A device and process for preparing high-purity iodine monochloride from crude iodine

Abstract

The present invention discloses a process for preparing high-purity iodine monochloride from crude iodine, comprising the following preparation steps: S1, inputting crude iodine; S2, passing chlorine; S3, absorbing excess chlorine; S4, filtering and separating. The present invention also discloses a device for preparing high-purity iodine monochloride from crude iodine, comprising a reactor, an air inlet pipe and a feed pipe are provided on the reactor, a stirring shaft is provided for rotation in the reactor, and the stirring shaft is hollowly arranged, a reciprocating screw is fixedly connected to the top of the reactor, and the reciprocating screw is rotatably arranged inside the stirring shaft, and two reciprocating thread sections are provided on the reciprocating screw. The present invention can greatly shorten the effective reaction time of the process for preparing high-purity iodine monochloride from crude iodine by improving process conditions and equipment, from 8-10 hours in the prior art to less than 1-5 hours, and the purity content of the iodine monochloride obtained is high, which meets the requirements of modern process production.

Description

Technical Field

[0001] The invention relates to the technical field of chemical industry, and in particular to a device and a process for preparing high-purity iodine monochloride from crude iodine. Background Art

[0002] Iodine monochloride is an important basic chemical raw material. It can be used as an iodination reagent and as an iodine substitution on the benzene ring. In the modern preparation process, crude iodine is generally used as the production raw material, and chlorine gas is introduced into the reaction to obtain the iodine monochloride product.

[0003] In the current process flow of iodine monochloride preparation, it is necessary to start the stirring device in the reaction vessel after the chlorine is introduced so that the reactants are fully mixed. This processing method is less efficient for the following reasons: since the blades of the stirring device are rotating, the blades of each layer height can only stir the crude iodine raw material of each layer, and most of the chlorine is above the crude iodine raw material, so it is difficult for chlorine to contact and react with the crude iodine raw material on the lower side, so under the current equipment and process conditions, it generally takes 8-10 hours to react completely, and the reaction time is long and inefficient. Accordingly, the present application proposes a process and device for preparing high-purity iodine monochloride from crude iodine. Summary of the invention

[0004] The purpose of the present invention is to provide a device and process for preparing high-purity iodine monochloride from crude iodine with high reaction efficiency.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] The present invention proposes a device for preparing high-purity iodine monochloride from crude iodine, comprising a reactor, wherein an air inlet pipe and a feed pipe are provided on the reactor, a stirring shaft is rotatably provided in the reactor, and the stirring shaft is hollowly arranged, a reciprocating screw is fixedly connected to the top of the reactor, and the reciprocating screw is rotatably arranged inside the stirring shaft, two reciprocating thread sections are provided on the reciprocating screw, and a screw nut is threadedly connected to each reciprocating thread section, swing grooves are provided on both sides of the stirring shaft, stirring blades are rotatably connected in the swing grooves, and gears are fixedly connected to the side walls of the stirring blades, racks are fixedly connected on both sides of the screw nut, and the racks are meshed with the gears, a plurality of sealing plates are provided in the stirring shaft, and every two adjacent sealing plates are arranged on the upper and lower sides of the screw nut, and the reciprocating screw seal passes through the sealing plate.

[0007] Preferably, two transmission rollers are rotatably connected to the inner walls on both sides of the reactor, and two adjacent transmission rollers are connected by a transmission belt. A plurality of hoppers are fixedly provided on the side walls of the transmission belt, and the plurality of hoppers are evenly spaced on the transmission belt. A driving groove is provided on the side walls of the reactor, and a rotating device for rotating the transmission roller is installed in the driving groove.

[0008] Preferably, the rotating device includes a first bevel gear rotatably connected to the bottom of the driving groove, and two second bevel gears are also rotatably connected in the driving groove, the two second bevel gears are meshed with the first bevel gear, and each of the second bevel gears is fixedly connected to the adjacent transmission roller via a rotating shaft. A driving motor is fixedly installed on the side wall of the reactor, and the output shaft of the driving motor is fixedly connected to the second bevel gears.

[0009] Preferably, two vibration plates are rotatably connected to the inner wall of the reactor, and the vibration plates are connected to the top of the reactor through springs. A telescopic cylinder is fixedly installed on the upper end of the reactor, and the telescopic end seal of the telescopic cylinder passes through the top of the reactor and extends into it.

[0010] Preferably, the rotation connection between the vibration plate and the reaction kettle is located at the center of the vibration plate, and the telescopic ends of the spring and the telescopic cylinder are respectively arranged on both sides of the vibration plate.

