CN216910299U - Sulfonation reaction device for 2B acid production - Google Patents
Sulfonation reaction device for 2B acid production Download PDFInfo
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- CN216910299U CN216910299U CN202220146382.9U CN202220146382U CN216910299U CN 216910299 U CN216910299 U CN 216910299U CN 202220146382 U CN202220146382 U CN 202220146382U CN 216910299 U CN216910299 U CN 216910299U
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Abstract
The utility model discloses a sulfonation reaction device for 2B acid production, which comprises a kettle body, a stirrer, a jacket arranged outside the kettle body, a heat conducting oil cavity formed in the space between the jacket and the kettle body, a blocking cylinder fixed in the kettle body and having a hollow cylindrical structure with an upper opening and a lower opening, wherein a gap is reserved between the lower end of the blocking cylinder and the bottom of the kettle body, this clearance forms return flow channel, it forms circulation channel to block the clearance between a section of thick bamboo and the internal wall of cauldron, the lateral wall lower part that blocks a section of thick bamboo is equipped with along blockking a section of thick bamboo axial interval and is the liquid hole that gets rid of that the circumference array distributes, it all is equipped with annular water conservancy diversion limit on the lateral wall to be located the liquid hole outside that gets rid of on the same circumference to block a section of thick bamboo lateral wall, annular water conservancy diversion limit downward sloping sets up and blocks completely and gets rid of the liquid hole, the agitator is located and blocks a section of thick bamboo and is just surrounded by getting rid of the liquid hole, the agitator links to each other with the drive arrangement who fixes at cauldron body top. The utility model has simple structure, uniform material mixing and heating, and can improve the purity and yield of the product.
Description
Technical Field
The utility model relates to the technical field of 2B acid production, in particular to a sulfonation reaction device for 2B acid production.
Background
The 2B acid with the chemical name of 4-amino-2-chlorotoluene-5-sulfonic acid is an important organic pigment intermediate and is mainly used for synthesizing organic pigments such as fast scarlet BBN, fast scarlet BBS, fast scarlet MGP, fast scarlet F5R, fast scarlet 2BL and the like.
The liquid phase sulfonation method is a common process for producing 2B acid, and comprises the main steps of reacting 2B oil with concentrated sulfuric acid in a high-boiling point inert organic solvent (such as 1, 4-dichlorobenzene and the like) to form salt, then carrying out high-temperature dehydration transposition rearrangement, forming an azeotrope by the high-boiling point inert organic solvent and water in the reaction, continuously guiding out the water generated in the reaction to complete the reaction, condensing the azeotrope, then entering a water separator, refluxing the high-boiling point inert organic solvent separated by the water separator again, cooling to below 50 ℃ after the reaction is finished, and recovering the solvent through suction filtration to obtain a crude product for further purification.
At present, high-temperature dehydration transposition rearrangement during 2B acid production is generally carried out in a vertical jacket stirring kettle, heated heat conduction oil is introduced into a jacket of the vertical jacket stirring kettle, for example, application publication No. CN109180537A, a method for preparing 3-chloro-p-toluidine-6-sulfonic acid by a liquid-phase baking method in 2019, 1 month and 11 days of authorized publication No. is adopted, high-purity 2B oil is adopted as a raw material, a compound organic solvent is adopted as a liquid-phase dispersing agent, sulfonation reaction is carried out on the 2B oil and concentrated sulfuric acid in the liquid-phase dispersing agent, and 2B acid is obtained by dehydrating and drying a sulfonation product. In the method, high-temperature dehydration transposition rearrangement is carried out in a baking kettle, namely a conventional vertical jacket stirring kettle, and the method has the following defects: (1) the material mixing and heating are not uniform, and the product purity and yield are influenced; (2) 2B acid is easy to adhere to the bottom and the wall of the kettle, which is not only unfavorable for discharging, but also easy to cause carbonization and influence heat transfer; (3) the generated 2B acid is easy to wrap the outside of the sulfate to form particles, so that the reaction is incomplete, and the yield is influenced.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the problems of the baking kettle in the prior art, and provides the sulfonation reaction device for 2B acid production, which has a simple structure, can uniformly mix and heat materials, and can improve the purity and yield of products.
