WO2016110521A1 - Dispositif et procédé de séchage continu par sublimation de gouttes et microgouttes congelées dans un circuit de gaz fermé - Google Patents

Dispositif et procédé de séchage continu par sublimation de gouttes et microgouttes congelées dans un circuit de gaz fermé Download PDF

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Publication number
WO2016110521A1
WO2016110521A1 PCT/EP2016/050163 EP2016050163W WO2016110521A1 WO 2016110521 A1 WO2016110521 A1 WO 2016110521A1 EP 2016050163 W EP2016050163 W EP 2016050163W WO 2016110521 A1 WO2016110521 A1 WO 2016110521A1
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WO
WIPO (PCT)
Prior art keywords
station
collecting
drops
workstation
freezing tube
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.)
Ceased
Application number
PCT/EP2016/050163
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German (de)
English (en)
Inventor
Richard Süverkrüp
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.)
Individual
Original Assignee
Individual
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 Individual filed Critical Individual
Priority to EP16700690.7A priority Critical patent/EP3243033A1/fr
Publication of WO2016110521A1 publication Critical patent/WO2016110521A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00—Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
    • F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
    • F26B5/065—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing the product to be freeze-dried being sprayed, dispersed or pulverised

Definitions

  • the invention relates to a device for producing freeze-dried drops from a liquid solution comprising a freezing gas acted upon by a cooled freezing tube and an injector arranged at the upper end of the freezing tube for dropwise injection of the liquid solution into the freezing tube and a screening device arranged below the freezing tube, by means of which collected from the freezing tube frozen drops are collected and a corresponding method.
  • Freeze-dried or lyophilized powders of spherical particles combine some important for the formulation of drugs
  • thermolabile and hydrolysis-sensitive materials are suitable for the processing of thermolabile and hydrolysis-sensitive materials
  • suitable matrix-forming auxiliaries are added, they can improve the dissolution rate of poorly water-soluble active substances.
  • They are suitable as carriers of vaccines for nasal and ballistic intradermal administration.
  • irritant-free ophthalmic drugs As an irritant-free ophthalmic drug, they contain no preservatives, dissolve rapidly in the tear fluid, are easy and safe to use and reduce the risk of side effects from systemic absorption.
  • the invention is particularly suitable for the preparation of frozen powders such as are obtained, for example, according to US Pat. No. 7,007,406 by spraying a solution with the aid of a two-substance nozzle.
  • Other methods for producing drops which can be dried after sublimation freezing are based, for example, on the piezoelectric atomization of liquids (C. Rochelle and G. Lee (2007): Dextran or hydroxyethyl starch in spray-freeze-dried trehalose / mannitol microparticles intended as ballistic particulate carriers for proteins, J. Pharm Sci. 96, 2296-2309).
  • the object of the invention is therefore to propose a device and a method with significantly improved manufacturing quality and efficiency.
  • the invention has the following objectives:
  • Dispensing vessels is dosed and
  • the screening device comprises a plurality of collecting sieves, which are movable in cycles in a housing between a plurality of workstations, wherein a workstation is arranged as a receiving station below the freezing tube.
  • a workstation is arranged as a receiving station below the freezing tube.
  • the collecting sieves are received in a rotatably mounted in the housing rotor disk and the rotor disk is cyclically rotatable between the work stations. Furthermore, the
  • Subsequent station at least one drying station and an unloading station are provided as further workstations and all
  • Workstations have inflow and outflow openings for a flow of gas through the housing and the collection screen located in the workstation.
  • the at least one, preferably all, drying station can flow through a drying gas stream in order to carry out sublimation drying of the frozen drops collected on the collecting sieve.
  • the first drying station can perform a sublimation drying of the frozen drops by means of a first dry gas stream as primary drying and in the subsequent workstation, the second drying station, a further drying by evaporation of the bound adsorbed water in the drops by a second dry gas stream as
  • a further workstation in the form of an unloading station is provided following the at least one drying station, within which the previously collected and dried drops are discharged from the collecting screen by means of a discharge gas flow, which flows counter to the direction of gravity through the unloading station and then eg in a suitable
  • a solids separator can be formed by a cyclone separator.
  • a cooling station in which a cooling gas flows.
