EP1703897A2 - Procede de production de granules d'acide ceto-l-gulonique obtenus par pulverisation - Google Patents

Procede de production de granules d'acide ceto-l-gulonique obtenus par pulverisation

Info

Publication number
EP1703897A2
EP1703897A2 EP04804409A EP04804409A EP1703897A2 EP 1703897 A2 EP1703897 A2 EP 1703897A2 EP 04804409 A EP04804409 A EP 04804409A EP 04804409 A EP04804409 A EP 04804409A EP 1703897 A2 EP1703897 A2 EP 1703897A2
Authority
EP
European Patent Office
Prior art keywords
keto
gulonic acid
fluidized bed
drying
spray
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Withdrawn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
EP04804409A
Other languages
German (de)
English (en)
Inventor
Martin Merger
Tillmann Faust
Robert Bayer
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.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Publication of EP1703897A2 publication Critical patent/EP1703897A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1682—Processes
    • A61K9/1688—Processes resulting in pure drug agglomerate optionally containing up to 5% of excipient
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/185—Acids; Anhydrides, halides or salts thereof, e.g. sulfur acids, imidic, hydrazonic or hydroximic acids
    • A61K31/19—Carboxylic acids, e.g. valproic acid
    • A61K31/191—Carboxylic acids, e.g. valproic acid having two or more hydroxy groups, e.g. gluconic acid

Definitions

  • the present invention relates to a process for the preparation of keto-L-gulonic acid spray granules.
  • Keto-L-gulonic acid is an important intermediate in the production of ascorbic acid (vitamin C).
  • crystalline keto-L-gulonic acid is produced via the process steps of the fermentative production of sodium ketogulonate, cell separation, ion exchange chromatography, evaporation and crystallization.
  • keto-L-gulonic acid spray granules from finely divided, pure keto-L-gulonic acid by using an aqueous or water-containing solution of keto-L-gulonic acid a) a spray fluidized-bed drying, b) a single-component atomization drying or c) a spray drying Sputtering drying supplies.
  • the process according to the invention is particularly advantageous if the aqueous or water-containing solution of pure keto-L-gulonic acid is fed to a fluidized-bed dryer.
  • keto-L-gulonic acid as is available in the prior art, is used as the starting material for the process according to the invention.
  • Keto-L-gulonic acid which has been produced in a fermentative process, is used particularly advantageously.
  • the aqueous or water-containing solution of the pure keto-L-gulonic acid usually contains 10 to 80% by weight, preferably 40 to 70% by weight of keto-L-gulonic acid.
  • water-miscible solvents include, for example, alkanols with a chain length of 1 to 4 carbon atoms.
  • Pure keto-L-gulonic acid is hereinafter referred to as a keto-L-gulonic acid with a degree of purity of higher than 95%, preferably 98 or 99%.
  • the solution is sprayed continuously or discontinuously into a fluidized bed of dry reaction product in the spray fluidized bed drying according to the invention.
  • keto-L-gulonic acid in the form of a keto-L-gulonic acid dry powder is placed in a fluidized bed dryer in a fluidized bed kept at 50 to 150 ° C., for this purpose adds the aqueous or water-containing solution of keto-L-gulonic acid in sprayed form in accordance with the drying rate, removes the keto-L-gulonic acid particles from the fluidized bed after a suitable dwell time and separates them into particle fractions by means of a suitable device, which removes the particle fraction in the particle size range of approximately and returns the finely divided particles and / or the coarser particles to the granulation process, if necessary after comminution.
  • the spray fluidized bed drying can be carried out batchwise or continuously, but the continuous mode of operation is preferred.
  • keto-L-gulonic acid product To carry out the process, such a keto-L-gulonic acid product must first be produced from dry keto-L-gulonic acid powder, with the aid of which a fluidized bed can be produced. In the case of discontinuous operation, a relatively fine-particle product can be placed in the fluidized bed. Depending on the residence time of the particles in the fluidized bed, a dry product with a smaller or larger particle size range is then obtained. Particles in the size range from 50 to 1000 ⁇ m, preferably 100 to 500 ⁇ m, have the desired handling properties and are therefore obtained as a valuable product. Smaller particles and keto-L-gulonic acid product obtained by suitable grinding, for example grinding larger particles, are used as fluidized bed material for further batches.
  • the aqueous or water-containing solution of keto-L-gulonic acid is sprayed continuously into a fluidized bed.
  • the rate of spraying is adjusted so that the fluidized bed has a temperature corresponding to the desired degree of drying. Accordingly, it is ultimately determined by the difference between the inlet and outlet temperatures of the fluidizing gas. If the process is carried out continuously, the first time the fluidized bed dryer is started up, fine-particle keto-L-gulonic acid in the fluidized bed is assumed. Then you get a dry product with an almost constant particle size ratio. A certain part of this is continuously removed and separated into particle size fractions.
  • Customary binders for the spray fluidized-bed drying process according to the invention can also be added to the keto-L-gulonic acid, but the embodiment without the addition of binders is preferred.
  • keto-L-gulonic acid An aqueous solution containing 50% by weight of keto-L-gulonic acid was placed in a laboratory stirred tank, heated to approx. 45 ° C. and continuously pumped into the Miniplant spray vortex dryer under the in Boundary conditions listed in Table 1 injected.
  • the solid produced was continuously discharged. This resulted in 8.5 kg of free-flowing, dust-free keto-L-gulonic acid granules with a residual moisture content of ⁇ 0.5% by weight and the following particle size distribution: 91% ⁇ 900 ⁇ m, 9%> 900 ⁇ m
  • aqueous solution with 35% by weight of keto-L-gulonic acid was placed in a stirred tank and heated to about 35 to 40 ° C. With the help of a peristaltic pump, the solution was continuously injected into the pilot plant spray vortex dryer under the boundary conditions listed in Table 1 over a period of 18 hours.
  • the solid produced was continuously discharged. This resulted in 320 kg of free-flowing, dust-free keto-L-gulonic acid granulate with a residual moisture content of ⁇ 0.5% by weight and the following particle size distribution:

