Reaction system, and method for performing chemical reactions in a liquid phase

Abstract

The present invention relates to a reaction system which is designed to perform chemical reactions in a liquid phase, in particular with the removal of a reaction substance, e.g. a reaction gas, without material losses caused by mechanical stirring devices, said reaction system comprising: a reaction vessel (1) having an upper region (1A) and a lower region B; and a circulation line arrangement (2) having at least one pump device (3), wherein the circulation line arrangement (2) comprises at least one fluid supply line part (4), which enters the reaction vessel (1) and has at least one outlet nozzle (5), and a fluid discharge line part (6), which exits the reaction vessel (1) in the lower region (1B) of the reaction vessel (1), wherein the at least one pump device (3) fluidically connects the at least one fluid supply line part (4) and the fluid discharge line part (6) outside the reaction vessel (1), wherein the at least one outlet nozzle (5) is oriented such that, in a circulation operation of the reaction system, a fluid exiting from the outlet nozzle sets the fluid present in the reaction vessel (1) into motion relative to a vertical axis of the reaction vessel (1). The present invention also relates to a method for performing chemical reactions in a liquid phase by means of the aforementioned reaction system.

Description

[0001] Reaction system and method for carrying out chemical reactions in the liquid phase The invention relates to a reaction system for carrying out chemical reactions in the liquid phase and to methods for carrying out chemical reactions in the liquid phase using the reaction system. Applications of the invention are in chemical process engineering and / or the production of chemical compounds. A variety of reaction systems or reactors for carrying out chemical reactions in the liquid phase, in particular those involving gas evolution during the reaction, are generally known in the prior art. The type of reaction system most commonly used in industry utilizes reaction vessels with a mechanical agitator mounted in an upper region of the reaction vessel, which causes mechanical mixing of the reaction vessel contents. Furthermore, the mechanical agitator also enables efficient heat supply to and removal from the reaction vessel, since the stirring ensures intensive contact between the reaction vessel contents and the reaction vessel walls. The reaction vessel is usually equipped with a double wall, into the cavity of which a cooling or heating medium is conducted for heat exchange.However, this type of reaction system has disadvantages for certain applications. A mechanical agitator has an agitator shaft that must be guided from above through the reaction vessel wall in a sealed manner. For sealing purposes, devices such as stuffing boxes are used in a conventional manner, in which a sealant is usually used to ensure tightness during operation. However, during longer operating times of such a reaction system – particularly under demanding reaction conditions, e.g., with regard to pressure, temperature, and aggressive reaction media – sealant can leak downwards into the reaction vessel, which can contaminate the contents of the reaction vessel. This is particularly the case with chemical reactions, e.g.This can be particularly problematic in the pharmaceutical sector, where very high levels of reaction product purity are essential, or in other areas as well. On the other hand, leakage of the sealant and / or general wear of the stuffing box can cause any reaction gas or solvent vapors to escape from the reaction vessel and contaminate the system's surroundings. This can lead to economic loss if the reaction gas has commercial value and is to be recovered as a reaction (by-)product, and can also pose a risk to personnel in the vicinity of the reaction system if the reaction gas or solvent is harmful to health. Against this background, it is an object of the present invention to provide a reaction system and a method for carrying out chemical reactions in the liquid phase, with which the disadvantages of the prior art can be avoided or significantly reduced. The invention is intended, in particular, to avoid limitations and problems of mechanical agitators. This object is achieved according to the invention by providing the reaction system according to claim 1 and the method according to claim 18. Preferred embodiments of the invention are the subject of the dependent claims. Description of the Invention The present inventors have found that the aforementioned disadvantages of the prior art can be avoided if, instead of a mechanical agitator on a reaction vessel for mixing the reaction vessel contents and for heat exchange, a reaction system with a circulation line device is used.by which a fluid present in the reaction vessel is set into motion, such as a rotational movement, a circulation, a swirling, a laminar or turbulent flow, or a combination or subcombination thereof, preferably relative to a vertical axis, in particular a vertical central axis, of the reaction vessel. Advantageously, the circulation line device generates a movement of the