A microinterface reactor and reaction process for continuous production of ferric chloride

Abstract

The present invention relates to the field of reactor technology, and in particular to a micro-interface reactor and a reaction process for continuous production of ferric chloride, comprising a reactor body, wherein the top of the reactor body is connected with an external air extraction pipe and an internal air extraction pipe, the ends of the external air extraction pipe and the internal air extraction pipe are connected with the input end of an external air extraction device, a micro-interface generator is arranged at the bottom of the reactor body, an air guide pipe is arranged on the inner wall of the reactor body, the air guide pipe is connected with the output end of the external air extraction device, a transmission component is arranged at the top of the reactor body, and a transmission rod is connected to the output end of the transmission component, gas enters the reactor body in the form of fine bubbles through the micro-interface generator at the bottom of the reactor body, the oxygen-enriched air entering the reactor body passes through and participates in the reaction of the electrolytic mother liquor in the reactor body, and the gas passing through the electrolytic mother liquor is re-sent to the micro-interface generator through the external air extraction device and the air guide pipe.

Description

Technical Field

[0001] The invention relates to the technical field of reactors, and in particular to a microinterface reactor and a reaction process for continuous production of ferric chloride. Background Art

[0002] Chinese patent publication number CN113235111B discloses a method of obtaining chlorine at the anode by electrolyzing ferric chloride without a diaphragm. The mother liquor containing ferrous chloride obtained after electrolysis is introduced into a mother liquor tank. At the same time, a mixed gas of by-product hydrogen chloride gas and oxygen-enriched air is introduced into the mother liquor tank for oxidation reaction to obtain ferric chloride electrolysis mother liquor, which is an important part of the process of producing chlorine using by-product nicotinic acid.

[0003] The reaction between ferrous chloride and oxygen after absorbing hydrogen chloride is a gas-liquid heterogeneous reaction. The solubility of oxygen in the mother liquor is not large. The reaction mainly takes place at the gas-liquid interface and is controlled by the mass transfer rate. The reactor currently used has the disadvantages of large volume, large oxygen-enriched air ventilation demand and high energy consumption in actual use. Therefore, a microinterface reactor and reaction process for continuous production of ferric chloride are proposed. Summary of the invention

[0004] In order to solve the technical problems existing in the above-mentioned prior art, the present invention provides a micro-interface reactor and a reaction process for continuous production of ferric chloride.

[0005] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a micro-interface reactor for continuous production of ferric chloride, comprising a reactor body, the top of the reactor body is connected with an external air extraction pipe and an internal air extraction pipe, the ends of the external air extraction pipe and the internal air extraction pipe are connected with the input end of an external air extraction device, a micro-interface generator is arranged at the bottom of the reactor body, an air guide pipe is arranged on the inner wall of the reactor body, the air guide pipe is connected with the output end of the external air extraction device, a transmission assembly is arranged at the top of the reactor body, the output end of the transmission assembly is connected with a transmission rod, and a plurality of groups of foam-breaking blades are arranged in the middle of the transmission rod;

[0006] The gas enters the reactor body in the form of tiny bubbles through the micro-interface generator at the bottom of the reactor body. The oxygen-rich air entering the reactor body passes through and participates in the reaction of the electrolytic mother liquor in the reactor body. The gas passing through the electrolytic mother liquor is collected by the external exhaust pipe and the internal exhaust pipe and is sent back to the micro-interface generator through the air duct through the external exhaust device.

[0007] Preferably, the outer exhaust pipe and the inner exhaust pipe are both annular in design, and are staggered up and down, the ends of the outer exhaust pipe and the inner exhaust pipe extend to the outside of the reactor body, and the ends of the outer exhaust pipe and the inner exhaust pipe are connected to external exhaust equipment.

[0008] Preferably, the foam-breaking paddle is located at the upper surface of the electrolytic mother liquid inside the reactor body, and the foam-breaking paddle blades are inclined.

