EP1185611A1 - Procede de production d'acide tartrique et d'un concentre de pigments de raisin - Google Patents

Procede de production d'acide tartrique et d'un concentre de pigments de raisin

Info

Publication number
EP1185611A1
EP1185611A1 EP00908140A EP00908140A EP1185611A1 EP 1185611 A1 EP1185611 A1 EP 1185611A1 EP 00908140 A EP00908140 A EP 00908140A EP 00908140 A EP00908140 A EP 00908140A EP 1185611 A1 EP1185611 A1 EP 1185611A1
Authority
EP
European Patent Office
Prior art keywords
tartaric acid
accordance
solution
pigments
resin
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.)
Withdrawn
Application number
EP00908140A
Other languages
German (de)
English (en)
Inventor
Fernando Glenadel Braga
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Subvidouro CRL
Original Assignee
Subvidouro CRL
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Subvidouro CRL filed Critical Subvidouro CRL
Publication of EP1185611A1 publication Critical patent/EP1185611A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12F—RECOVERY OF BY-PRODUCTS OF FERMENTED SOLUTIONS; DENATURED ALCOHOL; PREPARATION THEREOF
    • C12F3/00—Recovery of by-products
    • C12F3/06—Recovery of by-products from beer and wine

Definitions

  • the present invention describes a process for the production of tartaric acid and a concentrate of grape anthocyanin pigments, from winery by-products, by means of an operation of selective adso ⁇ tion of the pigments onto a polymeric adsorbent resin and the use of an ion exchange process using a strong cation resin, contained in a fixed bed, to produce the tartaric acid.
  • tartaric acid can be produced from one or more of the following byproducts:
  • tartaric acid is produced industrially from only two sources, the wine lees and press-filter cakes, in a process involving two main steps: 1) the formation of the calcium tartrate from the potassium bitartrate through the use of diverse calcium compounds (Ca(OH) 2 , CaC0 3 , CaCl 2 , etc.)
  • the tartaric acid thus produced is used as an acidifying agent in drinks (it is the only additive allowed in Europe for the correction of acidity in wines), grape juice, confectionery, jams and various industrialised food products.
  • the first is due to the need of a great excess of the calcium compounds in order to ensure a good recovery of the calcium tartrate, the which generates high volumes of the solution in the final steps of the production of the tartaric acid. This would require an industrial plant calling for the type of financial investment that would not be justifiable unless the availability of winery by-products in the region were to be above one hundred thousand tons per year.
  • tartaric acid and fodder yeast are produced by passing an aqueous suspension of wine sediments through a column containing a fluidised bed of an industrial grade cation exchange resin.
  • the present invention describes a method to produce tartaric acid from winery byproducts such as the wine lees, the press-filter cakes from wine filtration and the precipitate produced after the cooling of the leaching solution of the grape pomace, through the use of an ion exchange process with a gel type strong cation resin (hydrogen form) such as, for example, Amberlite SR1L (Rohm & Haas Co.), contained in a fixed bed, after the removal of anthocyanic pigments through two adso ⁇ tion operations, using an adequate polymeric adsorbent resin as, for example, Duolite XAD761 (Rohm & Haas Co.).
  • a gel type strong cation resin such as, for example, Amberlite SR1L (Rohm & Haas Co.)
  • an adequate polymeric adsorbent resin as, for example, Duolite XAD761 (Rohm & Haas Co.).
  • both the Amberlite SR1L and the Duolite XAD761 do not introduce the possibility of the contamination of the tartaric acid or the pigment concentrate yielded by the process described in the present invention. Such a fact is of special importance for the process, since the use of these two products in the European market is mainly in the wine and food industries.
  • the anthocyanic pigments are removed in order to guarantee that the diluted solution of the potassium bitartrate (KHT) present in the by-products of vinification is transformed into tartaric acid without the reduction of the exchange capacity of the resin bed.
  • the adsorbed pigments are eluted (regeneration of the adsorbent resin) with ethanol and the resultant solution is concentrated, under reduced pressure and a maximum temperature of 40°C.
  • Such anthocyanic pigments are approved additives in the European Union (El 63) and United States of America (Grape Color Extract and Grape Skin Extract) for the coloration of some dairy products, ice-cream, candies, confectionery, tinned vegetables, meat products, soups and non alcoholic beverages.
  • the present invention also concerns the recycling of the used cation exchange regenerant solution.
