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  • 专利说明
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    • 专利摘要:
    1535472 Solubilising tea tannins SOC DES PRODUITS NESTLE SA 28 Feb 1977 [17 March 1976] 08378/77 Heading A2B [Also in Division C2] Cold water-soluble tea tannins are made by chilling a hot water extract of tea leaves, e.g. to 0-15‹C, to precipitate tannins, dispersing the separated precipitate in an aqueous medium and contacting with oxygen and an oxidation catalyst, e.g. MnO 2 , Co 3 O 4 , CuO, V 2 O 5 , CuCO 3 , NiO, Cr 2 O 3 , Ag to effect oxidative solubilisation. The oxidation may take place at 5-50 kg/cm<SP>2</SP> O 2 , partial pressure and 80-110‹C, the initial and final pH being 4.5-9.0 and 3.0-4.0 respectively. The catalyst may be supported and may be promoted. Acids may be removed or neutralised by adding absorbent or alkali during reaction. The initial extract may be steam stripped to remove volatiles and the final product may be decolourised by bleaching or by contacting with a tea extract containing unoxidised tannins.
    公开号:SU1048978A3
    申请号:SU772461324
    申请日:1977-03-16
    公开日:1983-10-15
    发明作者:Амод Хосейн Сид
    申请人:Сосьете Де Продюи Нестле С.А (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to a method for producing water soluble tannins tea.  In aqueous extracts, tea is contained in substances with different extensibility.  - One part of the extracted solids dissolves easily in hot and cold water.  The remaining part, tannins, is soluble in hot water, but does not substantially dissolve in holnd water, This tannin part does not create difficulties in preparing a hot drink, but cold tea and iced tea containing these natural tannins, lower quality due to precipitation and turbidity due to the limited solubility of said tannins.  Moreover, in the presence of these natural tannins, the ease and completeness of diluting water with dehydrated tea leaves is difficult.  To eliminate these drawbacks, the tannin portion is removed.  The rest is dissolved in cold water. may be consumed or, for example, concentrated and dried to obtain a powder.  In the practical implementation of this method, the insoluble part is discarded, which leads to a large loss of the usual aromatic component of tea.  One of the known ways to avoid such losses is.  that the insoluble in cold water tannin part of the aqueous extract of tea is separated when the extract is cooled to precipitate.  This precipitate of tannins is oxidized to a highly basic.  medium sufficient to improve its solubility. The tannin portion is then acidified to a normal pH, if necessary, combined with another portion of the original extract 1.  When tannin is made soluble in cold water according to this method, the tannin part is exposed to a highly basic oxidation medium.  In order for this reaction to proceed satisfactorily to the medium, significant amounts of alkali or other base must be added (this medium is usually acidic as a result of tannin content).  Such an added alkali is difficult to separate from the oxidized tan ov and sweat may remain as an impurity in the resulting tea product.  In addition, during acidification of the medium, often necessary after an oxidation reaction, the concentration of impurities in the prepared beverage may increase.  The closest to the proposed technical essence and the achieved result is a method of obtaining water soluble tannins, which involves cooling the aqueous extract of tea leaves, separating precipitated tannins, adding water to. the resulting dispersion, oxidation of tannins with oxygen under pressure at 80-110 ° C and separation of tannins 2.  Oxidation of tannins is a catalytic reaction produced by the bases, and acidic substances are formed during the oxidation process, which prevent the tannins from becoming soluble in cold water.  This problem is solved by adding alkali at the beginning of the reaction, which, however, creates two drawbacks: foreign material is mixed with tea. , after oxidation, the pH decreases to normal for dl.  .  cha  . A decrease in pH can be made by adding food acid, or by electrodialysis, or by ion exchange.  All three options require additional technological operations.    The aim of the invention is to improve the quality of the finished product by eliminating impurities while simplifying the process.  This goal is achieved due to the fact that according to the method of obtaining water soluble tannins, which involves cooling an aqueous extract of tea leaves, separating precipitated tannins, adding water to the resulting dispersion, oxidizing tannins with oxygen under pressure at a temperature of 80-110 ° C, separating the solution of oxidized tannins , the oxidation is carried out in the presence of MnO or, or Ag, or, or SiCO, as a catalyst, maintaining the pH of the environment 4.5-6.0, by neutralizing or removing the acid formed by the absorbent.  