CN116534800A - Device and process for preparing high-purity iodine monochloride from crude iodine - Google Patents

Abstract

The invention discloses a process for preparing high-purity iodine monochloride from crude iodine, which comprises the following preparation steps: s1, inputting crude iodine; s2, introducing chlorine; s3, absorbing redundant chlorine; s4, filtering and separating. The invention also discloses a device for preparing high-purity iodine monochloride from crude iodine, which comprises a reaction kettle, wherein an air inlet pipe and an air inlet pipe are arranged on the reaction kettle, a stirring shaft is rotationally arranged in the reaction kettle, the stirring shaft is arranged in a hollow mode, a reciprocating screw rod is fixedly connected to the inner top of the reaction kettle, the reciprocating screw rod is rotationally arranged in the stirring shaft, and two reciprocating thread sections are arranged on the reciprocating screw rod. The invention can fully and greatly shorten the effective reaction time of the process for preparing the high-purity iodine monochloride from the crude iodine by improving the process conditions and equipment, shortens the time from 8-10 hours to within 1-5 hours in the prior art, and simultaneously ensures that the prepared iodine monochloride has high purity and meets the production requirements of the modern process.

Description

A kind of crude iodine prepares high-purity iodine monochloride device and process

technical field

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

Background technique

Iodine monochloride is an important basic chemical raw material, which can be used as an iodination reagent, as the iodide on the benzene ring. In the contemporary preparation process, crude iodine is generally used as the raw material for production, and it can be obtained by introducing chlorine gas for reaction. Iodine monochloride product.

However, in the current technical process for the preparation of iodine monochloride, it is necessary to start the stirring device in the reaction vessel after introducing chlorine gas, so that the reactants can be fully mixed. This processing mode efficiency is low, and reason is as follows: because the blade of stirring device is in the rotation process, the blade of each layer height can only stir the thick iodine raw material of each layer, and chlorine gas major part is all in above the thick iodine raw material, therefore It is difficult for chlorine gas 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 the efficiency is low. Accordingly, the application proposes a process and device for preparing high-purity iodine monochloride from crude iodine.

Contents of the invention

The purpose of the invention is to propose a high-purity iodine monochloride device and technique for the high crude iodine of the proposed reaction efficiency.

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

The present invention proposes a device for preparing high-purity iodine monochloride from crude iodine, comprising a reaction kettle, the reaction kettle is provided with an air inlet pipe and a feed pipe, and the rotation of the reaction kettle is provided with a stirring shaft, and the stirring The shaft is hollow, and the top of the reaction kettle is fixedly connected with a reciprocating screw, and the reciprocating screw is rotated inside the stirring shaft. There are two reciprocating thread sections on the reciprocating screw, and each reciprocating thread section There are lead screw nuts threaded on the top, 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, and the lead screw nuts are There are racks fixedly connected to both sides of the shaft, and the racks are meshed with the gears. There are multiple sealing plates inside the stirring shaft, and every two adjacent sealing plates are arranged on the upper and lower sides of the lead screw nut. The reciprocating lead screw seal runs through the sealing plate.

Preferably, two drive rollers are respectively rotatably connected to the inner walls on both sides of the reaction kettle, and two adjacent drive rollers are connected by a drive belt, and a plurality of hoppers are fixed on the side wall of the drive belt, and a plurality of the The hoppers are distributed at equal intervals on the transmission belt, and the side wall of the reaction kettle is provided with a driving groove, and a rotating device for rotating the driving roller is installed in the driving groove.

Preferably, the rotating device includes a first bevel gear that is rotatably connected to the bottom of the driving groove, and there are two second bevel gears that are rotatably connected in the driving groove, and the two second bevel gears are both connected to the first bevel gear. The gears are meshed, and each second bevel gear is fixedly connected to the adjacent drive roller through a rotating shaft. A driving motor is fixedly installed on the side wall of the reaction kettle, and the output shaft of the driving motor is fixedly connected to the second bevel gear.