reaction vessel contents that acts essentially correspondingly to the movement generated by a mechanical agitator. In particular, the present invention provides a reaction system designed to carry out chemical reactions in the liquid phase, in particular with a reaction substance removal, e.g. reaction gas removal, without substance losses, e.g. gas losses, by mechanical agitators, comprising: a reaction vessel with an upper region and a lower region,and a circulation line device with at least one pumping device, wherein the circulation line device comprises at least one fluid supply line part which enters the reaction vessel and has at least one outlet nozzle, and a fluid discharge line part (in particular as a reaction substance discharge) which exits the reaction vessel in the lower region of the reaction vessel, wherein the at least one pumping device fluidly connects the at least one fluid supply line part and the fluid discharge line part outside the reaction vessel, wherein the at least one outlet nozzle is oriented such thatthat a fluid flowing out of it, during circulation operation of the reaction system, sets the fluid present in the reaction vessel in motion relative to the vertical axis of the reaction vessel. Furthermore, the present invention provides a method for carrying out chemical reactions in the liquid phase by means of a reaction system according to the invention, the method comprising: introducing at least one liquid reactant, optionally at least one solid reactant, and optionally at least one solvent into the reaction vessel, and carrying out at least one reaction in the reaction vessel, wherein, during circulation operation of the reaction system, the fluid present in the reaction vessel is set in motion around the vertical axis of the reaction vessel. The outlet nozzle is generally an opening of the fluid supply line part,preferably at its downstream end in the reaction vessel. Preferably, the at least one outlet nozzle can be arranged in the lower region of the reaction vessel. The outlet nozzle can be formed by the end of a pipe of the fluid supply line part or by a narrowed opening at the end of the fluid supply line part. According to a preferred embodiment of the invention, the at least one outlet nozzle can be oriented horizontally. This advantageously supports the movement of the reaction vessel contents around the vertical axis. Preferably, the reaction vessel does not have a mechanical stirring device. This advantageously eliminates any disadvantages of mechanical stirring devices. According to a further preferred embodiment of the invention, the fluid supply line part can be arranged outside the reaction vessel.wherein an end section of the fluid supply line part with the at least one outlet nozzle is introduced into the reaction vessel. This advantageously simplifies maintenance of the fluid supply line part and optimally utilizes the volume of the reaction vessel. Alternatively, a front section of the fluid supply line part can be introduced into the reaction vessel, with the remaining fluid supply line part entering the reaction vessel and being arranged within the reaction vessel. This embodiment has the advantage that the fluid supply line part can contribute to the temperature control of the reaction vessel contents. According to a further preferred embodiment of the invention, it can be provided that the reaction vessel does not have a heating and / or cooling jacket, ie, in particular, a wall of the reaction vessel is free of heating and / or cooling devices that contribute to the active,for targeted temperature control of the reaction vessel with a locally acting temperature control agent. This allows the design effort of the reaction vessel to be significantly reduced, which also allows a cost reduction. Advantageously, according to a further preferred embodiment of the invention, the circulation line device outside the reaction vessel can comprise a heat exchanger with which the circulated fluid can be heated or cooled. The heat exchanger has the advantage that a targeted influencing and / or adjustment of a reaction temperature in the reaction vessel is enabled or improved. According to a further preferred embodiment of the invention, the circulation line device outside the reaction vessel can comprise a drain line,through which the reaction vessel can be emptied. This advantageously promotes continuous operation of the reaction system, for example in a production process. Preferably, the reaction vessel can comprise, in the upper region, supply devices for at least one of at least one solvent, at least one liquid reactant, and at least one solid reactant, wherein the supply device for the at least one solid reactant can particularly preferably be sealed in a gas-tight manner. The supply devices offer advantages in feeding the reaction system without environmental influences impairing the reaction taking place in the reaction vessel. According to a further preferred embodiment of the invention, the reaction vessel can comprise, in the upper region, a discharge line for gases (in particular as a further part of the reaction substance discharge).whereby the functionality and safety of the reaction system is