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WO2025176256A1 - Dispositif pour la réalisation de processus chimiques et physiques - Google Patents

Dispositif pour la réalisation de processus chimiques et physiques

Info

Publication number
WO2025176256A1
WO2025176256A1 PCT/DE2025/100161 DE2025100161W WO2025176256A1 WO 2025176256 A1 WO2025176256 A1 WO 2025176256A1 DE 2025100161 W DE2025100161 W DE 2025100161W WO 2025176256 A1 WO2025176256 A1 WO 2025176256A1
Authority
WO
WIPO (PCT)
Prior art keywords
reactor
nozzles
reactor housing
housing
outlet opening
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.)
Pending
Application number
PCT/DE2025/100161
Other languages
German (de)
English (en)
Inventor
Hermann Schirra
Christian CAVELIUS
Aljosha-Rakim JOCHEM
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.)
Nanosaar AG
Original Assignee
Nanosaar AG
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 Nanosaar AG filed Critical Nanosaar AG
Publication of WO2025176256A1 publication Critical patent/WO2025176256A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/02—Feed or outlet devices therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/002—Nozzle-type elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
    • B01J2219/00792—One or more tube-shaped elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00801—Means to assemble
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00858—Aspects relating to the size of the reactor
    • B01J2219/0086—Dimensions of the flow channels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00889—Mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/0095—Control aspects
    • B01J2219/00952—Sensing operations
    • B01J2219/00954—Measured properties
    • B01J2219/00959—Flow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/007—Feed or outlet devices as such, e.g. feeding tubes provided with moving parts