Oxidation of tannins according to invented. with known oxidation catalysts, such as MnO2, ViOg. , CuCOj, Ag allows to increase the reaction rate and yield, and this increase is most significant under relatively mild conditions, which are preferably used.  When dispersing raw tannins in water, a medium is usually obtained having a pH of 4.8-5.0.  Such a natural value j) H is suitable for imparting solubility by the catalytic oxidation method provided by the present invention.  If the pH of the medium is in the acidic region, then the yield of dissolved tannins may decrease.  Therefore, a pH of less than about 4.5 is undesirable.  When a less acidic environment is established at the stage of imparting solubility, a greater yield of dissolved annin is obtained.  However, to increase the pH of the medium, it is necessary to add an alkali, such as sodium or potassium hydroxide, which is undesirable.  Therefore, usually the pH is maintained in the range of about 4.5-6.0.  AT. as a result of an oxidative reaction, accompanied by a conversion of from about 10 to 15 weight. The% of tannins, in carbon dioxide, significantly increases the solubility of these tannins in cold water.  In addition, this is achieved without degrading their important properties necessary for obtaining good drinks.  Depending on the extraction method used, the extract obtained in hot water usually contains about li-1O weight. % solid substances To simplify the process, you can select a standard concentration of hot tea extract.  Typically, 5-15 or, preferably, about 8 wt. % solids.  These tea extracts also contain important aromatic components that are sensitive to reaction or loss during processing.  It is advantageous to minimize the impact on them of adverse conditions.  Components, usually referred to as volatile, are often temporarily separated to prevent their loss.  Even before standardization of the concentration of tea extract, it is desirable to isolate these components, for example, by steaming from the extract at a temperature of about 80-120 C.  The vapor containing the volatile components is collected, condensed and cooled to obtain the isolated important apo.  Mathematical substances.  They can be later.  use to obtain an aromatic beverage from a treated extract.  The removal of the insoluble in the cold water portion of the tannins is also easily performed.  This portion, tannins, is about 15-35% p. total number of twp delh. substances.  content in tea is usually precipitated from solution at iCooling to a temperature of about or preferably about.  The subsequent separation of the precipitated tannins from the water should be carried out with a potassium blend containing soluble solids that can be made by any known method, for example, by centrifuging the cooled suspension.  It is advisable to wash the separated precipitate of insoluble components with water: preferably at a temperature of 0-15 ° C or better, approximately 8-10 seconds.  This sediment usually contains about 15-30 weight. % enthusiastic products soluble in cold water.  When washing, the weight of the non-tannin soluble substances in the sediment is reduced and therefore they are not subjected to subsequent oxidation to impart solubility.  Then, the washed isolated substances are dispersed or dissolved in water, and it is very convenient for standardization to standardize the concentration of tannins.  Therefore, it is desirable to use water in an amount sufficient for.  obtain medium containing about 5-15 or preferably about 10 weight. % solids.  ; The amount of oxygen required to impart solubility by the catalytic method is essentially the same as that required for known oxidation processes.  The reaction proceeds completely when using at least 100 liters or preferably approximately 1 liter of oxygen ifa 1 kg of tannins Elh solid vent cTB.  However, it is desirable to use oxygen under pressure for catalytic oxidation.  To accelerate the reaction, it is desirable to apply a partial oxygen pressure of from about 5-60 kg / cm.  As with the known oxidation processes, the temperature influences the rate and extent of the reaction.  Elevated temperatures accelerate the reaction, and therefore preferred temperature is not lower.  At temperatures above: this is achieved an even greater reaction rate. however, temperatures above llOc have an adverse effect.  