advantageously expanded or improved. Advantageously, according to a further preferred embodiment of the invention, the discharge line for gases can be connected downstream to a separation device with which liquid components, in which solid components may be dissolved, can be separated from a gas. The separation device offers the advantage that any unintentionally transported components of the reaction vessel contents can be retained. For this purpose, the separation device can particularly preferably be connected to the reaction vessel via a line through which liquid components, in which solid components may be dissolved and which have been separated from the gas,can be returned to the reaction vessel. This can advantageously improve the substance yield. According to further preferred embodiments of the invention, the reaction system can be equipped with at least one sensor device configured to measure at least one of a temperature, a flow rate, a fluid level, and a pH value. Advantageously, the at least one sensor device allows the detection of at least one operating state of the reaction system. Furthermore, the at least one sensor device allows the provision of at least one control loop for controlling the reaction system, in which, for example, an adjustment of the circulation line device is provided depending on an output signal from a temperature sensor and / or a level sensor. Preferably, the fluid supply line section can have two or more outlet nozzles.which are particularly preferably distributed throughout the reaction vessel. The outlet nozzles can be arranged at the same height or at different heights in the reaction vessel. Alternatively or additionally, the outlet nozzles can be arranged on opposite sides of the interior of the reaction vessel. Brief Description of the Drawings Further details and advantages of the invention are described below with reference to the attached drawings. Figure 1 shows a reaction system according to a first embodiment of the present invention, and Figure 2 shows a reaction system according to a second embodiment of the present invention. The embodiments and examples given below serve merely to illustrate the invention and are not to be construed as limiting. First Embodiment Figure 1 shows a reaction system according to a first embodiment of the present invention. According to Figure 1, the reaction system according to the first embodiment comprises a reaction vessel 1 with an upper region 1A and a lower region 1B. The design and size of the reaction vessel 1 are not specifically limited, and conventional, e.g. generally cylindrical, reaction vessels made of, for example, metal, ceramic, glass, plastic, and / or composite material can be used. The reaction vessel can be made of a single material or of multiple materials. Multiple materials can, for example, form a layered composite. Particularly suitable metals, ceramics, glasses, plastics, and composite materials are known to those skilled in the art, e.g.Stainless steel, enamel, or borosilicate glass or quartz glass. The material is selected, for example, to provide the reaction vessel with sufficient mechanical stability and / or to protect it against aggressive substances. The internal volume of reaction vessel 1 can be up to 300 m³, for example. 3 , preferably from 5 liters to 200 m 3 , more preferably 50 liters to 100 m 3 , even more preferably 200 liters to 50 m 3 and especially 500 liters to 10 m 3 However, the internal volume can also be less than 5 liters or more than 300 m 3The terms “upper region 1A” and “lower region 1B” are not subject to any particular restriction and merely serve as a vertical orientation when describing the reaction vessel 1. For example, the upper region 1A, vertically from top to bottom, can comprise 50%, 60%, 70% or 80% of the vessel height, with the remainder of the vessel height, i.e. 50%, 40%, 30% or 20%, being taken up by the lower region 1B.The reaction system according to the first embodiment further comprises a circulation line device 2 with at least one pump device 3, wherein the circulation line device 2 comprises at least one fluid supply line part 4, which is arranged outside the reaction vessel 1 and enters the reaction vessel 1 and ends with at least one outlet nozzle 5, and a fluid discharge line part 6, which exits the reaction vessel 1 in the lower region B of the reaction vessel 1, wherein the at least one pump device 3 fluidly connects the at least one fluid supply line part 4 and the fluid discharge line part 6 outside the reaction vessel 1. The pump device 3 can be any pump known in the art with a suitable delivery capacity, such as a centrifugal pump or a piston pump, which is selected depending on the viscosity of the reaction fluid.The fluid supply line part 4, the outlet nozzle 5 and the fluid discharge line part 6 can be made of, for example, metal, ceramic, glass, plastic and / or composite material. Particularly suitable metals, ceramics, glasses, plastics and composite materials are known to those skilled in the art, e.g. stainless steel or borosilicate glass or quartz glass. The specific configuration of the arrangement of these components is not particularly limited and can be selected depending