In order to achieve the purpose, the utility model adopts the following technical scheme: the sulfonation reaction device for producing 2B acid comprises a kettle body, a stirrer and a jacket arranged outside the kettle body, the space between the jacket and the kettle body forms a heat conducting oil cavity, the sulfonation reaction device for 2B acid production further comprises a blocking cylinder, the blocking cylinder is fixed in the kettle body, the blocking cylinder is of a hollow cylindrical structure with an upper opening and a lower opening, a gap is reserved between the lower end of the blocking cylinder and the bottom of the kettle body, the clearance forms a backflow channel, the clearance between the blocking cylinder and the inner wall of the kettle body forms a circulating channel, liquid throwing holes distributed in a circumferential array are arranged at intervals along the axial direction of the blocking cylinder at the lower part of the side wall of the blocking cylinder, annular flow guide edges are arranged on the side wall of the blocking cylinder positioned outside the liquid throwing holes on the same circumference, the annular flow guide edge is arranged in a downward inclined mode and completely blocks the liquid throwing hole, the stirrer is located in the blocking cylinder and is surrounded by the liquid throwing hole, and the stirrer is connected with a driving device fixed to the top of the kettle body. The existing sulfonation reaction kettle for producing 2B acid is optimized and improved, the sulfonation reaction device for producing 2B acid is mainly used for carrying out high-temperature dehydration transposition rearrangement on sulfate, the stirrer is a conventional component in the field, different types or shapes of stirrers can be selected according to actual needs, the stirrer is driven by a driving device such as a speed reduction motor, and the driving device is adopted to rotate the stirrer, so that the conventional technical means in the field are provided; the key point of the utility model is that a blocking cylinder is added, and a liquid throwing hole and an annular flow guide edge are arranged on the blocking cylinder; the materials can be sucked from the bottom of the blocking cylinder and lifted into the blocking cylinder to form rolling disorder flow (laminar flow cannot be formed) under the action of the stirrer, and are thrown out from the liquid throwing hole under the centrifugal action and obliquely guided downwards to the bottom of the kettle through the forced guide of the annular flow guide edge, the generated 2B acid is not easy to adhere to the inner wall of the kettle body due to horizontal pressure, the generated 2B acid is not easy to wrap the outside of sulfate to form particles, and meanwhile, the generated 2B acid cannot rise along the inner wall of the kettle body, so that the materials can be quickly refluxed and lifted into the blocking cylinder, and the circulation time can be shortened; the sulfonation reaction device for producing the 2B acid can realize continuous circulation of materials among the circulation channel, the backflow channel and the blocking cylinder, so that the materials are mixed and heated more uniformly, and the materials can continuously scour the blocking cylinder and the inner wall of the kettle body in the circulation process, and are not easy to adhere to the 2B acid.
The inner wall of the kettle body is provided with a plurality of particle boards at intervals along the circumferential direction of the kettle body, and the side face of the particle board facing the blocking cylinder is provided with prismatic particle parts. The particle board is fixed on the inner wall of the kettle body, so that the heat exchange area between the inner wall of the kettle body and the materials can be increased, and the heating uniformity of the materials is further improved; secondly, the structural strength of the kettle body can be improved, and the kettle body is supported and reinforced; thirdly, the material can be contacted and collided, so that particles are crushed, and the reaction is more sufficient; fourthly, the vortex phenomenon is eliminated, the materials are prevented from spirally rising along the inner wall of the kettle body under the action of centrifugal force, and the circulation time and the effect of the materials among the circulation channel, the backflow channel and the blocking barrel are influenced.
Preferably, the crushed aggregates are triangular prism-shaped or quadrangular prism-shaped. The crushed aggregates are in a triangular prism shape or a quadrangular prism shape, have more edges and corners and have good crushing effect on particles.
Preferably, the particle board and the inner wall of the kettle body are in arc transition. The arc transition between the particle board and the inner wall of the kettle body has no dead angle, small resistance and difficult material accumulation.
Preferably, a plurality of inner spinning plates are arranged at the bottom of the kettle body at intervals along the circumferential direction, an inner spinning channel is formed in a gap between every two adjacent inner spinning plates, the spinning direction of each inner spinning plate is the same as the rotating direction of the stirrer, and an area formed by surrounding the inner end of each inner spinning plate corresponds to the lower end opening of the blocking barrel. In order to prevent the generated 2B acid from adhering to the bottom of the kettle and enable the materials to quickly enter the blocking cylinder, the bottom of the kettle body is provided with the inner vortex sheet, the materials at the bottom of the kettle can be concentrated below the blocking cylinder along the inner vortex flow channel and rise into the blocking cylinder, the scouring force of the materials in the inner vortex flow channel is large and concentrated, and the generated 2B acid is not easy to adhere to the bottom of the kettle.
Preferably, the height of the inner swirler increases from the outer end to the inner end. The height of the inner swirl plate increases from the outer end to the inner end so as to guide the concentrated material upwardly into the baffle cylinder.
Preferably, the bottom of the kettle body is a concave round bottom.