Definitions

  • the invention relates to a device for carrying out chemical and physical processes, wherein at least two nozzles, each with an associated pump and supply line, are provided for spraying a liquid medium into a reactor space enclosed by a reactor housing onto a common collision point, and an outlet opening is provided for removing the resulting products and excess gas from the reactor housing.
  • WO 00/61275 A2 discloses a method for carrying out chemical and physical processes.
  • at least two liquid media are injected via pumps, preferably high-pressure pumps, through a nozzle into a reactor chamber enclosed by a reactor housing to a common collision point, so that a gas, a vaporized liquid, a cooling liquid or a cooling gas is injected into the reactor chamber via an opening.
  • pumps preferably high-pressure pumps
  • a gas, a vaporized liquid, a cooling liquid or a cooling gas is injected into the reactor chamber via an opening.
  • DE 101 41 054 A1 describes a jet reactor for carrying out physical and chemical material transformations in a collision point of liquid jets located in a gas space, the adjustment of the reactor, the protection of the reactor against destruction by cavitation by means of tetrahedrally arranged ceramic balls and the use of the reactor for homogenization and emulsification.
  • a method for carrying out chemical and physical processes wherein two or more liquids or suspensions are injected into a vortex chamber through two or more nozzles that are not coaxially aligned with each other, at a pressure between 1 and 1,000 bar and a volume flow between 5 and 500 l/h, without using a carrier gas flow, is known from DE 102 49 747 A1.
  • the sleeve can be inserted into the reactor chamber through an inlet opening and/or an outlet opening.
  • the outer contour of the sleeve can correspond to the inner contour of the reactor housing.
  • the sleeve can have recesses for the at least two nozzles.
  • the sleeve can be designed as a one-piece or two-piece unit. In particular, in a two-piece unit, one part can be inserted through an inlet opening and the other part through an outlet opening.
  • the sleeve can include a seal for the inlet opening and/or outlet opening.
  • the sleeve can be changed depending on the reaction in the reactor chamber. This allows for a particularly rapid changeover of the reaction in the device.
  • One embodiment of the invention is that the at least two nozzles can be screwed into the reactor housing.
  • the advantage is that at least two nozzles can be changed particularly quickly and easily.
  • the at least two nozzles have a nozzle diameter (inner diameter of the nozzle) of 50 pm to 3 mm.
  • a further embodiment of the invention consists in that an inlet opening is provided in the reactor housing.
  • reactants can be introduced into the reactor chamber through the inlet opening in the reactor housing.
  • a gas, a vaporized liquid, a cooling liquid or a cooling gas can be introduced through the inlet opening to maintain the gas atmosphere inside the reactor, especially at the collision point of the liquid jets, or to Cooling of the resulting products can be initiated
  • the conversion of the reaction product and its comminution and/or the comminution of the reactants can take place simultaneously in the reaction chamber.
  • a preferred embodiment of the invention is characterized in that the reactor space enclosed by the reactor housing does not taper in the direction of the outlet opening for removing the resulting products and excess gas from the reactor housing.
  • the reactor space enclosed by the reactor housing thus has at least a constant cross-section in the direction of the outlet opening for removing the resulting products and/or excess gas from the reactor housing, but can also preferably have an expanding cross-section.
  • the flow through the outlet opening is designed for a flow volume of 0.1 l/h to 5000 l/h, preferably from 1 l/h to 800 l/h.
  • a further embodiment of the invention is that the device has three to eight, preferably four to six nozzles.
  • a further embodiment of the invention is that the reactor housing is adjustable by the at least two nozzle holders.
  • the reactor housing automatically adjusts itself in relation to the nozzle holders.
  • the nozzles do not have to be common collision point, so that subsequent adjustment of the nozzles is not necessary.
  • the device has additional means for supporting the discharge of reaction products from the reactor chamber, wherein the additional means can be introduced into the reactor housing or attached to the reactor housing.
  • the additional means can include, for example, mechanical disruption devices, filters, such as edge filters, ultrasonic transmitters, such as sonotrodes, or electromagnetic emitters.
  • the mechanical disruption devices can include, for example, mixers or impact plates.
  • the additional means can be introduced via the inlet and/or outlet openings.
  • the same device can be used for a variety of physical and chemical processes, or the results of the physical and chemical processes can be improved by introducing the additional means.
  • the mechanical discharge means can discharge the reaction products from the reactor chamber to the outlet opening. This is particularly advantageous for viscous reaction products.
  • the discharge means can comprise, for example, blade stirrers or rotors.
  • a further embodiment of the invention is that the reactor chamber is cylindrically shaped.
  • the diameter of the cylindrical reactor chamber can be changed.
  • a further preferred embodiment of the invention is that the at least two nozzles can be screwed into a nozzle holder, wherein the nozzle holders can be screwed into the reactor housing.
  • the reactor housing has two elements, wherein a first element encloses the reactor space and can be inserted into a second element, wherein the first and the second element can be connected by the at least two nozzles.
  • the diameter of the reactor housing can be changed by replacing the first element.
  • the second element can, for example, comprise means for holding the device.
  • inlet means and outlet means are provided, wherein the inlet means and the inlet opening and the outlet means and the outlet opening are detachably connectable.
  • the inlet means and the outlet means may comprise valves.
  • a further development of the invention is that a pressure of 0.5 to 1000 bar, preferably 10 to 100 bar, can be achieved by the pumps.
  • the pumps can be selected according to the pressure requirements.
  • the pumps can be micro annular gear pumps, gear pumps, piston pumps, piston diaphragm pumps, or high-pressure pumps.
  • Ceramic or diamond nozzles are made of a particularly hard and wear-resistant material.
  • the ceramics can include, for example, oxides, carbides, nitrides, or mixed compounds, especially aluminum oxide.
  • Other advantageous materials include sapphire, ruby, or diamond, or metals, especially hardened metals.
  • barium sulfate is produced by neutralizing barium hydroxide with sulfuric acid.
  • nozzle spacing 16 mm, 1.2 mm nozzle
  • the reactant dispersion can be pumped through the reactor chamber which does not taper towards the outlet opening.
  • Another exemplary process for preparing a low-viscosity aqueous barium sulfate dispersion at room temperature comprises the following steps a) Providing a barium salt solution (halide, nitrate, or carboxylate). b) Providing an alkali sulfate solution. c) Providing at least one comb polymer having a specific charge of -10 C/g to -500 C/g at pH 8. d) Mixing the barium salt solution from step a) with the comb polymer from step c) in an amount of preferably 0.5 to 20%, preferably 1 to 10%, and most preferably 3 to 8%, relative to the solid product.
  • nanoscale barium sulfate particles with a diameter of 90 nm are obtained at 30 bar nozzle pressure.
  • the particle size is significantly larger at 162 nm without using the device according to the invention while maintaining the remaining reaction conditions.