Landscapes

  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Epidemiology (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un procédé de production de granulés d'acide céto-L-gulonique ayant une bonne faculté d'écoulement, ne formant pas de poussière, à partir d'acide céto-L-gluonique pur en fines particules. Selon ledit procédé, une solution d'acide céto-L-gulonique aqueuse ou contenant de l'eau est conduite à a) une installation de séchage par pulvérisation en lit fluidisé, b) une installation de séchage par pulvérisation à buse à un seul fluide ou c) une installation de séchage par pulvérisation à disque.
EP04804409A 2004-01-05 2004-12-30 Procede de production de granules d'acide ceto-l-gulonique obtenus par pulverisation Withdrawn EP1703897A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200410001187 DE102004001187A1 (de) 2004-01-05 2004-01-05 Verfahren zur Herstellung von Keto-L-gulonsäuresprühgranulaten
PCT/EP2004/014824 WO2005065655A2 (fr) 2004-01-05 2004-12-30 Procede de production de granules d'acide ceto-l-gulonique obtenus par pulverisation

Publications (1)

Publication Number Publication Date
EP1703897A2 true EP1703897A2 (fr) 2006-09-27

Family

ID=34716328

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04804409A Withdrawn EP1703897A2 (fr) 2004-01-05 2004-12-30 Procede de production de granules d'acide ceto-l-gulonique obtenus par pulverisation

Country Status (3)

Country Link
EP (1) EP1703897A2 (fr)
DE (1) DE102004001187A1 (fr)
WO (1) WO2005065655A2 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102008045739B4 (de) 2008-09-04 2021-12-30 ABUS August Bremicker Söhne Kommanditgesellschaft Schließzylindersystem
CN103110105A (zh) * 2012-11-14 2013-05-22 江苏江山制药有限公司 食品添加剂无糖维生素c钠盐颗粒的生产方法
CN107473959B (zh) * 2017-08-30 2021-03-12 沈阳农业大学 一种维生素c生产中的古龙酸减排提取法
CN108774125A (zh) * 2018-05-28 2018-11-09 苏州澄江环境科技有限公司 一种从古龙酸母液中回收原料的工艺