At such a high temperature, some tannins can be carbonized and polymerized, making them less soluble in water.  Therefore, temperatures in the range of 80-11 ° C are preferred, and temperatures in the range of 100-110 seconds are most preferable.  Minor side effects are observed with some of the catalysts.  For example, some of these catalysts, especially vanadium pentoxide. and silver may cause excessive amounts of acid.  On the other hand, when using cobalt and copper catalysts, a slight metallic or foreign flavor may appear.  manganese oxide is essentially free of such defects and is very active at the same time. .  Therefore, it is the preferred catalyst.  . In accordance with the invention, the catalyst can be applied on an essentially inert base, thereby facilitating the handling of the catalyst.  Such carriers are well known and include materials such as alumina, silica, silicon carbide, and the like. P.  When used in such a form, the active catalyst is usually contained on the butcher in an amount of from 1-10 wt. %  The amount of catalyst also affects the rate of solubility imparted during oxidation.  This occurs even when the reaction mass is stirred during the reaction in order to provide a more frequent contact of the catalyst, oxygen and unoxidized tannin.  Therefore, in order to facilitate the reaction, it is preferable to use an active catalyst in an amount of 0.1-1. weight. % solid tannin substances.  The catalyst in excess rio compared with this amount does not provide significant benefits.  It has been found that during the oxidation reaction, the solubility of oxidized tannin in cold water reaches a maximum, depending on the conditions used.  In all cases. However, at first, under the continuous action of oxidation conditions, the solubility of tannin increases and then gradually decreases.  However, by simply monitoring the medium during the reaction, an optimal oxidation time can be established.  .  Controlling is achieved by periodically determining the solubility of aliquot amounts of tannin.  When the maximum solubility is reached, the reaction is prekrgitsayut.  An increase in the yield of solvent tannins is achieved by removing or neutralizing the side acids during solubility during oxidation (oxidium).  Neutralization is most easily achieved by adding aliquots of alkali during the reaction.  In this way, during the reaction, the desired pH can be maintained in the range 4.5-5.5.  However, the acids formed during solubility are preferably removed by sorbents and similar agents.  For example, the medium may be contacted with an acid scavenger such as an anion exchange resin.  Such a contact.  This can be done, for example, by placing the absorbent in the reaction chamber together with the Catalyst or with continuous circulation of the tannin medium between the two chambers — the reaction chamber containing the catalyst and the second chamber,. containing absorbent.  Absorbent;  it holds the pH at acid removal and makes it possible to achieve a greater degree of solubility.  After the termination of the tannin reaction, the medium is easily separated and remains unchanged.  An increase in catalytic oxidation efficiency can be achieved by introducing a promoter into the medium during the reaction.  For example, sulfur dioxide (usually in the form of dilute sulfuric acid, lots) can be added to the medium.  Such a sulfite promoter acting upon catalytic oxidation increases the yield and rate of the solubility imparting reaction.  However, usually in the practical implementation of this image. such promoters are not applicable because of the added costs and difficulties associated with their use.  In addition, since the promoters may remain in the resulting product, it is preferable to accelerate the reaction by other methods described above.  In the implementation of the proposed method, catalytic oxidation to impart solubility is usually achieved periodically.  However, a continuous or semi-continuous process can be used, for example, in a suitable packed column in the presence of a catalyst.  The selection of the most advantageous oxidation method depends largely on the amount of tannin treated for solubility and is easily determined by one skilled in the art.  Oxidized tannins are preferably freshly extracted from tea.  After extraction, tannins tend to degrade and lose their ability to become soluble.  However, they can be stabilized.  For example, if production conditions require extracting raw tannins for more than 24 hours, they can be dehydrated, for example, when drying at temperatures below zero.  