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EP3408015A1 - Procédé de production d'émulsions - Google Patents

Procédé de production d'émulsions

Info

Publication number
EP3408015A1
EP3408015A1 EP17706142.1A EP17706142A EP3408015A1 EP 3408015 A1 EP3408015 A1 EP 3408015A1 EP 17706142 A EP17706142 A EP 17706142A EP 3408015 A1 EP3408015 A1 EP 3408015A1
Authority
EP
European Patent Office
Prior art keywords
emulsion
collision
bar
liquid streams
room
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.)
Granted
Application number
EP17706142.1A
Other languages
German (de)
English (en)
Other versions
EP3408015B1 (fr
Inventor
Bernd BAUMSTÜMMLER
Hermann Schirra
Akif Emre TÜRELI
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.)
Instillo GmbH
Original Assignee
Instillo GmbH
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 Instillo GmbH filed Critical Instillo GmbH
Publication of EP3408015A1 publication Critical patent/EP3408015A1/fr
Application granted granted Critical
Publication of EP3408015B1 publication Critical patent/EP3408015B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • B01F23/4105—Methods of emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • B01F23/413—Homogenising a raw emulsion or making monodisperse or fine emulsions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/70—Pre-treatment of the materials to be mixed
    • B01F23/702—Cooling materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/70—Pre-treatment of the materials to be mixed
    • B01F23/711—Heating materials, e.g. melting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/80—After-treatment of the mixture
    • B01F23/802—Cooling the mixture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/80—After-treatment of the mixture
    • B01F23/811—Heating the mixture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
    • B01F25/23—Mixing by intersecting jets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0418—Geometrical information
    • B01F2215/0427—Numerical distance values, e.g. separation, position
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0418—Geometrical information
    • B01F2215/0431—Numerical size values, e.g. diameter of a hole or conduit, area, volume, length, width, or ratios thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/0468—Numerical pressure values
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/0481—Numerical speed values