Preferably, two vibrating plates are rotatably connected to the inner wall of the reactor, and the vibrating plates are connected to the top of the reactor through springs, and a telescopic cylinder is fixedly installed on the upper end of the reactor, and the telescopic end of the telescopic cylinder is sealed It runs through the top of the reactor and extends into it.

Preferably, the rotational connection between the vibrating plate and the reactor is located at the center of the vibrating plate, and the spring and telescopic ends of the telescopic cylinder are respectively arranged on both sides of the vibrating plate.

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

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

S2, feed chlorine gas, according to the production metering (chlorine gas: iodine molar ratio=1-1.2:1), feed chlorine gas into the reaction vessel, stir at the same time, force the thick iodine and chlorine gas to mix uniformly, the reaction and stirring time are 1-5 Hour;

S3, absorb excess chlorine gas, pump the gas in the reaction vessel into the absorption vessel, and use lye to absorb excess chlorine gas;

S4. Filtration and separation. After the obtained mixed reaction product is filtered and separated, liquid iodine monochloride can be collected.

Preferably, in the step S1, the crude iodine raw material used must be clean and free of impurities to avoid mixing of organic impurities, and the feeding temperature is preferably 45° C. to prevent iodine sublimation.

Preferably, in step S2, stoichiometric number (chlorine: iodine molar ratio = 1.05:1), stirring time is 2.5 hours.

Preferably, in the step S3, sodium hydroxide solution may be used as the lye for absorbing chlorine gas, and the mass concentration of the sodium hydroxide solution is 2%-5%.

The present invention has the following beneficial effects:

1. By setting the reciprocating screw, screw nut, rack and gear and other components, the stirring blade can be swung up and down when the stirring shaft drives the stirring blade to rotate, so that the crude iodine raw materials in each layer of the reactor can be Up and down flow and transposition, so that the crude iodine raw material in the lower layer can be continuously turned to the upper layer, which greatly improves the reaction efficiency of chlorine gas and crude iodine raw material.

2. By setting the transmission roller, transmission belt and hopper, during the operation of the device, the transmission belt can be continuously operated, and the crude iodine raw materials inside the reaction kettle can be continuously turned to the top of the reaction kettle by using the hopper on the transmission belt. Sprinkling at a high position, on the one hand, improves the reaction efficiency between the crude iodine raw material and chlorine gas in various parts of the reactor, on the other hand, it can also increase the contact area between the crude iodine raw material and chlorine gas, and further accelerate the reaction speed;

3. By setting the vibrating plate, it can continue to act on the hopper under the joint action of the telescopic cylinder and the spring, which can not only dump the crude iodine raw material in the hopper completely, but also increase the throwing area of the crude iodine raw material to speed up the reaction efficiency .

Description of drawings

Fig. 1 is a kind of crude iodine that the present invention proposes and prepares the structural representation of high-purity iodine monochloride device;

Fig. 2 is the enlarged schematic view of the structure at A in Fig. 1;

Fig. 3 is the side structural representation of a kind of thick iodine preparation high-purity iodine monochloride device drive roller, transmission belt, hopper, vibrating plate and spring.

In the figure: 1 reaction kettle, 2 intake pipe, 3 feed pipe, 4 telescopic cylinder, 5 spring, 6 vibrating plate, 7 stirring shaft, 8 reciprocating screw, 9 stirring blade, 10 transmission roller, 11 transmission belt, 12 hopper, 13 drive grooves, 14 first bevel gears, 15 second bevel gears, 16 drive motors, 17 sealing plates, 18 lead screw nuts, 19 tooth racks, 20 swing grooves, 21 gears.

Detailed ways

The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention.

A kind of crude iodine prepares high-purity iodine monochloride technique, comprises following preparation steps:

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

S2, feed chlorine gas, according to production metering (chlorine gas: iodine=1-1.2:1), feed chlorine gas to reaction vessel, stir simultaneously, force thick iodine and chlorine gas to mix, reaction and stirring time are 1-5 hour;

S3, absorb excess chlorine, pump the gas in the reaction vessel into the absorption container, and utilize lye to absorb excess chlorine; the lye for absorbing chlorine can use sodium hydroxide solution, and the mass concentration of the sodium hydroxide solution is 2%-5 %.