  • the conductivity of this solution is measured and, in accordance with the graph in Figure 1 , it is possible to control the addition of the exact amount of produced potassium chloride to reduce the solubility of the KHT, by the common ion effect ( Figure 2), in the winery by-product that will be processed in the next cycle.
  • Figure 2 common ion effect
  • Such procedure makes the total recovery of the potassium bitartrate (solid) contained in the winery by-product by filtration possible at room temperature.
  • the remainder of the used regenerant solution is stored in order to be used as the first portion of regenerant solution in the next regeneration cycle of the cation exchange resin.
  • the small amount of hydrochloric acid that comes with the potassium chloride has a beneficial effect on the extraction of the pigments due to the increase in the solubility of the anthocyanins present in the solid sediments of the wine lees and filter cakes, as well as in the diluted wine produced by the leaching of the grape pomace.
  • No harmful effect related to the presence of traces of hydrochloric acid hinders the use of the pigment produced that way, even because almost all the actual processes of extraction use various types of mineral acids, in higher concentrations, with the same objective.
  • the resultant 650 litres of suspension (4) are filtered in a press-filter (5), at room temperature (18 - 20°C), the filtered solution (6) being introduced by means of an adequate pump (7) (flow of 13 litres/min.), in a fixed bed column CA (100 cm high X 30 cm diameter) containing 65 litres of the polymeric adsorbent resin Amberlite XAD761 (Rohm & Haas Co.) in order to remove the existing anthocyanic pigments. After this operation, the discoloured solution (8) is transferred to another tank (9).
  • the cake (10) produced by the above filtration (125 kg), which has about 40% w/w of KHT, is then suspended in 1,500 litres of potable water (11) at 70°C, with the help of mechanical agitation, in a heating jacketed vessel (12), for 15 minutes and, after that, this suspension (13) is fractionated by filtration (14), yielding 1,550 litres of a coloured solution (15) containing 0.17 moles per litre of KHT and 75 kg of a solid composed mainly of grape skins and seed (SS).
  • This coloured solution (15) is then introduced into the column CB by means of the centrifugal pump (16) (13 litres/min.).
  • This column of the same dimensions as the previously cited column CA, contains the same adsorbent resin and the temperature of the solution is maintained between 65°C and 75°C during the operation of adso ⁇ tion by the circulation of warm water or steam inside a coil welded to the exterior of the column CB.
  • the colourless solution (17) eluted from the column CB is pumped (18), while still hot and with a flow of 30 litres/min. into the fixed bed column CC through a piping system that can be closed in a way to make the recirculation of this solution (Re) possible.
  • This column CC (100 cm high X 50 cm diameter) contains 175 litres of the strong cation resin Amberlite SR1L (Rohm & Haas Co.). After 2 hours of operation, the resultant solution (19) is transferred to a crystallizer (20) to be concentrated, at atmospheric pressure (maximum temperature of 60°C), until almost the water has evaporated.
  • the wet crystals of tartaric acid (21) obtained are then dried with the aid of a fluidised bed dryer (22) (maximum temperature of 60°C). Later, tartaric acid (TA) containing a maximum of 0,5% w/w of moisture is packed up (23) (38 kg - 95% of recovery).
  • TA tartaric acid
  • Both the resin that composes the bed of the column CA as that of the column CB are regenerated (24), at room temperature, by passing the ethanol (Et) (94 - 96°) produced by the distillation (25) of the discoloured solution (8).
  • the alcoholic solution (26) obtained is cooled at 5°C during 12 hours, with constant agitation and then filtered (27). Later, in the stage of concentration, the ethanol is recycled (28) at reduced pressure and 40°C, from the alcoholic solution (26) by adding a condenser (29) between the concentrator (30) and an appropriate vacuum pump (31).
  • the cationic resin bed is regenerated (3) through the passing (by gravity) of 2,000 litres of solution (32) of hydrochloric acid 7,3% w/v, with a flow of 15 litres/min., followed by the rinsing of the resin bed with 700 litres of de-ionised water (33).
  • the first 150 litres of the regenerant solution (2) eluted from column CC, are used for adjusting the potassium concentration in the next 500 kg of the wine lees to be processed, so that less than 1% of the potassium bitartrate will remain in the solution.
  • the remaining volume of the regenerant solution (34) is recycled and will constitute the first portion of regenerant solution to be used in the next cycle of regeneration.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Non-Alcoholic Beverages (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