[0009] Preferably, the method comprises the following steps:

[0010] Step A, preparing a secondary absorption tower, a primary absorption tower and a micro-interface reactor, connecting the secondary absorption tower, the primary absorption tower and the micro-interface reactor through a pipeline, injecting an electrolytic mother liquid into the secondary absorption tower and the primary absorption tower, and the electrolytic mother liquid absorbs hydrogen chloride in the industrial tail gas to form an electrolytic mother liquid containing hydrogen chloride;

[0011] Step B, the electrolytic mother liquid containing hydrogen chloride is poured into the reactor body, oxygen-enriched air is input into the reactor body, the oxygen-enriched air is broken into micron-sized bubbles by a micro-interface generator at the bottom of the reactor body, and then enters the reactor body, the bubbles pass through the electrolytic mother liquid containing hydrogen chloride, and in the reactor body, the ferrous chloride in the electrolytic mother liquid reacts with hydrogen chloride and the oxygen-enriched air to generate ferric chloride, and the content of ferric chloride in the electrolytic mother liquid increases as the reaction continues;

[0012] Step C, setting a reaction liquid self-circulation system outside the micro-interface reactor, the self-circulation system circulates the electrolytic mother liquid in the micro-interface reactor up and down and maintains the temperature during the circulation;

[0013] Step D, the electrolytic mother liquor containing ferric chloride is drawn out from the bypass pipeline of the circulation system and enters into the evaporation tank to obtain the ferric chloride solution of the required concentration for electrolysis.

[0014] Preferably, in step A, the secondary absorption tower and the primary absorption tower are arranged in parallel, the bottom end of the secondary absorption tower is connected to the primary absorption tower through a pipeline, a delivery pump is arranged in the middle of the pipeline, and the delivery pump cooperates with the pipeline to form a liquid delivery path from the bottom end of the secondary absorption tower to the top end of the primary absorption tower, and the electrolytic mother liquor entering the secondary absorption tower enters the primary absorption tower through the liquid delivery path.

[0015] Preferably, in step A, the top end of the primary absorption tower is connected to the lower end of the secondary absorption tower via a conduit, and the hydrogen chloride-containing tail gas entering the primary absorption tower enters the secondary absorption tower via the conduit.

[0016] Preferably, in step B, an air pump is connected to the bottom of the micro-interface reactor, and the air pump is connected to an external oxygen-enriched air supply device.

[0017] Preferably, in step B, the total flux of oxygen-enriched air entering the reactor body is 100%-300% of the theoretical consumption.

[0018] Preferably, in step C, the reaction liquid self-circulation system includes a heat exchanger and a circulation pump. The input and output ends of the heat exchanger are respectively connected to the upper and lower parts of the micro-interface reactor through pipes. A circulation pump is arranged between the pipe and the heat exchanger. The circulation pump extracts the electrolytic mother liquor from the upper part of the micro-interface reactor through the pipe. The extracted electrolytic mother liquor passes through the heat exchanger to maintain the temperature at 30-60°C and then re-enters the lower end of the micro-interface reactor.

[0019] Preferably, a group of evaporation tanks are connected between the circulation pump and the pipeline of the micro-interface reactor via a bypass pipeline.

[0020] Compared with the prior art, the present invention provides a microinterface reactor and reaction process for continuous production of ferric chloride, which has the following beneficial effects:

[0021] The present invention is provided with a micro-interface generator, and the bubbles entering the reactor body are broken into micron-sized bubbles by the reactor micro-interface generator and then enter the reactor body, and the bubbles pass through the electrolytic mother liquor containing hydrogen chloride. In the reactor body, the ferrous chloride in the electrolytic mother liquor reacts with hydrogen chloride and oxygen-enriched air to generate ferric chloride, and the surface area of ​​the bubbles is increased by generating micron-sized bubbles, thereby accelerating the reaction rate;

[0022] In the present invention, an external air extraction pipe and an internal air extraction pipe are connected to the top of the reactor body, and the ends of the external air extraction pipe and the internal air extraction pipe are both connected to an external air extraction device. After the oxygen-enriched air entering the reactor body passes through the hydrogen chloride-containing electrolytic mother liquid in the reactor body and floats to the top of the reactor body, the external air extraction device works to extract the oxygen-enriched air that continuously floats to the top of the reactor body through the external air extraction pipe and the internal air extraction pipe. The external air extraction device re-sends the oxygen-enriched air extracted from the top of the reactor body by the external air extraction pipe and the internal air extraction pipe to the micro-interface generator through the air guide pipe, so that the air is re-bubbled and participates in the reaction again, thereby improving the utilization rate of the oxygen-enriched air, reducing the waste of resources, and reducing the production cost.