on the dimensions and design of the entire system, as is known to those skilled in the art. Specific to the first embodiment is that the fluid supply line part 4 is arranged on the outside of the reaction vessel 1 and enters the reaction vessel 1, ie, passes through it into the interior of the reaction vessel 1.The inlet height is not specifically defined and, depending on the intended fill level of the reaction vessel 1, can be located either in the upper region 1A or, preferably, in the lower region 1B, as defined above. The number of fluid supply line sections 4 and outlet nozzles 5 is not specifically limited and can each be one or at least two, such as two, three, four, five, or more. With only one fluid supply line section 4, this can enter the reaction vessel 1 laterally and end as or with an outlet nozzle 5 inside the reaction vessel 1. However, one fluid supply line section 4 can also end with at least two outlet nozzles 5 inside the reaction vessel 1, optionally at different heights.Alternatively, the fluid supply line section 4 can run outside the reaction vessel 1, and two or more branches thereof can enter the reaction vessel 1 laterally at different heights, each ending with at least one outlet nozzle 5 inside the reaction vessel. Finally, in a further alternative, two or more fluid supply line sections 4 can run outside the reaction vessel 1, and one branch thereof can enter the reaction vessel 1 laterally at the same or different heights, each ending with at least one outlet nozzle 5 inside the reaction vessel. The fluid discharge line section 6 serves to discharge the reaction fluid from the reaction vessel 1 for the purpose of circulation, on the one hand, and to empty the reaction vessel 1 after the reaction has ended, on the other hand.Preferably, at least a portion of the inlet opening of the fluid discharge line part 6 is located in the lower region B at the lowest point of the interior of the reaction vessel 1 in order to enable the reaction vessel 1 to be emptied as completely as possible. According to the present invention, the at least one outlet nozzle 5 is oriented such that a fluid flowing out of it, during circulation operation of the reaction system, sets the fluid present in the reaction vessel 1 in motion around the vertical axis of the reaction vessel 1. The orientation of the outlet nozzle 5 is preferably such that it branches off horizontally from the fluid supply line part 4 in the interior of the reaction vessel. The term "horizontal" with regard to the orientation of the outlet nozzle 5 is to be understood according to the present disclosure as including not only exactly horizontal (perpendicular to the direction of gravity), but also a deviation from + (ie(i.e., upwards) 45° to - (i.e., downwards) 45°, +35° to -35°, +25° to -25°, +15° to -15°, +15° to -15°, +10° to -10°, +5° to -5° or +3° to -3°. If there is more than one outlet nozzle 5, these can all have the same orientation or different orientations relative to the horizontal. In a preferred embodiment, the deviation from the horizontal is as small as possible, including 0. Furthermore, with a plurality of outlet nozzles 5, the orientation is not restricted to a same outflow direction, but can also be opposite. I.e., for example, two outlet nozzles 5 allow the fluid to flow out clockwise in a plan view, while two further outlet nozzles 5 allow the fluid to flow out counterclockwise, etc.The orientation of the horizontal (as defined above) outlet nozzle 5 preferably does not run exactly radially to the center of the reaction vessel 1, since otherwise the desired movement of the reaction fluid in the reaction vessel 1 may not be achieved. Rather, the orientation of the horizontal outlet nozzle 5 deviates from the radial direction by at least 10°, at least 20°, at least 30°, at least 40°, at least 50°, at least 60°, at least 70°, and at least 80° to 90°. 90° is also intended to include the case in which the outlet nozzle 5 extends along the wall of, for example, a cylindrical vessel, i.e., follows the curvature of the same. The at least one outlet nozzle can thus be oriented radially to the vessel center or tangentially to the vessel wall, or in a direction between these extremes. Finally, if two or more outlet nozzles 5 are present, they can be arranged at the same height or at different heights.In a preferred embodiment, the circulation line device 2 outside the reaction vessel 1 comprises a heat exchanger 7, with which the circulated fluid can be heated or cooled. This is preferred if the respective reaction taking place in the reaction vessel 1 requires cooling or heating in order to proceed effectively. Suitable heat exchangers, their design principles, and operating media are known to a person skilled in the art, and these can be selected as appropriate for the application. In a preferred embodiment, the circulation line device 2 outside the reaction vessel comprises a drain line 8 through which the reaction vessel can be drained. The drain line 8 can, for example, branch off from a connecting line between the pump device 3 and the heat exchanger 7, as shown in Fig.1, but can also be arranged at any other suitable location within the circulation line device 