Device for carrying out chemical and physical processes

Abstract

The invention relates to a device for carrying out chemical and physical processes, at least two nozzles being provided, the nozzles each having an associated pump and supply line for injecting a liquid medium, at a common collision point, into a reactor chamber surrounded by a reactor housing, an outlet opening being provided for removing the resulting products and excess gas from the reactor housing. In the context of the invention, the reactor chamber surrounded 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. Advantageously, material settling on the inner wall of the reactor housing can be minimised.

Description

[0001] DESCRIPTION

[0002] Device for carrying out chemical and physical processes

[0003] 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.

[0004] The known methods and devices for conducting chemical and physical processes usually require specific boundary conditions tailored to the respective reaction. Meeting these boundary conditions over a wide range of values ​​is often not possible in the same device. Examples of such reactions include chemical reactions in microreactors between multi-component systems with excellent mixing and optimal yields, the initiation of physical and chemical processes by utilizing cavitation caused by the process, such as ceramization and the progression of chemical reactions at the collision point.

[0005] - Homogenization, dispersing, emulsification, sterilization and cell disruption and

[0006] - Micronization and coating.

[0007] WO 00 / 61275 A2 discloses a method for carrying out chemical and physical processes. To initiate chemical and physical processes, at least two liquid media are sprayed via pumps, preferably high-pressure pumps, through a nozzle each into a reactor chamber enclosed by a reactor housing onto a common collision point. A gas, a vaporized liquid, a cooling liquid, or a cooling gas is introduced into the reactor chamber through an opening to maintain the gas atmosphere inside the reactor, in particular at the collision point of the liquid jets, or to cool the resulting products. The resulting products and excess gas are removed from the reactor housing through a further opening by means of overpressure on the gas inlet side or by negative pressure on the product and gas outlet sides.

[0008] 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.

[0009] 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.

[0010] DE 10 2007 008 876 A1 describes a comparable method for carrying out chemical and physical processes, whereby the jets of all nozzles are aligned at an angle of between 10 and 170° to each other to avoid clogging of the nozzles.

[0011] A disadvantage of all these known devices and methods for conducting chemical and physical processes is that they usually have a fixed geometry, particularly with regard to the nozzle spacing and the nozzle and reactor cross-section. Especially at high flow rates, the interior of the reactor housing can become clogged with reactants and / or reaction products. Viscous products and / or reactants in particular can lead to suboptimal mixing and reactor clogging.

[0012] The object of the invention is to provide a method and a device to carry out chemical or physical processes with better results and at high flow rates in the same device.

[0013] The problem is solved in a device for carrying out chemical and physical processes according to the generic term in that the cross-section of the reactor chamber is variable.

[0014] In particular, the cross-section of the reactor chamber can be varied depending on the particular physical or chemical process to be performed with the device. Advantageously, the nozzle spacing can also be varied. For example, the cross-section of the reactor chamber can be from 5 to 20 mm, preferably from 12 to 16 mm.

[0015] The cross-section of the reactor chamber can be changed, for example, by replacing the reactor housing or a part of it. Thus, reactor housings with different cross-sections can be used in a device according to the invention, which are easily interchangeable, for example, by screwing them in and out. Advantageously, the same nozzles can be used for different reactor housings with different nozzle spacing. This allows a wide range of chemical and physical processes to be implemented in the same device.

[0016] Advantageously, all reaction products and excess gas can be discharged through the outlet opening without causing material buildup and thus an undesirable pressure increase in the reactor. In particular, material settling on the inner wall of the reactor housing can be minimized, thereby extending the device's maintenance and cleaning intervals. Undesirable edge effects with the inner walls of the reactor housing are prevented or reduced. A particularly advantageous feature is that the product quality is independent of the flow rate, and the pressure drop required for the physical and chemical processes can be maintained over a wide range of flow rates. This enables flow rates of over 600 l / h without clogging the interior of the reactor housing.

[0017] In this context, a further development of the invention consists in that the reactor housing has a first element and a second element, wherein the first element encloses a reactor chamber in its interior and is inserted into the second element, wherein the second element has means for screwing in nozzle holders in which the nozzles are located, in the form of internal threads, wherein the first element is interchangeable with another first element with a different cross-section of the reactor chamber.

[0018] One embodiment of the invention is that the device has a sleeve that can be detachably connected to the reactor housing, wherein the sleeve can be introduced into the reactor chamber, wherein the cross-section of the reactor chamber can be changed by the sleeve.

[0019] 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.

[0020] Advantageously, the thickness of the sleeve allows the cross-section of the reactor chamber to be easily modified. For example, by inserting a sleeve with a thicker wall, the cross-section of the reactor chamber and thus also the volume can be reduced.