S4. Filtration and separation. After the obtained mixed reaction product is filtered and separated, liquid iodine monochloride can be collected.

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

Embodiment 1: input chlorine gas, thick iodine raw material metering ratio is 1:1, feeding temperature is 55 ℃, then fully reacts completely in 6 hours, obtains the iodine monochloride that content is 99.82%;

Embodiment two: drop into chlorine gas, thick iodine raw material metering ratio is 1.1:1, and feeding temperature is 35 ℃, then fully reacts completely in 3 hours, obtains the iodine monochloride that content is 99.90%;

Embodiment three: drop into chlorine gas, thick iodine raw material metering ratio is 1.2:1, and feeding temperature is 45 ℃, then fully reacts completely in 1 hour, obtains the iodine monochloride that content is 99.78%;

Embodiment four: drop into chlorine gas, thick iodine raw material metering ratio is 1.05:1, and feeding temperature is 45 ℃, then fully reacts completely in 2.5 hours, obtains the iodine monochloride that content is 99.95%;

The results obtained are shown in the table below:

Table 1: Table of iodine monochloride prepared under different reaction conditions

In summary, the present invention can fully shorten the effective reaction time of crude iodine preparation high-purity iodine monochloride process by improving process conditions and equipment, shortening from 8-10 hours in the prior art to within 1-5 hours , and the iodine monochloride obtained at the same time has a high purity content, which meets the production requirements of modern technology.

With reference to Fig. 1-Fig. 3, the present invention also proposes a kind of thick iodine and prepares high-purity iodine monochloride device, comprises reactor 1, and reactor 1 is provided with inlet pipe 2 and feed pipe 3, and rotation in reactor 1 A stirring shaft 7 is provided, and the stirring shaft 7 is hollowly set, and a reciprocating screw 8 is fixedly connected to the inner top of the reactor 1, and the reciprocating screw 8 is rotated and arranged inside the stirring shaft 7, and the reciprocating screw 8 is provided with two reciprocating threads section, and each reciprocating thread section is threaded with a lead screw nut 18, specifically, referring to Figure 1 and Figure 2, there is a certain distance between the thread sections of the reciprocating lead screw 8, and the rest are polished rods, which can effectively limit Lead screw nut 18 strokes.

Both sides of the stirring shaft 7 are provided with oscillating grooves 20, the oscillating grooves 20 are rotationally connected with stirring blades 9, and the side walls of the stirring blades 0 are fixedly connected with gears 21, and both sides of the lead screw nut 18 are fixedly connected with racks 19 , and the rack 19 meshes with the gear 21, a plurality of sealing plates 17 are arranged in the stirring shaft 7, and every two adjacent sealing plates 17 are arranged on the upper and lower sides of the lead screw nut 18, and the reciprocating lead screw 8 seals through the sealing plates 17. It should be noted that by setting the sealing plate 17, the hollow stirring shaft 7 can be blocked, so that the reaction product or raw material only remains in the exposed area between the two sealing plates 17, and only needs to be cleaned during later cleaning. The exposed area between the two sealing plates 17 is enough, which can greatly reduce the difficulty of cleaning.

There are two drive rollers 10 connected to the inner walls of both sides of the reaction kettle 1, respectively, and two adjacent drive rollers 10 are connected by a transmission belt 11, and a plurality of hoppers 12 are fixed on the side walls of the transmission belt 11, and the plurality of hoppers 12 are in the The transmission belts 11 are distributed at equal intervals, and the side wall of the reaction kettle 1 is provided with a driving groove 13, and a rotating device for rotating the driving roller 10 is installed in the driving groove 13.

The rotating device comprises a first bevel gear 14 that is rotatably connected to the inner bottom of the drive groove 13, and is also rotatably connected with two second bevel gears 15 in the drive groove 13, and the two second bevel gears 15 are all meshed with the first bevel gear 14, Each second bevel gear 15 is fixedly connected to the adjacent drive roller 10 through a rotating shaft, and a driving motor 16 is fixedly installed on the side wall of the reaction kettle 1 , and the output shaft of the driving motor 16 is fixedly connected to the second bevel gear 15 .