2. Furthermore, the reaction vessel 1 can comprise, in the upper region 1A, feed devices 9A, 9B, 9C for at least one of at least one solvent, at least one liquid reactant, and at least one solid reactant, wherein the feed device 9C for at least one solid reactant can preferably be closed in a gas-tight manner. Corresponding feed devices, their design principles, and arrangement are known per se and will not be explained in more detail here. In a preferred embodiment, the reaction vessel 1 further comprises, in the upper region A, a discharge line 10 for gases. This is necessary for reactions in which gases are produced which either have to be discharged and disposed of as harmful gases or can be isolated and used as commercially usable gases.In a preferred embodiment, the gas discharge line 10 is connected downstream to a separation device 11, with which liquid components, in which solid components may be dissolved, can be separated from a gas. Suitable separation devices 11 are known to those skilled in the art, such as cyclones. In a further preferred embodiment, the separation device 11 is connected to the reaction vessel 1 by a line 12, through which the liquid components, in which solid components may be dissolved and which have been separated from the gas, can be returned to the reaction vessel 1. Furthermore, the reaction system can further comprise at least one sensor device (not shown in Fig. 1), which is designed, for example, to measure at least one of a temperature, a flow rate, a fluid level, and a pH value.Such sensor devices, their arrangement and operation for controlling a reaction system are known to those skilled in the art and will not be explained in detail here. According to the first embodiment explained above, reactions can be carried out in the same way as in a reaction vessel with a mechanical stirrer, but without having the disadvantages explained above. Second Embodiment Fig. 2 shows a reaction system according to a second embodiment of the present invention. According to Fig. 2, the reaction system according to the second embodiment differs from that of the first embodiment only in that the fluid supply line part 4 enters the reaction vessel 1 in the upper region 1A and runs within the reaction vessel 1.The other components and arrangements of the components of the second embodiment are identical to those in the first embodiment, and the relevant description applies here accordingly. According to the specific arrangement of the fluid supply line part 4 in the second embodiment, the outlet nozzle(s) 5 branch off from the fluid supply line part 4 inside the reaction vessel 1. Because the fluid supply line part 4 is located inside the reaction vessel 1, comparatively greater turbulence occurs during the movement of the fluid present in the reaction vessel 1 than in the case where the fluid supply line part 4 is not located inside the reaction vessel 1 (cf. the first embodiment). As a further advantage, better mixing of the components of the fluid can be achieved at the same movement speed of the fluid.Third Embodiment According to a third embodiment of the present invention, a method for carrying out chemical reactions in the liquid phase by means of a reaction system according to the invention, preferably according to one of the preceding embodiments, is provided, wherein the method comprises: introducing at least one liquid reactant, optionally at least one solid reactant and optionally at least one solvent into the reaction vessel 1, and carrying out at least one reaction in the reaction vessel 1, wherein in a circulation mode of the reaction system, the fluid present in the reaction vessel 1 is set in motion around the vertical central axis of the reaction vessel 1. The method as such is not subject to any restriction, except for its implementation in a reaction system according to the invention, and the person skilled in the art can, in the usual way, make suitable settings for reaction parameters, such as, for example,Pressure, temperature, addition rates of reactants, amounts / concentrations of reactants and optionally solvents, etc., in order to arrive at the desired products. Suitable examples for carrying out the process according to the invention are shown in Examples 1 and 2 below. In one embodiment of the present invention, the process comprises at least one chemical reaction in the liquid phase, selected from the group comprising KHCO3 + H3PO4^ KH2PO4 + H2O + CO2; K2CO3 + H3PO4 ^ K2HPO4 + H2O + CO2; 3 KHCO3 + H3PO4^ K3PO4 + 3 H2O + 3 CO2; (NH4)HCO3 + H3PO4^ (NH4)H2PO4 + H2O + CO2; 2 (NH4)HCO3 + H3PO4 ^ (NH4)2H2PO4 + 2 H2O + 2 CO2; K2CO3+ H3PO4^ K2HPO4+ H2O + CO2 / (NH4)HCO3+ H3PO4^ (NH4)H2PO4+ H2O + CO2; K2CO3+ 2 HCOOH ^ 2 K(HCOO) + H2O + CO2; K2CO3 + 2 CH3COOH ^ 2 CH3COOK + H2O + CO2; K2CO3+ H2SO4^ K2SO4+ H2O + CO2; K2CO3+ 2 HCl ^ 2 KCl + H2O + CO2 and K2CO3 + 2 HF ^ 2 KCl + H2O + CO2.The above chemical reactions are merely examples, and modified or other chemical reactions compatible with the present reaction system can be carried out using the present process. In particular, suitable chemical reactions include those in which reaction gases are produced which are to be disposed of or recovered, and in which foam