L'invention concerne un procédé de production d'acide tartrique et d'un concentré d'anthocyane provenant de sous-produits vinicoles. Ce processus est caractérisé par le retrait des pigments présents dans les sous-produits par leur adsorption sur une résine adsorbante polymère appropriée, avant la production de l'acide tartrique. Cet acide tartrique est ensuite produit à partir de bitartrate de potassium au moyen d'un procédé d'échange d'ions utilisant une résine à fort échange de cations de type gel, développée notamment pour des applications alimentaires, contenue dans un lit fixe. Le procédé de l'invention concerne également le recyclage de la solution de régénération d'échange de cations et l'éthanol utilisé en tant qu'agent régénérant de la résine adsorbante. Cette opération permet de réduire sensiblement la quantité d'effluents à rejeter du système, d'augmenter la récupération de l'acide tartrique et d'extraire les anthocyanes. En outre, une exemplification de ce procédé est présentée de manière schématique dans la figure 3.
EP00908140A 2000-03-17 2000-03-17 Procede de production d'acide tartrique et d'un concentre de pigments de raisin Withdrawn EP1185611A1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/PT2000/000001 WO2001068797A1 (fr) 2000-03-17 2000-03-17 Procede de production d'acide tartrique et d'un concentre de pigments de raisin

Publications (1)

Publication Number Publication Date
EP1185611A1 true EP1185611A1 (fr) 2002-03-13

Family

ID=20081540

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00908140A Withdrawn EP1185611A1 (fr) 2000-03-17 2000-03-17 Procede de production d'acide tartrique et d'un concentre de pigments de raisin

Country Status (4)

Country Link
EP (1) EP1185611A1 (fr)
AU (1) AU2951200A (fr)
HK (1) HK1047447A1 (fr)
WO (1) WO2001068797A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10308045B3 (de) * 2003-02-26 2004-06-17 Lurgi Ag Verfahren und Vorrichtung zur kontinuierlichen Gewinnung freier Weinsäure aus Kaliumhydrogentartrat enthaltenden Rohstoffen
US20120014934A1 (en) * 2010-07-13 2012-01-19 Paul Altaffer Enhanced Natural Colors
GR20150100473A (el) * 2015-10-30 2017-07-03 Εθνικο Κεντρο Ερευνας Και Τεχνολογικης Αναπτυξης (Ε.Κ.Ε.Τ.Α.) Καινοτομος μεθοδος ανακτησης τρυγικου οξεος και συμπυκνωματος φαινολικων ουσιων απο αποβλητα οινοποιησης

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1291155A (fr) * 1961-05-13 1962-04-20 Benckiser Gmbh Joh A Procédé de préparation de colorants naturels à partir de fruits ou autres parties de plantes
FR2299385A1 (fr) * 1975-02-03 1976-08-27 Finedoc Sica Sa Procede d'extraction des anthocyanes des fruits
FR2318908A1 (fr) * 1975-07-22 1977-02-18 Sefcal Sarl Procede de traitement d'extraits anthocyaniques
FR2378070A1 (fr) * 1977-01-25 1978-08-18 Roussillon Alimentaire La Cata Procede d'extraction d'anthocyanes a partir de marcs de raisins, lies et vins
BR9510645A (pt) * 1995-09-27 1999-07-27 Zsuzsanna Balazs Processo contínuo para a preparação de ácido tartárico e levedura de forragem da borra de vinho (sedimentos)

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0168797A1 *

Also Published As

Publication number Publication date
WO2001068797A1 (fr) 2001-09-20
AU2951200A (en) 2001-09-24
HK1047447A1 (zh) 2003-02-21

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