[0011] The present invention also provides a process for preparing high-purity iodine monochloride from crude iodine, comprising the following preparation steps:

[0012] S1. Input crude iodine, input the crude iodine raw material into the reaction vessel according to the required production quantity, and ensure that the temperature is between 35°C and 55°C;

[0013] S2, pass chlorine, according to the production measurement (chlorine: iodine molar ratio = 1-1.2: 1), pass chlorine into the reaction vessel, stirring at the same time, forcing the crude iodine and chlorine to mix evenly, the reaction and stirring time is 1-5 hours;

[0014] S3, absorbing excess chlorine, pumping the gas in the reaction container into the absorption container, and using alkali solution to absorb excess chlorine;

[0015] S4, filtering and separating, after filtering and separating the obtained mixed reaction product, liquid iodine monochloride can be collected.

[0016] Preferably, in step S1, the crude iodine raw material used must be clean and free of impurities to avoid mixing with organic impurities. At the same time, the preferred feeding temperature is 45° C. to prevent iodine sublimation.

[0017] Preferably, in step S2, the stoichiometric ratio (chlorine: iodine molar ratio = 1.05:1) and the stirring time are 2.5 hours.

[0018] Preferably, in step S3, the alkali solution for absorbing chlorine gas may be a sodium hydroxide solution, and the mass concentration of the sodium hydroxide solution is 2%-5%.

[0019] The present invention has the following beneficial effects:

[0020] 1. By arranging components such as a reciprocating screw, a screw nut, a rack and a gear, the stirring blade can be driven by the stirring shaft to rotate, and the stirring blade can also be made to swing up and down, so that the layers of crude iodine raw materials in the reactor can flow up and down and shift, so that the lower layer of crude iodine raw materials can be continuously turned to the upper layer, which greatly improves the reaction efficiency of chlorine and crude iodine raw materials.

[0021] 2. By providing a transmission roller, a transmission belt and a hopper, during the operation of the device, the transmission belt can be continuously operated, and the hopper on the transmission belt can be used to continuously turn the crude iodine raw materials at various locations inside the reactor to the top of the reactor, and sprinkled at a higher position. On the one hand, the reaction efficiency of the crude iodine raw materials at various locations in the reactor and the chlorine gas can be improved, and on the other hand, the contact area between the crude iodine raw materials and the chlorine gas can be increased, further accelerating the reaction speed;

[0022] 3. By setting up a vibration plate, the telescopic cylinder and the spring can continuously act on the hopper, which can not only completely pour out the crude iodine raw material in the hopper, but also increase the scattering area of ​​the crude iodine raw material to accelerate the reaction efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 This is a schematic structural diagram of a device for preparing high-purity iodine monochloride from crude iodine proposed by the present invention;

[0024] Figure 2 for Figure 1 A schematic diagram of the structure enlargement at point A;

[0025] Figure 3 The figure is a schematic diagram of the side structure of a drive roller, a drive belt, a hopper, a vibration plate and a spring of a device for preparing high-purity iodine monochloride from crude iodine.

[0026] In the figure: 1 reactor, 2 air inlet pipe, 3 feed pipe, 4 telescopic cylinder, 5 spring, 6 vibration plate, 7 stirring shaft, 8 reciprocating screw, 9 stirring blade, 10 transmission roller, 11 transmission belt, 12 hopper, 13 driving groove, 14 first bevel gear, 15 second bevel gear, 16 driving motor, 17 sealing plate, 18 screw nut, 19 rack, 20 swing groove, 21 gear. DETAILED DESCRIPTION

[0027] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0028] A process for preparing high-purity iodine monochloride from crude iodine comprises the following preparation steps:

[0029] S1. Input crude iodine, input the crude iodine raw material into the reaction vessel according to the required production quantity, and ensure that the temperature is between 35°C and 55°C;

[0030] S2, pass into chlorine, according to the production measurement (chlorine: iodine = 1-1.2: 1), pass chlorine into the reaction vessel, stir at the same time, force the crude iodine and chlorine to mix evenly, the reaction and stirring time is 1-5 hours;

[0031] S3, absorbing excess chlorine, pumping the gas in the reaction container into the absorption container, and using alkali solution to absorb excess chlorine; the alkali solution for absorbing chlorine can be sodium hydroxide solution, and the mass concentration of the sodium hydroxide solution is 2%-5%.

[0032] S4, filtering and separating, after filtering and separating the obtained mixed reaction product, liquid iodine monochloride can be collected.