Definitions

  • the invention relates to a method for producing emulsions.
  • Emulsions are understood below to mean both colloidal emulsions and industrial emulsions, the latter differing from the colloidal emulsions by considerably larger particle dimensions in the micrometer range.
  • Emulsions are formed when two or more immiscible liquids are mixed together.
  • One of these liquids is usually water-soluble and the other is a lipophilic liquid which is immiscible with water.
  • either water-in-oil emulsions or oil-in-water emulsions can be prepared.
  • a disadvantage of emulsions is their instability, which relies on physicochemical mechanisms such as gravity separation, flocculation, coalescence, and Ostwald ripening.
  • oil-in-water emulsions the most common cause of instability is gravity separation in the form of creaming, which occurs due to the lower density of the oil particles.
  • Emulsions with a Oltröpfchen tend to go over in a short time in two separate phases, while at a Oltröpfchen pertain of less than 1 ⁇ increases the stability of the emulsion with decreasing Oltröpfchen stands.
  • a four times greater energy input is necessary to reduce the oil droplet size by 50%, which limits the minimum oil droplet size achievable.
  • due to the energy input there is a risk of a temperature rise to temperatures above 70 ° C, at which a destruction of the emulsifiers may occur.
  • the limiting factors are the pore size of the membranes used and the pressure resulting from the viscosity of the oil phase.
  • a microjet reactor corresponding to EP 1 165 224 B1 being used.
  • Such a microjet reactor has at least two opposing nozzles, each with associated pump and supply line for spraying each of a liquid medium in a reactor chamber enclosed by a reactor chamber to a common collision point, wherein a first opening is provided in the reactor housing, through which a gas, a evaporating liquid, a cooling liquid or a cooling gas for maintaining the gas atmosphere inside the reactor, in particular at the collision point of the liquid jets, or for cooling the resulting products can be introduced, and provided a further opening for removing the resulting products and excess gas from the reactor housing is.
  • a gas, an evaporating liquid or a cooling gas is maintained to maintain a gas atmosphere in the interior of the reactor, in particular at the point of collision introduced the liquid jets, or for cooling the resulting products and the resulting products and excess gas through an opening from the reactor housing by pressure on the gas inlet te or by under pressure on the product and gas outlet side away.
  • a solvent / non-solvent precipitation for example as described in EP 2 550 092 A1
  • a dispersion of the precipitated particles is obtained. With such a reactor, it is possible to generate particularly small particles.
  • a solvent / nonsolvent precipitation means that a substance is dissolved in a solvent and collides as a liquid jet with a second liquid jet, wherein the solute is precipitated again.
  • a disadvantage of solvent / Nonsolvent precipitation is the fact that the dissolved and reprecipitated substance is particulate in the solvent-Nonsolvent mixture after precipitation. In this case, the solvent content causes that for many particles time-dependent Ostwald ripening sets, which causes a growth of the particles.
  • a device for emulsifying at least two liquids which comprises an emulsion reactor having an outlet for removing the emulsion resulting from the mixing of the liquids and in which a plurality of for injection to substantially a common Collision point aligned nozzles is provided, each nozzle is associated with a respective supply line and a pump which pumps a liquid from an associated tank through the supply line in the emulsion reactor.
  • the object of the invention is therefore to provide a novel process for the preparation of emulsions, which also enables the preparation of asymmetric emulsions.
  • This object is achieved in that in a first step at least one pre-emulsion of at least two immiscible liquids is generated and then in a second step at least two liquid streams of the at least one pre-emulsion are pumped through separate openings with a defined diameter to flow rate of the liquid streams of more than 10 m / s and that the liquid streams meet at a collision point in a room.
  • emulsions namely the asymmetric emulsions in which the oil and the water phase are not present in a ratio of 1: 1
  • This pre-emulsion is then introduced in the form of two liquid streams into a device in which both streams of liquid meet at a collision point in a space, for example a microjet reactor.
  • a homogeneous emulsion Due to the collision of the liquid streams at high flow rates, which forms a plate-shaped collision plate in the collision point, a homogeneous emulsion is achieved with an oil droplet size of less than 1 ⁇ due to the kinetic energy, which is also very stable accordingly. There is no further input of energy, e.g. Shear forces needed. It can be carried out in the aqueous phase at temperatures between 0 ° C and 100 ° C, preferably at temperatures between room temperature and 70 ° C, more preferably at temperatures between room temperature and 50 ° C.
  • the pressure of the liquid jets is between 5 and 5,000 bar, preferably between 10 and 1,000 bar, and more preferably between 20 and 500 bar.
  • the diameter of the openings is identical or different and 10 to 5,000 ⁇ , preferably 50 to 3,000 ⁇ and particularly preferably 100 to 2,000 ⁇ . It is possible to work with openings of different diameters, for example, on one side of an opening with a diameter of 100 ⁇ and on the other side of an opening with a diameter of 300 ⁇ . Of course, the diameter of the openings on both sides can be the same.
  • the flow rate of the liquid streams after the nozzle are identical or different and more than 20 m / s, preferably more than 50 m / s and more preferably more than 100 m / s.
  • one of the liquid streams may have a higher flow rate than the other liquid stream, for example on the one hand 50 m / s and on the other hand 100 m / s. Again, it is possible that the flow rates of both liquid streams are equal.
  • the flow rate of the liquid streams after the nozzle can reach 500 m / s or 1,000 m / s.
  • the distance between the openings is less than 5 cm, preferably less than 3 cm, and more preferably less than 1 cm.
  • Belonging to the invention is also that the space is filled with gas or applied.
  • Gas in particular inert gas or inert gas mixtures, but also reactive gas can be supplied through a gas inlet in the room. It is preferred that the gas pressure in the space is 0.05 to 30 bar, preferably 0.2 to 10 bar, and more preferably 0.5 to 5 bar.
  • the droplet size can be influenced.
  • a solvent is introduced through a further inlet into the room.
  • propylene glycol may be introduced as a further solvent through the further inlet into the room.
  • An embodiment of the invention is that during the collision in the room, a pressure of less than 100 bar, preferably less than 50 bar and more preferably less than 20 bar prevails.
  • microjet reactor is used to carry out the process.
  • Such a microjet reactor is known from EP 1 165 224 Bl.