  • Calcium hydroxide was produced in a 12 mm diameter reactor chamber. Screw-in nozzles with 0.2 mm ruby bores were used for stoichiometric conversion. Stoichiometric processing of a 6.7% sodium hydroxide solution against a calcium nitrate solution in the presence of a polymer stabilizer resulted in stable calcium hydroxide dispersions with a particle size of 175 nm (polydispersity index: 0.161). Surprisingly, the resulting particle size was significantly smaller than without the device according to the invention (411.3 nm, polydispersity index: 0.356) or when using a reactor with a non-adjustable reactor geometry (178.9 nm, polydispersity index: 0.168).
  • Another example concerns the production of CAH. It takes place in a reactor chamber with a 16 mm diameter. Screw-in nozzles with 0.9 mm ruby bores were used for stoichiometric conversion. Stoichiometric processing of a sodium aluminate solution against a calcium nitrate solution in the presence of a polymer stabilizer (process pressure 25 bar) resulted in stable CAH dispersions. Surprisingly, continuous in-line processing in an additional reactor chamber (16 mm chamber diameter, 1.9 mm screw-in nozzles) results in a low-viscosity dispersion without gel-like agglomerates, which is storable for at least 6 months. Production in a stirred tank without processing through a reactor chamber yields a gel-like product with gel particles >2 mm, which is no longer pumpable after 24 hours.
  • the reactor chamber does not become clogged by the gel-like products.
  • the reactor chamber does not taper towards the outlet opening, which prevents pressure increase due to deposition of the gel-like product and clogging of the reactor chamber.
  • Fig. 1 shows a cross section of the device according to the invention
  • Fig. 2 is a plan view of the device of Fig. 1,
  • Fig. 3 is a further cross-section of the device from Fig.1,
  • Fig. 4 is a cross-section of another device according to the invention
  • Fig. 5 is a cross-section of another device according to the invention
  • Fig. 6 is a cross-section of another device according to the invention.
  • Fig. 7 is a cross-section of another device according to the invention.
  • Figures 1 to 3 depict a device 1 for conducting chemical and physical processes.
  • the device comprises at least two nozzles 2 and 3, each arranged in a nozzle holder 9.
  • the at least two nozzles 2 and 3, together with their respective nozzle holders 9, can be screwed into a reactor housing 4.
  • the reactor housing 4 comprises a first element 10 and a second element 11.
  • the first element 10 encloses a reactor chamber 5 within its interior and is inserted into the second element 11.
  • the collision point of the at least two nozzles 2 and 3 is located in the reactor chamber 5.
  • the second element has means for screwing in the nozzle holders 9 in the form of internal threads.
  • the first element 10 can be exchanged for a different first element 10 with a different cross-section of the reactor chamber 5.
  • the first element 10 can have a reactor chamber 5 with a diameter of 5 to 20 mm.
  • the first element 10 is secured and adjusted in the second element 11 by a positive fit with the front end of the nozzle holder 9.
  • the nozzle spacing varies according to the diameter of the reactor chamber 5.
  • the first element 10 and the second element 11 of the reactor housing 4 can be connected by the at least two nozzle holders 9.
  • the adjustment of the first element 10 in the second element 11 is carried out via the nozzle holders 9.
  • the at least two nozzle holders 9 are screwed through the second element 11 into the first element 10.
  • the adjustment of the reactor housing 4 is achieved by screwing in at least two nozzle holders 9, as their front area adjusts the reactor housing 4 through positive engagement. A complex adjustment of the reactor housing 4 after replacing the first element 10 is eliminated.
  • the at least two nozzles 2 and 3 are each provided with an associated pump and supply line (not shown) for spraying a liquid medium into the reactor chamber 5 enclosed by the reactor housing 4, directed towards a common collision point.
  • the reactor housing 4 has an inlet opening 6 through which a gas, a vaporized liquid, a cooling liquid, or a cooling gas can be introduced to maintain the gas atmosphere inside the reactor, particularly at the collision point of the liquid jets, or to cool the resulting products.
  • a reactant can also be introduced through the inlet opening.
  • the reactor housing 4 has an outlet opening 7 for removing the resulting products and excess gas from the reactor housing 4.
  • the reactor chamber 5 enclosed by the reactor housing 4 does not taper towards the outlet opening 7 for removing the resulting products and excess gas from the reactor housing 4.
  • Figure 4 shows a schematic representation of another device 1 according to the invention.
  • the reactants are sprayed through at least two nozzles 2 and 3 onto a collision point in the reactor chamber 5.
  • the device has additional means 8 to assist in the discharge of reaction products from the reactor chamber 5.
  • the additional means 8 are blade stirrers driven by a drive.
  • the additional means 8 discharge the reaction products from the outlet opening 7 (illustrated by arrows).
  • Figure 5 shows a schematic representation of another embodiment of the invention Device 1 is shown.
  • the reactants are sprayed through at least two nozzles 2 and 3 onto a collision point in the reactor chamber 5.
  • the device has additional means 8 to assist in the discharge of reaction products from the reactor chamber 5.
  • the additional means 8 are a rotor driven by a drive.
  • the additional means 8 discharge the reaction products from the outlet opening 7 (illustrated with arrows).
  • Figure 6 shows a schematic representation of a further device 1 according to the invention.
  • the reactants are sprayed through the at least two nozzles 2, 3 onto a collision point in the reactor chamber 5 enclosed by the reactor housing 4.
  • the reaction products are discharged from the outlet opening 7.
  • the device has a sleeve 15 that can be inserted into the reactor housing 4.
  • the sleeve 15 comprises a seal 16 for sealing an inlet opening 6 of the reactor housing 4.
  • the inlet opening 5 can be closed by a cap and the seal 16.
  • the sleeve 15 can be inserted through the inlet opening 6 into the reactor housing 4 and detachably connected to the reactor housing 4 by this cap.
  • the sleeve 15 can be changed particularly easily. By using different thicknesses of the sleeve 15, the cross-section of the reactor chamber 5 can be changed accordingly.
  • Figure 7 shows a representation of another device 1 according to the invention.
  • the reactants are sprayed through at least two nozzles 2 and 3 onto a collision point in the reactor chamber 5.
  • the reactor housing 4 has an inlet opening 5 closed with a cap.
  • the device has additional means 8 to assist in the discharge of reaction products from the reactor chamber 5.
  • the additional means 8 are a stirred tank driven by a drive.
  • the additional means 8 discharge the reaction products from the outlet opening 7.
  • the device 1 can be used to produce CAH according to embodiment 4.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne un dispositif pour réaliser des processus chimiques et physiques, au moins deux buses étant prévues, les buses ayant chacune une pompe et une conduite d'alimentation associées pour injecter un milieu liquide, au niveau d'un point de collision commun, dans une chambre de réacteur entourée par un boîtier de réacteur, une ouverture de sortie étant disposée pour éliminer les produits résultants et l'excès de gaz du boîtier de réacteur. Dans le contexte de l'invention, la chambre de réacteur entourée par le boîtier de réacteur n'est pas effilée dans la direction de l'ouverture de sortie pour éliminer les produits résultants et l'excès de gaz du boîtier de réacteur. Avantageusement, un dépôt de matériau sur la paroi interne du boîtier de réacteur peut être réduit au minimum.
PCT/DE2025/100161 2024-02-23 2025-02-12 Dispositif pour la réalisation de processus chimiques et physiques Pending WO2025176256A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102024105193.0A DE102024105193A1 (de) 2024-02-23 2024-02-23 Vorrichtung zur Durchführung chemischer und physikalischer Prozesse
DE102024105193.0 2024-02-23