  • the drip tray previously emptied of dried droplets, can be pre-cooled again to a suitable temperature before it is returned to the receiving station in the next working cycle and the process starts anew.
  • the invention proposes, at least the freezing gas, the
  • Dry gas streams and the discharge gas flow to lead in a common circuit and to use each partial gas flows of the entire gas stream for the respective application and to condition.
  • Figure 2 The invention according to Figure 1 in more detail in a horizontal development.
  • a device for producing freeze-dried drops which comprises in its essential components an injector 1 with a subsequent below freezing tube 10, from which drops 3 of a solution are injected into the freezing tube 10. Within the freezing tube 10, these drops come with a supplied at 12 and 13 cooled
  • the droplets 3 emerging from the freezing tube 10 following the gas flow and the force of gravity are collected by means of a sieve device 2 explained in detail below, dried and subsequently discharged from the circulation.
  • a sieve device 2 explained in detail below, dried and subsequently discharged from the circulation.
  • a plurality of similar collecting sieves 20 are arranged in a rotor disk 21 at the same distance from the center and at equal angular intervals, as can be seen in particular from FIG.
  • This rotor disc 21 is rotatably arranged in a housing 22 by means of a drive not shown in detail and is cyclically moved in equal angular increments in a rotational direction.
  • Each of the marked positions of the here five collection sieves is assigned to a work station I, II, III, IV, and V, which is successively and quasi continuously traversed by cyclically rotating the rotor disc 21 of each collection sieve 20.
  • the corresponding collection sieve 20 is positioned below the freezing tube 10, so that the freezing gas G flows from the freezing tube 10 as shown by arrows through the collecting sieve 20 and the entrained frozen drops 3 collected on the collecting sieve 20 become.
  • the collecting sieve 20 can be, for example, an optionally pre-cooled metal sieve which is earthed in order to discharge any electrostatic charge.
  • Angular step rotated when a defined layer of frozen drops 3 has been collected on the collecting screen 20 in the receiving station I.
  • the collecting strainer previously positioned in the receiving station I reaches the
  • the fraction of frozen drops 3 collected on the collecting screen 20 is primary dried in a cold gas stream whose temperature is higher than that of the freezing gas but below the melting point
  • the cold gas stream in the workstation II is also referred to as the first dry gas stream.
  • the bound and adsorbed water from the drops 3 is evaporated at elevated temperature in the secondary drying phase by means of a second dry gas stream passed through this workstation.
  • the surface temperature and the water content of the dry material are monitored in the area of the work stations II and III by analysis of the infrared reflectance and / or transmission spectrum and as a guide to the
  • part of the sublimation energy can also be supplied to the dry material by infrared or microwave radiation.
  • the dried droplets 3 are removed by an ascending, ie opposite to the dry gas streams directed gas flow of Entladegasstromes from collecting sieve 20 and removed from the housing 22 and preferably in a cyclone 4 and preferably transferred under aseptic conditions in pre-sterilized containers 5, see Figure 2).
  • V which is also called cooling station.
  • cooling station In this workstation
  • V is the emptied collecting sieve 20 by means of a flowing
  • Cooling gas cooled again to the temperature level required to re-collect frozen drops in the workstation I.
  • drying in steps II and III can also be distributed over several further work cycles, which may also be carried out at different temperatures.
  • Particles take place in an almost completely closed system in which energy and the drying solution are continuously fed in and cyclically from the dried product and the solvent separated therefrom
  • Solvent-laden process gas is collected and cooled in a condenser 60 to the temperature level required for freezing the drops 3. In this case, the solvent is frozen on the cooling surfaces of the capacitor 60.
  • at least one further condenser 61 is provided which is defrosted while in the other condenser 60 the vaporized solvent is separated from the process gas.
  • the capacitors 60, 61 are
  • the cycle of the process gas is by a compressor. 7
  • Capacitor outlet are used for freezing the droplet jet in the freezing tube 10 and for precooling a deflated collecting sieve 20 in the workstation V, on which the frozen drops 3 are collected in the respective following working cycle.
  • a third partial flow is heated to the temperature level required for primary drying. Of this, however, only one portion is used for the primary drying and supplied to the workstation II, while the temperature of the residual stream for the secondary drying is further increased.
  • Leaks can be detected and eliminated without compromising product quality.