[0023] In the present invention, a foam bursting paddle is provided, and the foam bursting paddle rotates synchronously under the drive of the transmission rod. During the rotation process, the foam bursting paddle continuously pushes the bubbles on the top of the liquid surface in the reactor body, accelerates the bursting of the bubbles and exposes the liquid surface, thereby ensuring that the bubbles are not restricted by the upper bubbles and burst quickly, thereby avoiding the generation of a large number of bubbles, and also preventing the bubbles from merging to form large bubbles and remaining in the reactor body for a long time. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation of the present invention. In the accompanying drawings:

[0025] Figure 1 It is a schematic diagram of the reaction process in the embodiment;

[0026] Figure 2 It is a schematic diagram of the three-dimensional structure of the micro-interface reactor in the embodiment;

[0027] Figure 3 It is a schematic cross-sectional view of the three-dimensional structure of the micro-interface reactor in the embodiment.

[0028] In the figure: 1. Secondary absorption tower; 2. Primary absorption tower; 3. Delivery pump; 4. Micro-interface reactor; 41. Reactor body; 42. External exhaust pipe; 43. Internal exhaust pipe; 44. Micro-interface generator; 45. Air guide pipe; 46. Transmission assembly; 47. Transmission rod; 48. Foam-breaking paddle; 5. Air pump; 6. Heat exchanger; 7. Circulation pump; 8. Evaporation tank. DETAILED DESCRIPTION

[0029] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. The components of the embodiments of the present invention generally described and shown in the drawings here can be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present invention provided in the drawings is not intended to limit the scope of the claimed invention, but merely represents the selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making creative work belong to the scope of protection of the present invention.

[0030] like Figure 1 - Figure 3 As shown, this embodiment proposes a reaction process for continuous production of ferric chloride using a microinterface reactor, comprising the following steps:

[0031] Step A, prepare a secondary absorption tower 1, a primary absorption tower 2 and a micro-interface reactor 4, connect the secondary absorption tower 1, the primary absorption tower 2 and the micro-interface reactor 4 through a pipeline, the secondary absorption tower 1 and the primary absorption tower 2 are arranged in parallel, the bottom end of the secondary absorption tower 1 is connected to the primary absorption tower 2 through a pipeline, a delivery pump 3 is arranged in the middle of the pipeline, the delivery pump 3 cooperates with the pipeline to form a liquid delivery path from the bottom end of the secondary absorption tower 1 to the top end of the primary absorption tower 2, inject the electrolyte mother solution into the secondary absorption tower 1, and enter the secondary absorption tower 1. The electrolytic mother liquid in the secondary absorption tower 1 enters the primary absorption tower 2 through the liquid transport path, the top of the primary absorption tower 2 is connected to the lower end of the secondary absorption tower 1 through a conduit, the tail gas containing hydrogen chloride is injected into the primary absorption tower 2 from the lower part of the primary absorption tower 2, the industrial tail gas containing hydrogen chloride entering the primary absorption tower 2 enters the secondary absorption tower 1 and the primary absorption tower 2 through the conduit, and the electrolytic mother liquid in the secondary absorption tower 1 and the primary absorption tower 2 absorbs the hydrogen chloride in the industrial tail gas to form the electrolytic mother liquid containing hydrogen chloride;

