kg|Method for decaffeinating tea|
    CN100387591C|2004-08-26|2008-05-14|上海交通大学|Removal of caffeine from polyhydric phenol by supercritical carbon dioxide process|
    ES2366039T3|2004-10-28|2011-10-14|Japan Tobacco, Inc.|METHOD FOR REMOVING A COMPONENT OF MATERIAL TO BE PROCESSED AND DEVICE USED IN THE METHOD.|
    DE102011010396A1|2011-02-04|2012-08-09|Nateco2 Gmbh & Co. Kg|CO2 extraction method|
    GB201405488D0|2014-03-26|2014-05-07|Infre S A|Decaffeination methods and systems|
    CN104757220B|2015-05-06|2016-05-25|美町宝植物科技有限公司|Decaffeination production technology of oolong|
    EP3120712B1|2015-07-22|2017-09-13|Evonik Degussa GmbH|Method for improved extraction of juniper berries, rose hips, sea buckthorn berries, sorbus|
    EP3165099A1|2015-11-03|2017-05-10|Evonik Degussa GmbH|Removing oil and simultaneous removal of unwanted contaminants from beans with supercritical co2|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE3515740A|DE3515740C2|1985-05-02|1985-05-02|
    [返回顶部]