Although dehydration reduces the weight of soluble tannin, however, large losses are eliminated due to; degradation.  Tannin environment, it is desirable to mix during the reaction.  Stirring is achieved by well-known mechanical means, as well as by controlling the flow rate.  This mixing provides close contact of the reactants with the catalysts, and therefore reduces the reaction time and providing. em uniformity of dissolution.  After the reaction, dissolved or.  oxide tannins have a slightly darker color. than natural non-oxidized tannins.  Therefore, prior to the introduction of these oxidized tannins 9, products suitable for use as a type of beverage are clarified by known methods.  This treatment provides the color and type of drinks containing soluble tannins, which are customary drinks. However, an aqueous extract is preferred. . use simultaneously to discolor oxidized tannins | chow and to combine them with commonly added nontany solids contained in tea.  By combining tea extract (containing unoxidized tannins with oxidized tannins, the last tannins become discolored.  Then, when cooled, non-oxidized tannins can be precipitated, in this way they can be removed (for separate processing, preferably for solubility) and at the same time to obtain a new extract of a normal composition, but containing tannins, made soluble by oxidation.  : After combining the oxidized tannins with other, usually completely soluble solids, the resulting extract can be subjected to a subsequent conventional treatment.  For example, it can be concentrated, reconstituted with previously isolated volatiles, and dried to form a soluble dry Chosh.  In this way, tea products are obtained, possessing properties and characteristics that are essentially identical to the properties of natural tea (with the exception of the desired solubility in cold water, achieved in accordance with this invention).  . In these examples, the yield or percentage of solubility is expressed by the weight ratio of solids, soluble in cold water after oxidation, to the initial solids in the reaction. environment.  Example 1.  From 2 l of 4% aqueous tea extract, volatile components are removed by distillation with 4 wt. %  couple at.  The volatile components are condensed, cooled, and a stable isolated product is obtained, and subsequently, 1 &amp; 1 amp is added to the finished tea producti. Then the extract is evaporated in Vacuum to a solid content of 10 wt. %  The concentrated extract of the ohla give up and centrifuged.  In this way, 24 g of raw solid tannins are recovered from the extract.  These tannins are dispersed in 400 g of water, the resulting dispersion has a pH of 4.95.  The tannins dispersion is loaded into a 2-liter reactor operating under pressure and equipped with an electric heating breaker, an agitator and an outlet for gases.  5.5 g of manganese dioxide on silicon carbide as a carrier are also placed in the apparatus (the total weight of the active manganese dioxide is 0.25 g).  In the apparatus create a partial pressure of oxygen.  10 kg / cm at.  .  These conditions and a stirring rate of 500 rpm are maintained for 15 minutes to impart solubility.  Then the tannin solution is removed from the apparatus and cooled to.  Small precipitation is observed at this temperature. the amount of solids.  . (The separated extract solution contains approximately 74% of the original tannins.  The solution is a darkish color and has a pH of 4.5.  .  This solution of oxidized tannins is added to 2 liters of 4% tea extract - (after removing the volatile and containing. raw tannins). The mixture is stirred for 20 minutes at 70 ° C and the solution is clarified before coloring, which is characteristic of non-oxidized tannins.  After cooling to 10 ° C and.  Centrifugation gives 24 g of solid, non-oxidized tannins.  The supernatant of the tea extract, containing oxidized cold-water soluble tannins, is evaporated in vacuo to a solids content of about 45%.  Previously separated volatile substances are added to this very concentrated extract and the resulting solution is spray dried to obtain soluble tea.  The color to appearance of this product does not differ from the color and type of industrial product.  After being added, to cold water to make tea with ice, the product dissolves easily and gives a clear, sparkling solution.  The color and taste of this drink do not differ much from the color and taste of ordinary tea products.  Example 2  50 g of raw tannins, dried at a temperature below zero, are dispersed in 1 liter of zod, as described in example 1.  In catalytic oxidation, the conditions are used in this case and the results are shown in  one.