development is particularly observed. The following examples are intended to illustrate processes that can be carried out using the present reaction system, although the invention is not limited to the specific parameters and process conditions of these embodiments. EXAMPLE 1 A reaction system according to the first embodiment explained above was used to carry out the reaction.In a 15-liter reaction vessel 1, potassium carbonate, ammonium bicarbonate, and phosphoric acid were reacted as follows to obtain an NPK fertilizer containing tripotassium phosphate and triammonium phosphate. a) In a first step of the process, the reaction vessel was filled with 9 liters of water (temperature 24.8 °C), and then 700 g of K2CO3 were mixed in while circulating the water. Vigorous foaming occurred, the temperature in the reaction vessel rose to 45.6 °C, and the pH reached 12.83. After this temperature rise, an endothermic reaction was used for cooling by first mixing in 664 g of NH4HCO3 while circulating. Vigorous foaming again occurred, the temperature in the reaction vessel fell to 40 °C, and the pH to 12.3. Then, 242 g of H3PO4 (78%) were added while stirring. The temperature continued to drop to 25.4 °C and the pH reached 9.78.b) In the next step of the process, 460 g of K2CO3 were mixed into the reaction mixture with circulation. Vigorous foaming occurred, the temperature in the reaction vessel rose to 38.0 °C, and the pH reached 12.5. Then, 322 g of H3PO4 (78%) were added with circulation. The temperature fell again to 32.8 °C, and the pH reached 9.98. Subsequent mixing in of a further 409 g of NH4HCO3 with circulation again led to vigorous foaming and a drop in temperature to 26.4 °C and a pH of 9.5. c) Now, 340 g of K2CO3 were mixed into the reaction mixture with circulation. Vigorous foaming occurred, the temperature in the reaction vessel rose to 30.9 °C, and the pH reached 9.8. Then, 436 g of H3PO4 (78%) were added while stirring. The temperature stabilized at 31.8 °C and the pH reached 8.9.Subsequent mixing in of another 247 g of NH4HCO3 with agitation again led to vigorous foaming and a temperature drop to 30.2 °C and a pH of 8.8. d) After a further addition of 611 g of H3PO4 (78%) with agitation, the temperature stabilized at 30.4 °C and the pH reached 8.5. e) Subsequently, 436 g of H3PO4 (78%) were added with agitation to essentially neutralize the reaction mixture, converting bicarbonate into carbonic acid and removing it from the reaction mixture as CO2. The temperature stabilized at 30.2 °C and the pH reached 7.04. The density of the resulting liquid NPK fertilizer mixture was 1.32 g / cm3. 3. The following Table 1 summarizes the essential reaction parameters of this exemplary embodiment for steps a) – d). Educts Total Order and amount (g) of addition amount (g) Water 9000 9000 K2CO3 1500 700 460 340 NH4HCO3 1320 664 409 247 H3PO4 1611 242 322 436 611 (78%) Step aaabbbcccd pH 7.26 12.83 12.3 9.78 12.5 9.98 9.5 9.8 8.9 8.8 8.5 Temperature 24.8 45.6 40 25.4 38 32.8 26.4 30.9 31.8 30.2 30.4 (°C) Table 1 EXAMPLE 2 To carry out the reaction, a reaction system according to the above explained second embodiment. In a reaction vessel 1 with a volume of 4 l, potassium carbonate, ammonium hydrogen carbonate, and phosphoric acid were reacted as follows to obtain an NPK fertilizer containing tripotassium phosphate and triammonium phosphate.a) In a first step of the process, the reaction vessel was filled with 0.7 l of water (temperature 22.4 °C) and 359 g of H3PO4 (78%), and then 62 g of K2CO3 were mixed in with circulation. Vigorous foaming occurred, and the temperature in the reaction vessel rose. After this temperature rise, an endothermic reaction was used for cooling by first mixing in 201 g of NH4HCO3 with circulation. Vigorous foaming again occurred, the temperature in the reaction vessel fell to 23.6 °C, and the pH rose to 4.7. b) In the next step of the process, 48 ​​g of K2CO3 were mixed into the reaction mixture with circulation. Vigorous foaming occurred, the temperature in the reaction vessel rose, and the pH increased further. Subsequent mixing of another 83 g of NH4HCO3 while agitating again led to vigorous foaming and a drop in temperature to 23.6 °C and a pH value of 8.1.c) 36.5 g of K2CO3 were then added to the reaction mixture with agitation. Vigorous foaming occurred, and the temperature in the reaction vessel and the pH increased. Subsequent mixing in of a further 168.7 g of NH4HCO3 with agitation again led to vigorous foaming and a drop in temperature to 23.6 °C and a pH of 8.5. d) 331 g of H3PO4 (78%) were then added with agitation to essentially neutralize the reaction mixture, convert bicarbonate into carbonic acid, and remove it from the reaction mixture as CO2. The temperature stabilized at 23.7 °C, and the pH reached 6.7. The density of the resulting liquid NPK fertilizer mixture was 1.32 g / cm3. 3. The following Table 2 summarizes the essential reaction parameters of this exemplary embodiment for steps a) – d). Educts Total Sequence and Amount (g) of Addition (g) Water 700 700 K2CO3 146.5 62 48 36.5 NH4HCO3 452.7 201 83 168.7 H3PO4 690 359 331 (78%) Step aaabbccd pH 4.7 8.1 8.5 6.7 Temperature 22.4 23.6 23.6 23.6 23.7 Water (°C) Table 2