The inner wall of the reactor 1 is also rotatably connected with two vibrating plates 6, the vibrating plates 6 are connected to the top of the reactor 1 through the spring 5, the upper end of the reactor 1 is fixedly installed with a telescopic cylinder 4, and the telescopic end of the telescopic cylinder 4 is sealed and runs through the reactor 1 inner top and extending into it. The rotating joint between the vibrating plate 6 and the reactor 1 is located at the center of the vibrating plate 6, and the spring 5 and the telescopic end of the telescopic cylinder 4 are respectively arranged on both sides of the vibrating plate 6. It should be noted that since the distance 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 down and pushes the vibration plate 6 to deflect At this time, the end of the vibrating plate 6 close to the transmission belt 11 is tilted, so that the side of the vibrating plate 6 is 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 vibrating plate 6. , and when the telescopic end of the telescopic cylinder 4 moves up, the spring 5 pushes the vibrating plate 6 to deflect, and the end of the vibrating plate 6 close to the transmission belt 11 moves downward, so that the overturned hopper 12 can just be knocked once to promote its inner The crude iodine raw material is thrown away.

During the use of the above-mentioned device, chlorine gas can be introduced into the reaction kettle 1 through the inlet pipe 2, and the crude iodine raw material can be transported into the reaction kettle 1 through the feed pipe 3. Start the driving motor 16, and the driving motor 16 can drive the second bevel gear 15 to rotate, so that the first bevel gear 14 meshed with the second bevel gear 15 will rotate, and then drive the stirring shaft 7 to continue to rotate. When the stirring shaft 7 rotates, the stirring blade 9 on it also rotates thereupon, and the gear 21 on the stirring blade 9 is engaged with the rack 19, and the rack 19 is fixed on the lead screw nut 18 at the same time, so it can drive The lead screw nut 18 rotates on the reciprocating lead screw 8, which will cause the lead screw nut 18 to 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 reversed up and down through the rack 19. Reciprocating rotation makes the stirring blade 9 swing up and down. Compared with the stirring device of the transmission reaction vessel, the stirring blade 9 in the present invention can also swing up and down during the rotation process with the stirring shaft 7, so that the reaction can be promoted. The crude iodine raw materials of each layer in the kettle 1 can flow up and down and transpose, so that the crude iodine raw materials of the lower layer can be continuously turned to the upper layer, which greatly improves the reaction efficiency of chlorine gas and the crude iodine raw materials.

Further, the second bevel gear 15 can also drive the transmission roller 10 to continuously rotate when rotating, and the transmission roller 10 can make the transmission belt 11 continuously rotate when rotating. Taking Fig. 1 as an example, during the operation of the transmission belt 11, the hopper 12 on it can continuously transport the crude iodine raw materials everywhere in the reaction kettle 1 to the top of the reaction kettle 1, and when turning over the transmission roller 10 on the upper side, , the direction of the hopper 12 is reversed (as shown in Figure 3), so 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 run together, take Figure 3 as an example, the left The hopper 12 on the side 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, so as to improve the efficiency of each reactor. The reaction efficiency of the crude iodine raw material and chlorine gas at the place, on the other hand, when the hopper 12 is turned over and the crude iodine raw material is thrown down, it will diffuse to a larger area, so that the contact area between the crude iodine raw material and chlorine gas can be effectively increased , to further speed up the reaction speed;

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 the vibration plate 6 can be rotated around its axis of rotation under the joint action of the telescopic cylinder 4 and the spring 5, and the vibration plate 6 is close to the transmission belt. When the end of 11 is deflected downward, it can hit the hopper 12 once. On the one hand, it can impel the crude iodine raw material in the hopper 12 to be thrown clean; Sprinkling exerts an external force, can further increase the throwing range of crude iodine raw material like this, further increases the contact area of crude iodine raw material and chlorine gas, thereby improves reaction rate again.

The above is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto, any person familiar with the technical field within the technical scope disclosed in the present invention, according to the technical solution of the present invention Any equivalent replacement or change of the inventive concepts thereof shall fall within the protection scope of the present invention.