[0033] By changing the reaction conditions, the following examples can be obtained:

[0034] Example 1: The chlorine gas and crude iodine raw material were added in a metering ratio of 1:1, and the feeding temperature was 55°C. The reaction was completed in 6 hours to obtain iodine monochloride with a content of 99.82%;

[0035] Example 2: The chlorine gas and crude iodine raw material were added in a metering ratio of 1.1:1, and the feeding temperature was 35°C. The reaction was completed in 3 hours to obtain iodine monochloride with a content of 99.90%;

[0036] Example 3: The chlorine gas and crude iodine raw material were added in a metering ratio of 1.2:1, and the feeding temperature was 45°C. The reaction was completed in 1 hour to obtain iodine monochloride with a content of 99.78%;

[0037] Example 4: The chlorine gas and crude iodine raw material were added in a metering ratio of 1.05:1, and the feeding temperature was 45°C. The reaction was completed in 2.5 hours to obtain iodine monochloride with a content of 99.95%;

[0038] The results are shown in the following table:

[0039]

[0040]

[0041] Table 1: Iodine monochloride prepared under different reaction conditions

[0042] In summary, the present invention can greatly shorten the effective reaction time of the process for preparing high-purity iodine monochloride from crude iodine by improving process conditions and equipment, from 8-10 hours in the prior art to within 1-5 hours, and the prepared iodine monochloride has high purity content, which meets the requirements of modern process production.

[0043] Reference Figure 1-Figure 3 The present invention also proposes a device for preparing high-purity iodine monochloride from crude iodine, comprising a reactor 1, an air inlet pipe 2 and a feed pipe 3 are provided on the reactor 1, a stirring shaft 7 is rotatably provided in the reactor 1, and the stirring shaft 7 is hollow, a reciprocating screw 8 is fixedly connected to the top of the reactor 1, and the reciprocating screw 8 is rotatably provided inside the stirring shaft 7, two reciprocating thread sections are provided on the reciprocating screw 8, and each reciprocating thread section is threadedly connected with a screw nut 18, for details, refer to Figure 1 and Figure 2 There is a certain distance between the threaded sections of the reciprocating screw 8, and the rest is a smooth rod, which can effectively limit the stroke of the screw nut 18.

[0044] Swinging grooves 20 are provided on both sides of the stirring shaft 7, and stirring blades 9 are rotatably connected in the swinging grooves 20, and gears 21 are fixedly connected to the side walls of the stirring blades 0, and racks 19 are fixedly connected to both sides of the screw nut 18, and the racks 19 are meshed with the gears 21. A plurality of sealing plates 17 are provided in the stirring shaft 7, and every two adjacent sealing plates 17 are arranged on the upper and lower sides of the screw nut 18, and the reciprocating screw 8 seals and penetrates the sealing plates 17. It should be noted that by providing the sealing plates 17, the hollow stirring shaft 7 can be blocked, so that the reaction products or raw materials only remain in the area between the two sealing plates 17 that is exposed to the outside, and in the later cleaning, only the exposed area between the two sealing plates 17 needs to be cleaned, which can greatly reduce the difficulty of cleaning.

[0045] Two transmission rollers 10 are rotatably connected to the inner walls on both sides of the reactor 1, and two adjacent transmission rollers 10 are connected by a transmission belt 11. A plurality of hoppers 12 are fixedly provided on the side wall of the transmission belt 11, and the plurality of hoppers 12 are evenly spaced and distributed on the transmission belt 11. A driving groove 13 is provided on the side wall of the reactor 1, and a rotating device for rotating the transmission roller 10 is installed in the driving groove 13.

[0046] The rotating device includes a first bevel gear 14 rotatably connected to the bottom of the driving groove 13. Two second bevel gears 15 are also rotatably connected in the driving groove 13. The two second bevel gears 15 are both meshed with the first bevel gear 14. Each second bevel gear 15 is fixedly connected to the adjacent transmission roller 10 through a rotating shaft. A driving motor 16 is fixedly installed on the side wall of the reactor 1, and the output shaft of the driving motor 16 is fixedly connected to the second bevel gear 15.