    Table
    Example 3. Copper carbonate / supported on silica (6% active catalyst) is used to impart a solubility to several portions of 50 g of dried tannins dispersed in 1 l of water at a temperature below zero.
    The method described in example .1 ;; catalytic oxidation is carried out using 10 g of a nasal catalyst;
    As a result of the use of promotoir, the solubility of tannins increases over the short period of the reaction.
    PR w mep 4. 50 g of raw tannip feoB, dried at a temperature below zero, dispersed in 1 l of water, as described in example 1, using
    ..........
    Konechna Pressure is sour. .PH of the genus, kg / cm
    4.9
    13
    5.5
    tele. To compare the effectiveness of solubility, two experiments were carried out, only in one of which tannin was introduced on Wednesday 25 before oxidation
    1, sulfur dioxide as a promoter (added as an aqueous sulfuric acid).
    30 The results obtained are presented in Table. 2
     table 2
    3 g of manganese dioxide on the carrier as katsshizator. In the reaction apparatus placed 100 ml of a weak ion exchange resin in hydroxyl form (Amberlite).
    The results of the catalytic oxide 55 Lenin are presented in Table. 3. T a b i c a 3
    g1 Time min I
    Temperature, Time, min. Strength,
    with I I%
    100
    120
    79
    When the medium is cooled until after the reaction, no precipitates of substances insoluble in cold water occur. All-dissolved tannins are soluble in cold water. The weight reduction is due to the formation of carbon dioxide removed and acids absorbed by the resin. .
    Example 5. 50 g of tannins are dispersed in 1000 ml of water in a Parr Jd autoclave equipped with an oxygen inlet, an exhaust pipe, a stirrer and a sample opening during the reaction. The initial pH value is 4.8. The catalyst (10 g, 35% cobalt oxide on kieselgur) and 60 ml of Amberlite IRA-93 ion exchange resin are added. At speed
    Examples 14, 15. In the same way as described, 2 experiments were carried out at a constant pH using 80 g of tannins in 800 ml of water and 0.5 g. powder without carrier quality-. ve catalyst. The conditions are as follows; temperature 105-112 C / oxygen pressure 8.8 kg / cm, time 25 min. The initial pH value of 4.60, in the first 55
    Schloch
    50.6
    52.5 51.9
    rotation of the stirrer at 600 rpm in an apparatus maintains a partial pressure of oxygen of 1.8 kg / cm and a temperature of lOS-llO C. These conditions are maintained for 25 minutes, and the 5 gas output has a speed of 500 ml / min. After completion of the reaction, the entire contents are cooled to room temperature, the pH value is measured therein, cooled further to and centrifuged at 10,000 rpm for 20 minutes. Determine the weight of the solid phase (soluble tannins) in the liquid above the sediment and calculate the yield. This procedure is repeated 5 in examples 6-13 under the conditions given in table. i. In examples 9-11, Amberlite type resin IRA-400 (100 ml) is used. Examples 5-13 are given in table. 4Table 4
    its experience is supported practically. a constant (final value of 4.5) and in the second, a pH value of 6.0 is maintained by adding a 2N solution of KOH. The yield is 84.0% and 84.5%, respectively.
    In tab. presents the output values of soluble c. water tannins.
    Table 5
    51.3 61.4
    53.2
    58.3 27.5 91.0
    The advantage of the proposed method is that, using a catalyst, no foreign substances alkali or acid are added to tannins, which remain in the final product. At the same time, the pH is not maintained, it is allowed to decrease as a result of the release of acid during oxidation.
    The ion exchange resin may be added (or it may not be added).
    neutralizing a certain amount of acid and for further reaction, i.e. oxidizing as many tannins as possible.
    Under normal conditions, however, without the use of a resin, the reaction is stopped because the pH is inhibited by a decrease in pH. This lower final pH value is nevertheless still quite acceptable for drinking.