  • the droplet size of the emulsion is dependent on the system and operating parameters, in particular the nozzle size in the microjet reactor and the pump pressure of the pumping pumps for the two fluid streams.
  • the customary use of microjet reactors in the method according to the invention by the collision energy no precipitation reactions are caused in the microjet reactor, but emulsions are formed.
  • the emulsion produced is encapsulated.
  • the produced and possibly encapsulated emulsion is provided with a surface modification.
  • Examples 1 to 4 show the effects of variation of individual parameters, while Examples 5 to 21 contain examples of possible encapsulation processes.
  • the effect of the gas pressure was examined by colliding a liquid flow of oil and a liquid flow of water containing lecithin under different gas pressures in a space in which gas having different gas pressures was introduced through a gas inlet.
  • the oil was pumped at a flow rate of 50 ml / min and the aqueous phase at a flow rate of 250 ml / min.
  • the oil droplet size was determined by DLS. In all cases, an oil droplet size of less than 500 nm was achieved. The results show that the oil droplet size decreases with increasing gas pressure.
  • the influence of the diameter of the orifices was determined by testing different orifice diameters while using an oil flow rate of 50 ml / min and a water flow rate of 250 ml / min and the gas pressure was 2 bar.
  • the oil and water phases were pre-emulsified and pumped through the two inlets into a closed cycle to determine the influence of the number of cycles on oil droplet size within the emulsion.
  • a flow rate of 250 ml / min and a gas pressure of 2 bar prevailed in the room.
  • the oil droplet size within the emulsion thus decreases with the number of cycles.
  • An essential oil to be encapsulated is emulsified at a flow rate of 67 g / min in the microjet reactor with an aqueous Na-caseinate solution (22.4 mg / ml) at a flow rate of 200 g / min in the microjet reactor.
  • this emulsion is processed at a flow rate of 200 g / min against an aqueous xanthan gum solution (0.25%) at 25 g / min.
  • the oppositely charged side groups of the protein and the polysaccharide are attached to each other. Lowering the pH to pH 4 with 10% citric acid enhances this interaction, creating microcapsules.
  • the microcapsules are 50-100 ⁇ large.
  • An essential oil to be encapsulated is emulsified at a flow rate of 50 g / min in the microjet reactor into an aqueous whey protein isolate solution at a flow rate of 200 g / min. After the addition of 20% maltodextrin as carrier material, the emulsion is spray-dried. Drying produces a powder containing microencapsulated essential oil.
  • Example 7 Melt Dispersion / Matrixyer Encapsulation
  • a fragrance to be encapsulated (15-30%) is dissolved at 85 ° C in melted Compritol AO 888.
  • This oil phase is emulsified at 68 ml / min into a 20 ° C cold aqueous Tween 20 solution (0.5-1.5%) at 200 ml / min. Due to the rapid cooling of the fat, emulsion formation directly causes particle formation and matrix encapsulation of the fragrance.
  • the microcapsules are on average 5 ⁇ (0.5% Tween 20) or 2 ⁇ (1.5% Tween 20).
  • a fragrance to be encapsulated (15-30%) is dissolved at 85 ° C in melted Compritol AO 888.
  • This oil phase is emulsified at 68 ml / min into a 20 ° C cold gum arabic solution (2.5%, 200 ml / min). Due to the rapid cooling of the fat, particle formation occurs directly after emulsion formation.
  • Modification of these microcapsules is accomplished by processing this melt dispersion (200 ml / min) in the microjet reactor against a 50 ° C gelatin solution (2.5%, 150 g / min). By lowering the pH to pH 4 with 10% citric acid, the ionic interactions are intensified and gelled by cooling.
  • a hydrophilic polyalcohol (active substance) to be encapsulated is added to an aqueous ammonia solution (1%) (water phase) and in the MIR reactor against an emulsifier-containing (polyethyl-alkyl-polymethylsiloxane) 1% encapsulation solution (TEOS) Isoparaffin (oil phase) processed.
  • TEOS emulsifier-containing (polyethyl-alkyl-polymethylsiloxane) 1% encapsulation solution (TEOS) Isoparaffin (oil phase) processed.
  • the encapsulating material is formed by hydrolysis of the precursors.
  • the capsules can be separated by simple sedimentation or Zentrifugati on and are between 5 and 10 ⁇ large.
  • the method given in FIG. 1 is applied to a TEOS-containing encapsulation solution with the modification that the concentration of the emulsifier used has been reduced to 50% or 25% of the original concentration.
  • the microcapsules obtained are larger than those obtained according to Example 1.
  • the method given in Figure 1 is applied to another encapsulation chemistry.
  • a 20%) solution of an aqueous active substance to be encapsulated containing 10 meq H 2 of the encapsulation component HMDA is processed in MJR against a 1% emulsifier solution in isoparaffin.
  • the emulsion thus obtained is made by adding 40 meq COC1 a 20% Trimesoyl chloride solution cured in Isopar.
  • the resulting capsules are 2 to 30 ⁇ large.
  • Example 17 The procedure given in Example 17 is followed with the modification that capsule hardening is carried out by means of trimesoyl chloride solution in situ by continuous introduction of the solution into the reactor chamber via the fifth opening of the MJR reactor.
  • the resulting capsules have approximately the same properties as obtained according to Example 9.
  • Example 5 The procedure given in Example 5 is applied to oil-soluble encapsulants.
  • An oil-soluble active ingredient to be encapsulated is placed in a 20% solution of the encapsulating material (OTMS) in isoparaffin and mixed at room temperature for 5 minutes by stirring.
  • the solution thus obtained is processed in the MJR reactor at a process pressure of 40 bar against a 2% aqueous emulsifier solution.
  • the result is a stable homogeneous emulsion, the addition of the catalyst dibutyltin laurate (0.5%), the curing of the capsules which can be separated after curing by centrifugation or sedimentation.
  • Example 19 The procedure given in Example 19 is used with the modification that the capsule hardening by means of dibutyltin laurate takes place in situ by continuous introduction of the solution into the reactor chamber via the fifth opening of the MJR reactor.
  • the resulting capsules have approximately the same properties as obtained according to Example 19.
  • Example 21 Melt Dispersion / Matrix Encapsulation: Example 21:
  • Step 1
  • Step 2b (as an alternative to step 2a):
  • Step 3b (as an alternative to step 3a):
  • pre-emulsion a warm non-solvent
  • This pre-emulsion is introduced into the MJR on the right and left with a flow rate ratio of 1: 1.
  • the loaded polymer is microscopically precipitated.
  • Step 3c (as an alternative to step 3a or step 3b):
  • the modified melt is mixed with a portion of the heated non-solvent to reduce melt viscosity.
  • the mixture is precipitated with the cold residual non-solvent in the MJR process precipitating the polymer beads.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Colloid Chemistry (AREA)