[0047] Two vibration plates 6 are also rotatably connected to the inner wall of the reactor 1. The vibration plates 6 are connected to the top of the reactor 1 through springs 5. A telescopic cylinder 4 is fixedly installed on the upper end of the reactor 1. The telescopic end of the telescopic cylinder 4 is sealed and penetrates the top of the reactor 1 and extends into it. The rotation connection between the vibration plate 6 and the reactor 1 is located at the center of the vibration plate 6, and the spring 5 and the telescopic end of the telescopic cylinder 4 are respectively arranged on both sides of the vibration plate 6. It should be noted that, since the spacing between every two adjacent hoppers 12 is fixed, by setting the telescopic interval period of the telescopic cylinder 4, it can be ensured that: when the telescopic end of the telescopic cylinder 4 moves downward and pushes the vibration plate 6 to deflect, the end of the vibration plate 6 close to the transmission belt 11 will be tilted, so that this side of the vibration plate 6 can be away from the transmission belt 11, and the hopper 12 on the transmission belt 11 can smoothly turn over the upper transmission roller 10 without being blocked by the vibration plate 6. When the telescopic end of the telescopic cylinder 4 moves upward, the spring 5 pushes the vibration plate 6 to deflect, and the end of the vibration plate 6 close to the transmission belt 11 moves downward, so that the turned over hopper 12 can be hit just once to cause the crude iodine raw material therein to be scattered and dropped.

[0048] During use of the device, chlorine gas can be introduced into the reactor 1 through the air inlet pipe 2, and the crude iodine raw material can be transported into the reactor 1 through the feed pipe 3. The drive motor 16 is started, and the drive motor 16 can drive the second bevel gear 15 to rotate, so that the first bevel gear 14 meshing with the second bevel gear 15 will rotate, thereby driving the stirring shaft 7 to continuously rotate. When the stirring shaft 7 rotates, the stirring blade 9 thereon also rotates accordingly, and the gear 21 on the stirring blade 9 is meshed with the rack 19, and the rack 19 is fixed on the lead screw nut 18, so that the lead screw nut 18 can be driven to rotate on the reciprocating lead screw 8, so that the lead screw nut 18 will reciprocate up and down, and during the up and down movement of the lead screw nut 18, the gears 21 on both sides can be reciprocated up and down in the opposite directions through the rack 19, so that the stirring blade 9 swings up and down. Compared with the stirring device of the transmission reaction container, the stirring blade 9 in the present invention can also swing up and down during the rotation of the stirring shaft 7, so that the layers of crude iodine raw materials in the reactor 1 can flow up and down and transpose, so that the lower layer of crude iodine raw materials can be continuously turned to the upper layer, which greatly improves the reaction efficiency of chlorine and crude iodine raw materials.

[0049] Furthermore, the second bevel gear 15 can also drive the transmission roller 10 to rotate continuously when rotating, and the transmission roller 10 can make the transmission belt 11 operate continuously when rotating. Figure 1 For example, during the operation of the transmission belt 11, the hopper 12 on it can continuously transport the crude iodine raw materials from various places in the reactor 1 to the top of the reactor 1, and when turning over the upper transmission roller 10, the direction of the hopper 12 is reversed (such as Figure 3As shown), the crude iodine raw material carried can be poured and sprinkled. On the one hand, when the hopper 12 is driven by the transmission belt 11 to operate together, Figure 3 For example, the hopper 12 on the left can push the crude iodine raw material on the upper layer into the lower layer, and the hopper 12 on the right can push the crude iodine raw material on the lower side to the upper layer, forcing the crude iodine raw material in the reactor 1 to interact with each other, so as to improve the reaction efficiency of the crude iodine raw material and chlorine gas at various locations in the reactor. On the other hand, when the hopper 12 is turned over and the crude iodine raw material is thrown down, it will spread to a larger area, so that the contact area between the crude iodine raw material and the chlorine gas can be effectively increased, and the reaction speed can be further accelerated;

[0050] In addition, it is worth mentioning that the telescopic end of the telescopic cylinder 4 will continue to expand and contract, so that one side of the vibration plate 6 can be continuously pushed down. When the telescopic cylinder 4 contracts, the spring 5 pulls the vibration plate 6 to rotate and reset, so under the joint action of the telescopic cylinder 4 and the spring 5, the vibration plate 6 can rotate back and forth around its rotation axis. When the end of the vibration plate 6 close to the transmission belt 11 deflects downward, it can knock the hopper 12 once. On the one hand, it can promote the crude iodine raw material in the hopper 12 to be thrown cleanly. On the other hand, due to the knocking effect of the vibration plate 6, an external force can be applied to the throwing of the crude iodine raw material, so that the throwing range of the crude iodine raw material can be further increased, and the contact area between the crude iodine raw material and the chlorine gas can be further increased, thereby increasing the reaction rate again.