[0021] The reactants and products primarily come into contact with the sleeve. Particularly advantageously, the sleeve can be made of polymers with low free surface energy, such as polytetrafluoroethylene (PTFE), silicone, perfluorocarbon rubber (FFKM), fluorocarbon rubber (FKM), or stainless steel. In particular, the sleeve can be coated with polytetrafluoroethylene or a polymer. The coating or the material of the sleeve can reduce the adhesion of material in the reactor chamber. Easy cleaning is possible by replacing the sleeve.

[0022] Advantageously, 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.

[0023] One embodiment of the invention is that the at least two nozzles can be screwed into the reactor housing.

[0024] The advantage is that at least two nozzles can be changed particularly quickly and easily.

[0025] It is advisable that the at least two nozzles have a nozzle diameter (inner diameter of the nozzle) of 50 pm to 3 mm.

[0026] A further embodiment of the invention consists in that an inlet opening is provided in the reactor housing.

[0027] For example, reactants can be introduced into the reactor chamber through the inlet opening in the reactor housing.

[0028] 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 cool the resulting products

[0029] However, it is also possible to insert a sleeve through the inlet opening to change the cross-section of the reactor housing.

[0030] Advantageously, the conversion of the reaction product and its comminution and / or the comminution of the reactants can take place simultaneously in the reaction chamber.

[0031] 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.

[0032] 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.

[0033] It is part of the invention that 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.

[0034] A further embodiment of the invention is that the device has three to eight, preferably four to six nozzles.

[0035] A further embodiment of the invention is that the reactor housing is adjustable by the at least two nozzle holders.

[0036] By screwing in the nozzle holders, the reactor housing automatically adjusts itself relative to the nozzle holders. Advantageously, the nozzles do not need to be aligned to a common collision point, eliminating the need for subsequent adjustment of the nozzles.

[0037] Furthermore, it can be provided that 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.

[0038] 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. Advantageously, 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.

[0039] Mechanical discharge means are also conceivable as 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.

[0040] A further embodiment of the invention is that the reactor chamber is cylindrically shaped.

[0041] The diameter of the cylindrical reactor chamber can be changed.

[0042] 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. One embodiment of the invention is that 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 second elements can be connected by the at least two nozzles.

[0043] Advantageously, 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.

[0044] It is also advantageous that 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.

[0045] The inlet means and the outlet means may comprise valves.

[0046] It is advisable that the inlet opening is aligned with the outlet opening.

[0047] 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.

[0048] The pumps can be selected according to the pressure requirements. For example, the pumps can be micro annular gear pumps, gear pumps, piston pumps, piston diaphragm pumps, or high-pressure pumps.

[0049] In high-pressure pumps, the pump pressure can be increased to 1,000 bar and the resulting increased impact velocity to such an extent that the hydrodynamic cavitation or kinetic energy occurring at the collision point when the jets collide is released for the course of physical and chemical reactions. Finally, according to the invention, the at least two nozzles are ceramic, stainless steel, or diamond nozzles.

[0050] 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.

[0051] In the following, the invention will be explained in more detail using exemplary embodiments.

[0052] In the exemplary embodiment, barium sulfate is produced by neutralizing barium hydroxide with sulfuric acid. In one example, a highly filled dispersion of barium hydroxide (5-70% w / w) in water (43.19 kg of barium hydroxide octahydrate in 12.32 kg of water) in the presence of a polymeric stabilizer (Melpers 0045, 8.63 kg) is neutralized with sulfuric acid (37%) in an advection chamber with an expanded reactor space (nozzle spacing = 16 mm, 1.2 mm nozzle). Surprisingly, it has been found that selecting an expanded reactor space allows the processing of even highly filled reactant dispersions. The resulting barium sulfate has a particle size of 180 nm and a PDI (polydispersity index) of <0.2.

[0053] Advantageously, the reactant dispersion can be pumped through the reactor chamber which does not taper towards the outlet opening.

[0054] Another exemplary process for producing 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. e) Precipitating barium sulfate by mixing liquid streams from steps b) and d) in flow through a reactor chamber with a diameter of 12 mm. Screw-in nozzles with 0.2 mm ruby ​​orifice stones were used for the reaction.

[0055] Using 10% comb polymer, nanoscale barium sulfate particles with a diameter of 90 nm are obtained at 30 bar nozzle pressure.

[0056] Surprisingly, the particle size is significantly larger at 162 nm without using the device according to the invention while maintaining the remaining reaction conditions.

[0057] Example 3

[0058] 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).

[0059] 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.

[0060] Advantageously, the reactor chamber does not become clogged by the gel-like products.

[0061] Advantageously, 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.

[0062] In the following, the invention is explained in more detail using exemplary embodiments.

[0063] It shows

[0064] Fig. 1 shows a cross section of the device according to the invention,

[0065] Fig. 2 is a plan view of the device of Fig. 1,

[0066] Fig. 3 is a further cross-section of the device from Fig.1,

[0067] Fig. 4 is a cross-section of a further device according to the invention, Fig. 5 is a cross-section of a further device according to the invention,

[0068] Fig. 6 is a cross-section of another device according to the invention,

[0069] Fig. 7 is a cross-section of another device according to the invention.