Landscapes

  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Drying Of Solid Materials (AREA)

Abstract

L'invention concerne un dispositif de production de particules sphériques séchées et congelées (3) constituées de gouttes congelées. Le dispositif comprend un tube de congélation (10) alimenté en gaz de congélation refroidi (G), un injecteur (1) disposé à l'extrémité supérieure du tube de congélation (10) et destiné à injecter goutte à goutte la solution liquide dans le tube de congélation (10) et un moyen de tamisage (2) disposé au-dessous du tube de congélation (2) et permettant de collecter les gouttes congelées (3) sortant du tube de congélation (10). Le moyen de tamisage (2) comprend une pluralité de tamis collecteurs (20) qui peuvent être déplacés dans un boîtier (22) de manière cadencée entre plusieurs stations de travail (I, II, III, IV, V). Une station de travail (I) est disposée en tant que station de collecte au-dessous du tube de congélation (10). L'invention concerne également un procédé correspondant.
PCT/EP2016/050163 2015-01-07 2016-01-07 Dispositif et procédé de séchage continu par sublimation de gouttes et microgouttes congelées dans un circuit de gaz fermé Ceased WO2016110521A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP16700690.7A EP3243033A1 (fr) 2015-01-07 2016-01-07 Dispositif et procédé de séchage continu par sublimation de gouttes et microgouttes congelées dans un circuit de gaz fermé

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE102015100126 2015-01-07
DE102015100126.8 2015-01-07
DE102015106791.9 2015-04-30
DE102015106791.9A DE102015106791A1 (de) 2015-01-07 2015-04-30 Vorrichtung und Verfahren zur kontinuierlichen Sublimationstrocknung gefrorener Tropfen und Mikrotropfen in einem geschlossenen Gaskreislauf

Publications (1)

Publication Number Publication Date
WO2016110521A1 true WO2016110521A1 (fr) 2016-07-14

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2016/050163 Ceased WO2016110521A1 (fr) 2015-01-07 2016-01-07 Dispositif et procédé de séchage continu par sublimation de gouttes et microgouttes congelées dans un circuit de gaz fermé

Country Status (3)

Country Link
EP (1) EP3243033A1 (fr)
DE (2) DE102015105375B4 (fr)
WO (1) WO2016110521A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118856807A (zh) * 2024-07-19 2024-10-29 东富龙科技集团股份有限公司 实验型雾化冷冻装置及操作方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102017119649A1 (de) 2017-08-28 2019-02-28 Richard Süverkrüp Verfahren zur kontinuierlichen Herstellung gefriergetrockneter Tropfen in einem geschlossenen Gaskreislauf
CN113101864B (zh) * 2021-04-08 2022-09-30 青岛鼎喜冷食有限公司 一种防拉丝益生菌凝胶颗粒成型装置

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002104659A (ja) * 2000-09-29 2002-04-10 Akatake Engineering Kk 粉体供給装置
EP2578974A1 (fr) * 2011-10-05 2013-04-10 Sanofi Pasteur Sa Chaîne de traitement pour la production de particules lyophilisées
DE102012109406A1 (de) * 2012-10-02 2014-04-03 Richard Süverkrüp Verfahren und Anlage zur kontinuierlichen Produktion von pharmazeutischen Lyophilisaten

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3144310A (en) * 1960-05-03 1964-08-11 Glatt Devices for drying damp granules
GB1030678A (en) * 1964-01-25 1966-05-25 Terenzio Bersano Apparatus for the cooling or heating, by continuous air circulation, of granulated materials
US7007406B2 (en) 2004-01-23 2006-03-07 Zhaolin Wang Powder formation by atmospheric spray-freeze drying
DE102008017461B4 (de) 2008-04-03 2010-04-15 Süverkrüp, Richard, Prof. Dr. Vorrichtung und Verfahren zur Herstellung eines pulverförmigen lyophilisierten Materials, bestehend aus annähernd gleich großen kugelförmigen Teilchen
DK2491255T5 (da) * 2009-10-21 2015-06-22 Gea Process Engineering As Luftfordeler til en spraytørrer og fremgangsmåde til indstilling af en luftfordeler
WO2013041542A1 (fr) * 2011-09-19 2013-03-28 Alf Lamprecht Formulations pharmaceutiques comprenant des sphérolyophilisats de molécules biologiques

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002104659A (ja) * 2000-09-29 2002-04-10 Akatake Engineering Kk 粉体供給装置
EP2578974A1 (fr) * 2011-10-05 2013-04-10 Sanofi Pasteur Sa Chaîne de traitement pour la production de particules lyophilisées
DE102012109406A1 (de) * 2012-10-02 2014-04-03 Richard Süverkrüp Verfahren und Anlage zur kontinuierlichen Produktion von pharmazeutischen Lyophilisaten

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118856807A (zh) * 2024-07-19 2024-10-29 东富龙科技集团股份有限公司 实验型雾化冷冻装置及操作方法

Also Published As

Publication number Publication date
DE102015106791A1 (de) 2016-07-07
DE102015105375B4 (de) 2016-11-03
DE102015105375A1 (de) 2016-07-07
EP3243033A1 (fr) 2017-11-15

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