[0032] Step B, the electrolytic mother liquid containing hydrogen chloride is poured into the reactor body 41, the bottom end of the micro-interface reactor 4 is connected to an air pump 5, the air pump 5 is connected to an external oxygen-enriched air supply device, and oxygen-enriched air is input into the reactor body 41 through the air pump 5. The oxygen-enriched air is broken into micron-sized bubbles by the micro-interface generator 44 at the bottom of the reactor body 41 and then enters the reactor body 41. The bubbles pass through the electrolytic mother liquid containing hydrogen chloride. In the reactor body 41, the ferrous chloride in the electrolytic mother liquid reacts with hydrogen chloride and the oxygen-enriched air to generate ferric chloride. The content of ferric chloride in the electrolytic mother liquid increases as the reaction continues. The total flux of oxygen-enriched air entering the reactor body 41 is 100%-300% of the theoretical consumption, thereby ensuring that the amount of oxygen-enriched air introduced can make the ferrous chloride in the electrolytic mother liquid react completely with hydrogen chloride;

[0033] Step C, setting a reaction liquid self-circulation system outside the micro-interface reactor 4, the reaction liquid self-circulation system includes a heat exchanger 6 and a circulation pump 7, the input end and the output end of the heat exchanger 6 are respectively connected to the upper and lower parts of the micro-interface reactor 4 through pipelines, and a circulation pump 7 is arranged between the pipeline and the heat exchanger 6. The circulation pump 7 extracts the electrolytic mother liquid from the upper part of the micro-interface reactor 4 through the pipeline. The temperature of the extracted electrolytic mother liquid is maintained at 30-60° C. after passing through the heat exchanger 6, and re-enters the lower end of the micro-interface reactor 4;

[0034] A group of evaporation tanks 8 are connected between the circulation pump 7 and the pipeline of the micro-interface reactor 4 through a bypass pipeline. The evaporation tanks 8 remove water from the electrolysis mother solution by evaporation to obtain a high-concentration ferric chloride solution. The high-concentration ferric chloride solution is electrolyzed to obtain ferric chloride.

[0035] In step B, when the reaction is carried out for 10min, 15min, 20min and 50min, the electrolytic mother solution in the micro-interface reactor 4 is sampled, and the sampling volume is 100ml each time, and the conversion rate of ferrous chloride in the electrolytic mother solution in 100ml is checked;

[0036] A total of three experiments were conducted to obtain conversion data of Experimental Example 1, Experimental Example 2 and Experimental Example 3, respectively. Comparative Examples 1 and Comparative Examples 2 were set up for comparison. The difference between Comparative Examples 1, Experimental Example 2 and Experimental Example 3 is that in Comparative Examples 1 and Comparative Examples 2, the oxygen-enriched air introduced was not broken by the micro-interface generator 44. The data are summarized in Table 1 below:

[0037] Sampling time experimental group 1min 1.5min 2min 5min Experimental Example 1 77.2% 97.2% 98.1% / Experimental Example 2 76.8% 97.8% 98.3% 99.2% Experimental Example 3 73.4% 97.5% / / Comparative Example 1 0.8% 1.9% 3.2% / Comparative Example 2 0.7% 1.5% 2.9% 5.4%

[0038] Table 1, ferrous chloride conversion rate

[0039] A micro-interface reactor for continuous production of ferric chloride comprises a reactor body 41, a micro-interface generator 44 is arranged at the bottom of the reactor body 41, the micro-interface generator 44 disperses the oxygen-enriched air input into the reactor body 41 into micron-sized bubbles with a diameter of 10-200 microns, and the oxygen-enriched air reacts with ferrous chloride and hydrogen chloride in a mother liquor in the form of bubbles;

[0040] The top of the reactor body 41 is connected with an external air extraction pipe 42 and an internal air extraction pipe 43, both of which are annular in design, and the external air extraction pipe 42 and the internal air extraction pipe 43 are staggered in vertical arrangement, the ends of the external air extraction pipe 42 and the internal air extraction pipe 43 extend to the outside of the reactor body 41, and the ends of the external air extraction pipe 42 and the internal air extraction pipe 43 are both connected to an external air extraction device, after the oxygen-enriched air entering the reactor body 41 passes through the hydrogen chloride-containing electrolytic mother liquid in the reactor body 41 and floats to the top of the reactor body 41, the external air extraction device works, and the oxygen-enriched air that continuously floats to the top of the reactor body 41 is extracted through the external air extraction pipe 42 and the internal air extraction pipe 43;

[0041] The inner wall of the reactor body 41 is provided with an air guide pipe 45, which is connected to the output end of the external air extraction device. The external air extraction device re-sends the oxygen-enriched air extracted from the top of the reactor body 41 by the external air extraction pipe 42 and the internal air extraction pipe 43 to the micro-interface generator 44 through the air guide pipe 45, so that the oxygen-enriched air is re-formed into bubbles and participates in the reaction again.