[0002] List of reference symbols 1 Reaction vessel 1A Upper area 1B Lower area 2 Circulation line device 3 Pump device 4 Fluid supply line part 5 Outlet nozzle 6 Fluid discharge line part 7 Heat exchanger 8 Drain line 9A Supply device for at least one solvent 9B Supply device for at least one liquid reactant 9C Supply device for at least one solid reactant 10 Discharge line for gases 11 Separation device 12 Line

Claims

Claims 1. Reaction system which is designed to carry out chemical reactions in the liquid phase, in particular with a reaction substance removal without substance losses by mechanical stirring devices, comprising: a reaction vessel (1) with an upper region (1A) and a lower region (1B), and a circulation line device (2) with at least one pump device (3), wherein the circulation line device (2) comprises at least one fluid supply line part (4) which enters the reaction vessel (1) and has at least one outlet nozzle (5), and a fluid discharge line part (6) which exits the reaction vessel (1) in the lower region (1B) of the reaction vessel (1), wherein the at least one pump device (3) fluidly connects the at least one fluid supply line part (4) and the fluid discharge line part (6) outside the reaction vessel (1),wherein the at least one outlet nozzle (5) is oriented such that a fluid flowing out of it, during circulation operation of the reaction system, sets the fluid present in the reaction vessel (1) in motion relative to a vertical axis of the reaction vessel (1).