    权利要求:
    Claims (1)
    [1]
    , METHOD FOR PRODUCING TEA TANININS SOLUBLE IN WATER OF TEA, which involves cooling the aqueous extract of tea leaves, separating the precipitated tannins, adding water to the resulting dispersion, oxidizing Fannins with oxygen under pressure at a temperature of 80-110 * C and separating the solution of oxidized tannins, Particularly with the fact that, in order to improve the quality of the finished product by eliminating impurities while simplifying the method, the oxidation is carried out in the presence of MORILI, or
    Ag, or Co ^ O ^., Or CuCoj as a catalyst, maintaining the pH of the medium 4.5-6.0 by neutralizing or removing the resulting acid with an absorbent.
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    同族专利:
    公开号 | 公开日
    JPS52145598A|1977-12-03|
    ZA771218B|1978-06-28|
    AR209884Q|1977-05-31|
    FR2344230B1|1983-02-04|
    GB1535472A|1978-12-13|
    CA1082980A|1980-08-05|
    JPS6022895B2|1985-06-04|
    KE3055A|1980-06-27|
    US4156024A|1979-05-22|
    DE2710070A1|1977-09-29|
    NZ183476A|1978-12-18|
    AU509413B2|1980-05-08|
    CH618327A5|1980-07-31|
    AU2328577A|1978-09-21|
    FR2344230A1|1977-10-14|
    DE2710070C2|1987-04-16|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
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    US2831772A|1956-03-22|1958-04-22|Afico Sa|Beverage preparation|
    US3065077A|1960-02-02|1962-11-20|Afico Sa|Method of making a soluble tea product|
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    GB1249932A|1969-07-10|1971-10-13|Tenco Brooke Bond Ltd|Enzymatic solubilisation of tea cream|
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    US3950553A|1974-06-10|1976-04-13|Societe D'assistance Technique Pour Produits Nestle S.A.|Process for preparing a soluble tea product|US4315036A|1978-01-12|1982-02-09|Societe D'assistance Technique Pour Produits Nestle S.A.|Process for decaffeinating tea|
    DE3679714D1|1985-05-08|1991-07-18|Nestle Sa|STABILIZING TEA IN COLD WATER.|
    JPH025596Y2|1986-12-11|1990-02-09|
    AU1525695A|1994-01-10|1995-08-01|Procter & Gamble Company, The|Tea extract and process for preparing|
    AU3142095A|1994-08-08|1996-03-07|Procter & Gamble Company, The|Color stable composition containing tea and fruit juice|
    US5427806A|1994-08-08|1995-06-27|The Procter & Gamble Company|Process for making a stable green tea extract and product|
    AT249148T|1996-06-03|2003-09-15|Unilever Nv|IMPROVEMENTS IN THE PRODUCTION OF SOLUBLE TEA SOLIDS|
    US5827560A|1997-04-14|1998-10-27|Nestec S.A.|Process for producing cold water soluble tea extract|
    CA2245995A1|1997-10-23|1999-04-23|Societe Des Produits Nestle S.A.|Tea bag for iced tea|
    GB9903429D0|1999-02-15|1999-04-07|Unilever Plc|Method for making a cold water soluble tea extract|
    GB0016312D0|2000-07-04|2000-08-23|Zylepsis Ltd|Separation method|
    US6761918B2|2002-07-18|2004-07-13|Tata Tea Ltd.|Method of processing green tea leaves to produce black tea that can be brewed in cold water|
    ITPD20030097A1|2003-05-08|2004-11-09|Enologica Vason Srl|MIXTURE FOR ENOLOGICAL USE OF THE TYPE INCLUDING TANNIN E|
    GB0409846D0|2004-05-04|2004-06-09|Unilever Plc|Tea extracts|
    US20090220668A1|2008-02-29|2009-09-03|Coca-Cola China Beverages Ltd|Clarified tea extract and method of making same|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US66790376A| true| 1976-03-17|1976-03-17|
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