[0042] A transmission assembly 46 is provided at the top of the reactor body 41, and a transmission rod 47 is connected to the output end of the transmission assembly 46. A plurality of groups of foam-breaking blades 48 are provided in the middle of the transmission rod 47. The foam-breaking blades 48 are located on the upper surface of the electrolytic mother liquid inside the reactor body 41. The foam-breaking blades 48 are inclined. An external driving device is connected to the transmission assembly 46, and the transmission rod 47 is driven to rotate by the transmission assembly 46. The foam-breaking blades 48 rotate synchronously under the drive of the transmission rod 47. During the rotation, the foam-breaking blades 48 continuously push the bubbles on the top of the liquid surface in the reactor body 41, accelerate the bursting of the bubbles, and expose the liquid surface, thereby ensuring that the bubbles are not restricted by the upper bubbles and burst quickly, thereby avoiding the generation of a large number of bubbles and also avoiding the merging of the bubbles to form large bubbles.

[0043] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "connected" and "connection" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. In addition, in the description of the present invention, unless otherwise specified, "plurality" means two or more.

[0044] Although the embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the claims and their equivalents.

Claims

1. A microinterface reactor for continuous production of ferric chloride, comprising a reactor body (41), characterized in that: The top of the reactor body (41) is connected to an external air extraction pipe (42) and an internal air extraction pipe (43), the ends of the external air extraction pipe (42) and the internal air extraction pipe (43) are connected to the input end of an external air extraction device, a micro-interface generator (44) is arranged at the bottom of the reactor body (41), an air guide pipe (45) is arranged on the inner wall of the reactor body (41), the air guide pipe (45) is connected to the output end of the external air extraction device, a transmission component (46) is arranged at the top of the reactor body (41), the output end of the transmission component (46) is connected to a transmission rod (47), and a plurality of groups of foam-breaking blades (48) are arranged in the middle of the transmission rod (47); The gas enters the reactor body (41) in the form of fine bubbles through the micro-interface generator (44) at the bottom of the reactor body (41). The oxygen-rich air entering the reactor body (41) passes through and participates in the reaction of the electrolytic mother liquid in the reactor body (41). The gas passing through the electrolytic mother liquid is collected by the external exhaust pipe (42) and the internal exhaust pipe (43) and is re-sent to the micro-interface generator (44) through the external exhaust device and the air guide pipe (45); The foam bursting blade (48) rotates synchronously with the driving rod (47). During the rotation process, the foam bursting blade (48) continuously pushes the bubbles on the top of the liquid surface in the reactor body (41) to accelerate the bursting of the bubbles and expose the liquid surface, thereby ensuring that the bubbles are not restricted by the bubbles in the upper layer and burst quickly, thereby avoiding the generation of a large number of bubbles and also preventing the bubbles from merging to form large bubbles and remaining in the reactor body (41) for a long time.

2. A microinterface reactor for continuous production of ferric chloride according to claim 1, characterized in that: The outer exhaust pipe (42) and the inner exhaust pipe (43) are both annular in design, and the outer exhaust pipe (42) and the inner exhaust pipe (43) are arranged in an up-down staggered manner, one end of the outer exhaust pipe (42) and the inner exhaust pipe (43) extend to the outside of the reactor body (41), and the ends of the outer exhaust pipe (42) and the inner exhaust pipe (43) are connected to an external exhaust device.

3. A microinterface reactor for continuous production of ferric chloride according to claim 1, characterized in that: The foam-breaking blade (48) is located on the upper surface of the electrolytic mother liquid inside the reactor body (41), and the foam-breaking blade (48) is arranged with an inclined blade.