[0051] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A device for preparing high-purity iodine monochloride from crude iodine, comprising a reactor (1), wherein the reactor (1) is provided with an air inlet pipe (2) and a feed pipe (3), wherein: A stirring shaft (7) is rotatably provided in the reactor (1), and the stirring shaft (7) is hollow. A reciprocating screw (8) is fixedly connected to the top of the reactor (1), and the reciprocating screw (8) is rotatably provided inside the stirring shaft (7). The reciprocating screw (8) is provided with two reciprocating threaded sections, and each reciprocating threaded section is threadedly connected with a screw nut (18). Both sides of the stirring shaft (7) are provided with swing grooves (20), and a stirring blade (9) is rotatably connected in the swing grooves (20), and a gear (21) is fixedly connected to the side wall of the stirring blade (9). Both sides of the screw nut (18) are fixedly connected with a rack (19), and the rack (19) meshes with the gear (21). A plurality of sealing plates (17) are provided in the stirring shaft (7), and every two adjacent sealing plates (17) are provided on the upper and lower sides of the screw nut (18), and the reciprocating screw (8) seals through the sealing plates (17); Two transmission rollers (10) are rotatably connected to the inner walls of both sides of the reactor (1), and two adjacent transmission rollers (10) are connected by a transmission belt (11). A plurality of hoppers (12) are fixedly provided on the side wall of the transmission belt (11), and the plurality of hoppers (12) are evenly spaced and distributed on the transmission belt (11). A driving groove (13) is provided on the side wall of the reactor (1), and a rotating device for rotating the transmission rollers (10) is installed in the driving groove (13). The transmission belt (11) is continuously operated, and the hoppers (12) on the transmission belt (11) are continuously used to turn the crude iodine raw materials at various locations inside the reactor (1) to the top of the reactor (1), and sprinkle them at a higher position.

2. The device for preparing high-purity iodine monochloride from crude iodine according to claim 1, characterized in that: The rotating device comprises a first bevel gear (14) rotatably connected to the bottom of the driving groove (13); two second bevel gears (15) are also rotatably connected in the driving groove (13); the two second bevel gears (15) are both meshed with the first bevel gear (14); each of the second bevel gears (15) is fixedly connected to an adjacent transmission roller (10) via a rotating shaft; a driving motor (16) is fixedly mounted on a side wall of the reaction kettle (1); an output shaft of the driving motor (16) is fixedly connected to the second bevel gears (15).

3. The device for preparing high-purity iodine monochloride from crude iodine according to claim 2, characterized in that: Two vibration plates (6) are rotatably connected to the inner wall of the reactor (1); the vibration plates (6) are connected to the top of the reactor (1) via springs (5); a telescopic cylinder (4) is fixedly mounted on the upper end of the reactor (1); the telescopic end of the telescopic cylinder (4) is sealed and passes through the top of the reactor (1) and extends into the reactor.

4. The device for preparing high-purity iodine monochloride from crude iodine according to claim 3, characterized in that: The rotational connection between the vibration plate (6) and the reaction kettle (1) is located at the center of the vibration plate (6), and the telescopic ends of the spring (5) and the telescopic cylinder (4) are respectively arranged on both sides of the vibration plate (6).

5. A process for preparing high-purity iodine monochloride using the crude iodine according to any one of claims 1 to 4, characterized in that: The method comprises the following preparation steps: S1. Input the crude iodine raw material into a reaction vessel and ensure that the temperature is between 35°C and 55°C; S2, chlorine: crude iodine molar ratio 1-1.2:1, chlorine is introduced into the reaction vessel, and stirred at the same time to force the crude iodine and chlorine to mix evenly, and the reaction and stirring time is 1-5 hours; S3, absorbing excess chlorine, pumping the gas in the reaction container into the absorption container, and using alkali solution to absorb excess chlorine; S4, filtering and separating, filtering and separating the obtained mixed reaction product, and collecting liquid iodine monochloride.

6. A process for preparing high-purity iodine monochloride from crude iodine according to claim 5, characterized in that: In the step S1, the crude iodine raw material used must be clean and free of impurities, and the feeding temperature is 45°C.

7. A process for preparing high-purity iodine monochloride from crude iodine according to claim 5, characterized in that: In step S2, the molar ratio of chlorine gas to crude iodine is 1.05:1, and the stirring time is 2.5 hours.

8. A process for preparing high-purity iodine monochloride from crude iodine according to claim 5, characterized in that: In step S3, the alkali solution for absorbing chlorine is a sodium hydroxide solution, and the mass concentration of the sodium hydroxide solution is 2%-5%.

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