Claims (9)

1. The utility model provides a coarse iodine preparation high-purity iodine monochloride device, includes reation kettle (1), be equipped with intake pipe (2) and inlet pipe (3) on reation kettle (1), its characterized in that, reation kettle (1) internal rotation is equipped with (mixing) shaft (7), just (mixing) shaft (7) cavity sets up, top fixedly connected with reciprocating screw (8) in reation kettle (1), just reciprocating screw (8) rotate and set up inside (mixing) shaft (7), be equipped with two reciprocating screw thread sections on reciprocating screw (8), and equal threaded connection has screw nut (18) on every reciprocating screw thread section, swing groove (20) have all been seted up in (mixing) shaft (7) both sides, swing groove (20) internal rotation is connected with stirring leaf (9), just fixedly connected with gear (21) on stirring leaf (9) lateral wall, the both sides of screw nut (18) all are fixedly connected with rack (19), just rack (19) meshes with gear (21), be equipped with a plurality of closing plates (17) in (7), and every two adjacent closing plates (17) set up on sealing screw (17) under sealing screw (17).

2. The device for preparing high-purity iodine monochloride from crude iodine according to claim 1 is characterized in that two driving rollers (10) are respectively connected to the inner walls of the two sides of the reaction kettle (1) in a rotating way, the two adjacent driving rollers (10) are connected through a driving belt (11), a plurality of hoppers (12) are fixedly arranged on the side wall of the driving belt (11), the hoppers (12) are distributed on the driving belt (11) at equal intervals, a driving groove (13) is formed in the side wall of the reaction kettle (1), and a rotating device for enabling the driving rollers (10) to rotate is arranged in the driving groove (13).

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

4. The device for preparing high-purity iodine monochloride from crude iodine according to claim 3, characterized in that two vibrating plates (6) are rotatably connected to the inner wall of the reaction kettle (1), the vibrating plates (6) are connected to the inner top of the reaction kettle (1) through springs (5), a telescopic cylinder (4) is fixedly arranged at the upper end of the reaction kettle (1), and the telescopic end of the telescopic cylinder (4) penetrates through the inner top of the reaction kettle (1) in a sealing manner and extends into the inner top of the reaction kettle.

5. The device for preparing high-purity iodine monochloride from crude iodine according to claim 4, wherein the rotation connection part of the vibrating plate (6) and the reaction kettle (1) is positioned at the center of the vibrating plate (6), and the telescopic ends of the spring (5) and the telescopic cylinder (4) are respectively arranged at two sides of the vibrating plate (6).

6. A process for preparing high purity iodine monochloride by using crude iodine according to any one of claims 1 to 5, comprising the following preparation steps:

s1, inputting a crude iodine raw material into a reaction container, and ensuring the temperature to be between 35 and 55 ℃;

s2, chlorine: introducing chlorine into the reaction vessel according to the molar ratio of the crude iodine of 1-1.2:1, stirring the chlorine at the same time, and forcing the crude iodine to be uniformly mixed with the chlorine, wherein the reaction and stirring time is 1-5 hours;

s3, absorbing redundant chlorine, pumping the gas in the reaction container into an absorption container, and absorbing the redundant chlorine by using alkali liquor;

s4, filtering and separating, and collecting liquid iodine monochloride after filtering and separating the obtained mixed reaction product.

7. The process for preparing high-purity iodine monochloride from crude iodine according to claim 6, wherein in said step S1, the crude iodine raw material is used to ensure clean and impurity-free raw material, and the feeding temperature is 45 ℃.

8. The process for preparing high purity iodine monochloride from crude iodine according to claim 7, wherein in step S2, chlorine: the molar ratio of crude iodine is 1.05:1, and the stirring time is 2.5 hours.

9. The process for preparing high-purity iodine monochloride from crude iodine according to claim 7, wherein in said step S3, the alkali solution absorbing chlorine gas adopts sodium hydroxide solution, and the mass concentration of said sodium hydroxide solution is 2% -5%.