4. A reaction process for a microinterface reactor for continuous production of ferric chloride according to any one of claims 1 to 3, characterized in that: The following steps are included: Step A, preparing a secondary absorption tower (1), a primary absorption tower (2) and a micro-interface reactor (4), connecting the secondary absorption tower (1), the primary absorption tower (2) and the micro-interface reactor (4) through a pipeline, injecting an electrolytic mother liquid into the secondary absorption tower (1) and the primary absorption tower (2), and allowing the electrolytic mother liquid to absorb hydrogen chloride in the industrial tail gas to form an electrolytic mother liquid containing hydrogen chloride; Step B, the electrolytic mother liquid containing hydrogen chloride is poured into the reactor body (41), oxygen-enriched air is input into the reactor body (41), the oxygen-enriched air is broken into micron-sized bubbles by the micro-interface generator (44) at the bottom of the reactor body (41), and then enters the reactor body (41), the bubbles pass through the electrolytic mother liquid containing hydrogen chloride, and in the reactor body (41), the ferrous chloride in the electrolytic mother liquid reacts with hydrogen chloride and the oxygen-enriched air to generate ferric chloride, and the content of ferric chloride in the electrolytic mother liquid increases as the reaction proceeds; Step C, a reaction liquid self-circulation system is arranged outside the micro-interface reactor (4), the self-circulation system causes the electrolytic mother liquid in the micro-interface reactor (4) to circulate up and down, and maintains the temperature during the circulation; Step D, the electrolytic mother liquor containing ferric chloride is drawn out from the bypass pipeline of the circulation system and enters into the evaporation tank to obtain the ferric chloride solution of the required concentration for electrolysis.

5. The reaction process for continuous production of ferric chloride using a microinterface reactor according to claim 4, characterized in that: In step A, the secondary absorption tower (1) and the primary absorption tower (2) are arranged in parallel, the bottom end of the secondary absorption tower (1) is connected to the primary absorption tower (2) via a pipeline, a delivery pump (3) is arranged in the middle of the pipeline, and the delivery pump (3) cooperates with the pipeline to form a liquid delivery path from the bottom end of the secondary absorption tower (1) to the top end of the primary absorption tower (2), and the electrolyte mother liquid entering the secondary absorption tower (1) enters the primary absorption tower (2) through the liquid delivery path.

6. The reaction process for the continuous production of ferric chloride using a microinterface reactor according to claim 4, characterized in that: In step A, the top end of the primary absorption tower (2) is connected to the lower end of the secondary absorption tower (1) via a conduit, and the hydrogen chloride-containing tail gas entering the primary absorption tower (2) enters the secondary absorption tower (1) via the conduit.

7. The reaction process for the continuous production of ferric chloride using a microinterface reactor according to claim 4, characterized in that: In the step B, the bottom end of the micro-interface reactor (4) is connected to an air pump (5), and the air pump (5) is connected to an external oxygen-enriched air supply device.

8. The reaction process for the continuous production of ferric chloride using a microinterface reactor according to claim 4, characterized in that: In the step B, the total flux of oxygen-enriched air entering the reactor body (41) is 100% to 300% of the theoretical consumption.

9. The reaction process for the continuous production of ferric chloride using a microinterface reactor according to claim 4, characterized in that: In step C, the reaction liquid self-circulation system comprises a heat exchanger (6) and a circulation pump (7); the input end and the output end of the heat exchanger (6) are respectively connected to the upper and lower parts of the micro-interface reactor (4) through pipelines; a circulation pump (7) is provided between the pipeline and the heat exchanger (6); the circulation pump (7) extracts the electrolytic mother liquid from the upper part of the micro-interface reactor (4) through the pipeline; the extracted electrolytic mother liquid passes through the heat exchanger (6) to maintain the temperature at 30-60° C. and then re-enters the lower end of the micro-interface reactor (4).

10. The reaction process for the microinterface reactor for continuous production of ferric chloride according to claim 9, characterized in that: A group of evaporation tanks (8) are connected between the circulation pump (7) and the pipeline of the micro-interface reactor (4) via a bypass pipeline.

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