2. Reaction system according to claim 1, wherein the at least one outlet nozzle (5) is oriented horizontally.

3. Reaction system according to claim 1 or 2, wherein the reaction vessel (1) has no mechanical stirring device.

4. Reaction system according to one of claims 1 to 3, wherein the fluid supply line part (4) is arranged outside the reaction vessel (1), and an end section of the fluid supply line part (4) with the at least one outlet nozzle (5) is introduced into the reaction vessel (1).

5. Reaction system according to one of claims 1 to 3, wherein a front section of the fluid supply line part (4) is introduced into the reaction vessel (1) and the remaining fluid supply line part (4) is arranged within the reaction vessel (1).

6. Reaction system according to one of the preceding claims, wherein the reaction vessel (1) does not have a heating and / or cooling jacket.

7. Reaction system according to one of the preceding claims, wherein the circulation line device (2) outside the reaction vessel (1) comprises a heat exchanger (7) with which the circulated fluid can be heated or cooled.

8. Reaction system according to one of the preceding claims, wherein the circulation line device (2) outside the reaction vessel (1) comprises a drain line (8) through which the reaction vessel (1) can be drained. 9.Reaction system according to one of the preceding claims, wherein the reaction vessel (1) in the upper region (1A) comprises feed devices (9A, 9B, 9Cc) for at least one of at least one solvent, at least one liquid reactant, and at least one solid reactant.

10. Reaction system according to claim 9, wherein the feed device (9C) for at least one solid reactant can be closed in a gas-tight manner.

11. Reaction system according to one of the preceding claims, wherein the reaction vessel (1) in the upper region (1A) further comprises a discharge line (10) for gases.

12. Reaction system according to claim 11, wherein the discharge line (10) for gases is connected downstream to a separation device (11) with which liquid components, in which solid components are optionally dissolved, can be separated from a gas.Reaction system according to claim 12, wherein the separation device (11) is connected to the reaction vessel (1) by a line (12) through which the liquid components, in which solid components are optionally dissolved and which are separated from the. Gas that has been separated can be returned to the reaction vessel (1).

14. Reaction system according to one of the preceding claims, further comprising at least one sensor device configured to measure at least one of a temperature, a flow rate, a fluid level, and a pH value.

15. Reaction system according to one of the preceding claims, wherein the fluid supply line part (4) has two or more outlet nozzles (5).

16. Reaction system according to claim 15, wherein the outlet nozzles (5) are arranged at the same height in the reaction vessel (1).

17. Reaction system according to claim 15, wherein the outlet nozzles (5) are arranged at different heights in the reaction vessel (1).A method for carrying out chemical reactions in the liquid phase by means of a reaction system according to one of claims 1 to 17, the method comprising: introducing at least one liquid reactant, optionally at least one solid reactant and optionally at least one solvent into the reaction vessel (1), and carrying out at least one reaction in the reaction vessel (1), wherein in a circulation mode of the reaction system a fluid present in the reaction vessel (1) is set in motion relative to a vertical axis of the reaction vessel (1).

19. The method according to claim 18, wherein the at least one reaction in the liquid phase is selected from the group consisting of KHCO3 + H3PO4 ^ KH2PO4 + H2O + CO2; K2CO3 + H3PO4 ^ K2HPO4 + H2O + CO2; 3 KHCO3 + H3PO4 ^ K3PO4 + 3 H2O + 3 CO2;. (NH4)HCO3 + H3PO4 ^ (NH4)H2PO4 + H2O + CO2; 2 (NH4)HCO3 + H3PO4^ (NH4)2H2PO4 + 2 H2O + 2 CO2; K2CO3 + H3PO4^ K2HPO4 + H2O + CO2 / (NH4)HCO3 + H3PO4^ (NH4)H2PO4 + H2O + CO2; K2CO3 + 2 HCOOH ^ 2 K(HCOO) + H2O + CO2; K2CO3 + 2 CH3COOH ^ 2 CH3COOH + H2O + CO2; K2CO3 + H2SO4^ K2SO4 + H2O + CO2; K2CO3 + 2 HCl ^ 2 KCl + H2O + CO2; and K2CO3 + 2 HF ^ 2 KCl + H2O + CO2.

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