[0070] 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.

[0071] 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. Depending on the planned process, the first element 10 can be exchanged for a different first element 10 with a different cross-section of the reactor chamber 5.

[0072] In particular, 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.

[0073] The nozzle spacing changes 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 means of 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. For this purpose, the at least two nozzle holders 9 are screwed through the second element 11 into the first element 10. Advantageously, the adjustment of the reactor housing 4 is carried out by screwing in the at least two nozzle holders 9, in that their front area adjusts the reactor housing 4 through positive engagement. Complex adjustment of the reactor housing 4 after replacing the first element 10 is no longer necessary.

[0074] 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.

[0075] 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.

[0076] 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.

[0077] 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).

[0078] Figure 5 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 a rotor driven by a drive. The additional means 8 discharge the reaction products from the outlet opening 7 (illustrated by arrows).

[0079] 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. Advantageously, 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.

[0080] 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 for the production of CAH according to embodiment 4.

Claims

CLAIMS 1. Device (1) for carrying out chemical and physical processes, wherein at least two nozzles (2, 3), each with an associated pump and feed line, are provided for spraying a liquid medium into a reactor chamber (5) enclosed by a reactor housing (4) onto a common collision point, wherein an outlet opening (7) is provided for removing the resulting products and / or excess gas from the reactor housing (4), characterized in that the cross-section of the reactor chamber (5) is variable.

2. Device (1) according to claim 1, characterized in that the cross section of the reactor chamber (5) by replacing the reactor housing (4) is changeable.

3. Device (1) according to claim 2, characterized in that the reactor housing (4) comprises a first element (10) and a second element (11), wherein the first element (10) has in its interior a reactor space (5) and is inserted into the second element (11), wherein the second element (11) has means for screwing in (12) nozzle holders (9) in which the nozzles (2, 3) are located, in the form of internal threads, wherein the first element (10) is interchangeable with another first element (10) with a different cross-section of the reactor space (5).

4. Device (1) according to claim 1, characterized in that the device (1) has a sleeve (15) which can be detachably connected to the reactor housing (4), wherein the sleeve (15) can be introduced into the reactor space (5), wherein the cross section of the reactor space (5) can be changed by the sleeve (15).

5. Device (1) according to one of claims 1 to 4, characterized in that the at least two nozzles (2, 3) can be screwed into the reactor housing (4).

6. Device (1) according to one of the preceding claims, characterized in that the at least two nozzles (2, 3) have a nozzle diameter of 50 pm to 3 mm.

7. Device (1) according to one of the preceding claims, characterized in that an inlet opening (6) is provided in the reactor housing (4).

8. Device (1) according to claim 6, characterized in that reactants can be introduced via the inlet opening (6).

9. Device (1) according to one of the preceding claims, characterized in that the reactor space (5) enclosed by the reactor housing (4) does not taper in the direction of the outlet opening (7) for removing the resulting products and excess gas from the reactor housing (4).

10. Device (1) according to one of the preceding claims, characterized in that the flow through the outlet opening (7) is from 0.1 l / h to 5000 l / h, preferably from 1 l / h to 800 l / h.

11. Device (1) according to one of the preceding claims, characterized in that the device (1) has three to eight, preferably four to six nozzles.

12. Device (1) according to one of the preceding claims, characterized in that the reactor housing (4) is adjustable by the at least two nozzles (2, 3).

13. Device (1) according to one of the preceding claims, characterized in that the device has additional means (8), wherein the additional means (8) can be introduced into the reactor housing (4) and / or attached to the reactor housing (4).

14. Device (1) according to one of the preceding claims, characterized in that the reactor space (5) is cylindrically shaped.

15. Device (1) according to one of the preceding claims, characterized in that the at least two nozzles (2, 3) can be screwed into a nozzle holder (9), wherein the nozzle holders can be screwed into the reactor housing (4).

16. Device (1) according to one of the preceding claims, characterized in that the reactor housing (4) has two elements (10, 11), wherein a first element (10) encloses the reactor space (5) and can be inserted into a second element (11), wherein the second element (11) has means for holding (12) the device, wherein the first and the second element (10, 11) can be connected by the at least two nozzles (2, 3).

17. Device (1) according to one of the preceding claims, characterized in that inlet means (13) and outlet means (14) are provided, wherein the inlet means (13) and the inlet opening (6) and the outlet means (14) and the outlet opening (7) are detachably connectable.

18. Device (1) according to one of the preceding claims, characterized in that the inlet opening (6) is aligned with the outlet opening (7).

19. Device (1) according to one of the preceding claims, characterized in that a pressure of 0.5 to 1000 bar, preferably 10 to 100 bar, can be achieved by the pumps.

20. Device (1) according to one of the preceding claims, characterized in that the at least two nozzles (2, 3) are ceramic, stainless steel or diamond nozzles.

Images