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5268283A (en) * 1990-10-05 1993-12-07 Miles Inc. Method for the production of detergent builder formulations utilizing spray granulated citric acid and salts thereof
AU1343997A (en) * 1995-12-27 1997-07-28 Genencor International, Inc. Process for the preparation of gluconic acid and gluconic acid produced thereby
US6187570B1 (en) * 1998-05-26 2001-02-13 The Electrosynthesis Company, Inc. Electrodialysis methods for purification and recovery of gluconic acid derivatives
WO2001009074A1 (fr) * 1999-08-03 2001-02-08 Archer-Daniels-Midland Company Procede pour la recuperation d'acides organiques

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2005065655A3 *

Also Published As

Publication number Publication date
WO2005065655A3 (fr) 2005-11-03
DE102004001187A1 (de) 2005-08-04
WO2005065655A2 (fr) 2005-07-21

Similar Documents

Publication Publication Date Title
EP0131097B1 (fr) Procédé de préparation de polyphosphates d'ammonium pulvérulents et stables à l'hydrolyse
EP1185634B1 (fr) Formulations instantanees d'enzymes pour l'alimentation des animaux
DE4141351A1 (de) Stabile pulverfoermige vitamin- und/oder carotinoid-praeparate und verfahren zu deren herstellung
DE3409063A1 (de) Verfahren zur herstellung von fliessfaehigen cholinchlorid-kieselsaeure-pulvern
DE10161402A1 (de) Verfahren zur Herstellung von direkt tablettierbarem beta-Mannit
EP2872481A1 (fr) Procédé pour traiter des résidus de distillation provenant de la production d'isocyanate
EP0345717B1 (fr) Procédé de fabrication de riboflavine, préparée par voie microbienne en granulés séchés par pulvérisation ou en microgranulés
EP0959068A2 (fr) Procédé pour la préparation d'une solution aqueuse de méthioninate de sodium et l'utilisation de ces solutions pour la préparation d'un granulat
EP0017972A1 (fr) Procédé pour la récupération du toluène diisocyanate et/ou de solvants à point d'ébullition élevé dans un lit fluidisé, à partir de résidus de distillation de la fabrication du toluène diisocyanate
CH643526A5 (de) Verfahren zur herstellung von 2-hydroxynaphthalincarbonsaeuren.
EP1703897A2 (fr) Procede de production de granules d'acide ceto-l-gulonique obtenus par pulverisation
EP0870537B1 (fr) Procédé de préparation des granulés contenant de l'alcool
DE1667979B2 (de) 1,3-benzodioxolcarbamate sowie verfahren zu deren herstellung und schaedlingsbekaempfungsmittel mit einem gehalt dieser verbindungen
EP1072581A2 (fr) Procédé de préparation du propionate de calcium et installation pour la mise en oeuvre du procédé
EP0390826B1 (fr) Procede de production de composes d'aminmoaryl-beta-sulfatoethylesulfones
WO2020174019A1 (fr) Procédé pour obtenir de la fucoxanthine et des acides gras à partir d'une biomasse algale
DE947159C (de) Verfahren zur Herstellung von Sulfochloridgruppen tragenden Isocyanaten
EP0119463B2 (fr) Procédé de séparation d'isomères d'acides cyclopropane-carboxyliques substitués
DE10212322A1 (de) Herstellung von Alkalisalzen von alpha-Ketoncarbonsäuren
EP0095569B1 (fr) Procédé de préparation de phénylpyridazines
AT313854B (de) Sprühtrockenverfahren
WO2004089889A2 (fr) Procede de production de riboflavine de la modification b/c sous forme de granules
EP2651397A2 (fr) Procédé de préparation de mannitol delta pouvant être directement transformé en comprimés
DE102008000265A1 (de) Verfahren zur Herstellung von verfestigtem Menthol
DE3840362A1 (de) Verfahren zur herstellung von aminoaryl-ss-sulfatoethylsulfon-verbindungen

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20060807

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU MC NL PL PT RO SE SI SK TR

DAX Request for extension of the european patent (deleted)
STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION HAS BEEN WITHDRAWN

18W Application withdrawn

Effective date: 20061114