Publications (1)

Publication Number Publication Date
WO2025176256A1 true WO2025176256A1 (fr) 2025-08-28

Family

ID=94772122

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE2025/100161 Pending WO2025176256A1 (fr) 2024-02-23 2025-02-12 Dispositif pour la réalisation de processus chimiques et physiques

Country Status (2)

Country Link
DE (1) DE102024105193A1 (fr)
WO (1) WO2025176256A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000061275A2 (fr) 1999-04-08 2000-10-19 Bernd Penth Procede et dispositif pour la realisation de processus chimiques et physiques
DE10141054A1 (de) 2001-08-22 2003-03-06 Bernd Penth Strahlreaktor und dessen Justierung
DE10249747A1 (de) 2002-10-25 2004-05-06 Clariant Gmbh Verfahren und Vorrichtung zur Durchführung chemischer und physikalischer Prozesse
DE102007008876A1 (de) 2006-02-21 2007-12-27 Sachtleben Chemie Gmbh Verfahren zur Durchführung chemischer und physikalischer Prozesse und Reaktionszelle

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000061275A2 (fr) 1999-04-08 2000-10-19 Bernd Penth Procede et dispositif pour la realisation de processus chimiques et physiques
DE10141054A1 (de) 2001-08-22 2003-03-06 Bernd Penth Strahlreaktor und dessen Justierung
DE10249747A1 (de) 2002-10-25 2004-05-06 Clariant Gmbh Verfahren und Vorrichtung zur Durchführung chemischer und physikalischer Prozesse
DE102007008876A1 (de) 2006-02-21 2007-12-27 Sachtleben Chemie Gmbh Verfahren zur Durchführung chemischer und physikalischer Prozesse und Reaktionszelle

Also Published As

Publication number Publication date
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