Abstract

L'invention vise à créer un nouveau procédé de production d'émulsions qui permette d'obtenir des gouttelettes d'huile homogènes pour un apport d'énergie le plus réduit possible. À cet effet, au moins deux flux de liquide dont les liquides ne sont pas miscibles l'un avec l'autre sont pompés à travers des orifices séparés d'un diamètre défini pour atteindre une vitesse d'écoulement des flux de liquide supérieure à 10 m/s, et les flux de liquide se rencontrent dans une chambre en un point de collision, l'émulsion obtenue étant évacuée de la chambre par une sortie. Du fait de la collision des flux de liquide à des vitesses d'écoulement élevées auxquelles se forme une plaque de collision en forme de disque au point de collision, on obtient en raison de l'énergie cinétique une émulsion homogène dont la taille des gouttelettes d'huile est inférieure à 1 |xm et qui est en conséquence très stable. Aucun autre apport d'énergie, par exemple forces de cisaillement ou haute pression, n'est nécessaire.
EP17706142.1A 2016-01-25 2017-01-25 Procédé de production d'émulsions Active EP3408015B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102016101232.7A DE102016101232A1 (de) 2016-01-25 2016-01-25 Verfahren zum Herstellen von Emulsionen
PCT/DE2017/100046 WO2017129177A1 (fr) 2016-01-25 2017-01-25 Procédé de production d'émulsions

Publications (2)

Publication Number Publication Date
EP3408015A1 true EP3408015A1 (fr) 2018-12-05
EP3408015B1 EP3408015B1 (fr) 2021-08-11

Family

ID=58094095

Family Applications (1)

Application Number Title Priority Date Filing Date
EP17706142.1A Active EP3408015B1 (fr) 2016-01-25 2017-01-25 Procédé de production d'émulsions

Country Status (9)

Country Link
US (1) US20190030497A1 (fr)
EP (1) EP3408015B1 (fr)
JP (1) JP7031103B2 (fr)
KR (1) KR20180101573A (fr)
CN (1) CN108495708B (fr)
DE (1) DE102016101232A1 (fr)
DK (1) DK3408015T3 (fr)
ES (1) ES2893124T3 (fr)
WO (1) WO2017129177A1 (fr)

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WO2020234448A1 (fr) 2019-05-23 2020-11-26 Helm Ag Nanoparticules à base d'enzalutamide

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020234448A1 (fr) 2019-05-23 2020-11-26 Helm Ag Nanoparticules à base d'enzalutamide

Also Published As

Publication number Publication date
EP3408015B1 (fr) 2021-08-11
CN108495708B (zh) 2021-07-30
CN108495708A (zh) 2018-09-04
DK3408015T3 (da) 2021-11-01
JP7031103B2 (ja) 2022-03-08
DE102016101232A1 (de) 2017-07-27
ES2893124T3 (es) 2022-02-08
WO2017129177A1 (fr) 2017-08-03
JP2019508233A (ja) 2019-03-28
US20190030497A1 (en) 2019-01-31
KR20180101573A (ko) 2018-09-12

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