Preferably, the upper part of the side wall of the blocking cylinder is provided with an annular flow baffle, the annular flow baffle is arranged in a downward inclined mode, and circular arc transition is adopted between the annular flow baffle and the blocking cylinder. Under the action of centrifugal force, part of materials in the blocking cylinder can spirally rise along the inner wall of the blocking cylinder to influence the circulation and mixing of the materials, so that the annular flow baffle is arranged on the upper part of the side wall of the blocking cylinder (above the liquid throwing hole of the annular flow baffle), and can block the spirally rising materials and guide the materials to the center of the blocking cylinder again.
Preferably, the bottom of the kettle body is provided with a discharge hole, the top of the kettle body is provided with a feed inlet and a gas phase discharge hole, and the upper part of the kettle body is provided with a solvent return opening. The discharge port, the feed port, the gas phase discharge port and the solvent reflux port are all conventional in the field, the gas phase discharge port is connected with a water distribution device which is of a conventional structure in the field, the water distribution device comprises a distillation column, a condenser, a water distributor and the like, and the solvent obtained by separation of the water distributor flows back into the kettle body through the solvent reflux port.
Preferably, the lower part of the jacket is provided with an oil inlet, and the upper part of the jacket is provided with an oil return port.
Preferably, the blocking cylinder is fixedly connected with the inner wall of the kettle body through connecting plates distributed circumferentially.
Therefore, the utility model has the following beneficial effects:
(1) the continuous circulation of the materials among the circulation channel, the backflow channel and the blocking cylinder can be realized, so that the materials are mixed and heated more uniformly, the generated 2B acid is not easy to wrap the outside of the sulfate to form particles, the materials can continuously wash the inner walls of the blocking cylinder and the kettle body in the circulation process, the 2B acid is not easy to adhere and coke, and the purity and the yield of the product can be improved;
(2) a plurality of particle boards are arranged on the inner wall of the kettle body at intervals along the circumferential direction of the kettle body, and the particle boards can improve the heat exchange area between the inner wall of the kettle body and the materials and further improve the heating uniformity of the materials; the structural strength of the kettle body can be improved, and the kettle body is supported and reinforced; the material can be contacted and collided, so that particles are crushed, and the reaction is more sufficient; the vortex phenomenon can be eliminated, and the material is prevented from spirally rising along the inner wall of the kettle body under the action of centrifugal force, so that the circulation time and the effect of the material between the circulation channel and the backflow channel and the blocking barrel are influenced.
Drawings
Fig. 1 is a cross-sectional view of the present invention.
Fig. 2 is an enlarged view at a in fig. 1.
Fig. 3 is a schematic diagram of the distribution of the particle boards and the inner swirl sheets in the kettle body.
In the figure: the device comprises a kettle body 1, a stirrer 2, a jacket 3, a heat conducting oil cavity 4, a backflow channel 6, a circulating channel 7, a liquid throwing hole 8, an annular flow guide edge 9, a crushed aggregate plate 10, a crushed aggregate part 11, an inner cyclone sheet 12, an inner cyclone flow channel 13, an annular flow baffle plate 14, a discharge hole 15, a feed inlet 16, a gas phase discharge hole 17, a solvent backflow port 18, an oil inlet 19, an oil return port 20, a connecting plate 21 and a driving device 22.
Detailed Description
The utility model is further described with reference to the following figures and detailed description.
The sulfonation reaction device for producing 2B acid as shown in figures 1 and 2 comprises a kettle body 1, a stirrer 2, a jacket 3 and a blocking cylinder 5, wherein the jacket 3 and the blocking cylinder 5 are arranged outside the kettle body, a discharge hole 15 is arranged at the bottom of the kettle body, a feed inlet 16 and a gas phase discharge hole 17 are arranged at the top of the kettle body, a solvent return port 18 is arranged at the upper part of the kettle body, a heat conduction oil cavity 4 is formed in the space between the jacket and the kettle body, an oil inlet 19 is arranged at the lower part of the jacket, an oil return port 20 is arranged at the upper part of the jacket, a plurality of crushed aggregates plates 10 (shown in figure 3) are welded on the inner wall of the kettle body at intervals along the circumferential direction of the kettle body, arc transition is adopted between the crushed aggregates plates and the inner wall of the kettle body, prismatic crushed aggregates parts 11 are arranged on the side surface of the crushed aggregates plates facing the blocking cylinder, the crushed aggregates parts 11 are triangular prism-shaped, the crushed aggregates parts and the crushed aggregates are of an integrated structure, and the blocking cylinder and the inner wall of the kettle body are fixedly connected through connecting plates 21 which are distributed circumferentially, the blocking cylinder is a hollow cylindrical structure with an upper opening and a lower opening, a gap is reserved between the lower end of the blocking cylinder and the bottom of the kettle body, the gap forms a backflow channel 6, the gap between the blocking cylinder and the inner wall of the kettle body forms a circulating channel 7, liquid throwing holes 8 distributed in a circumferential array are axially arranged at intervals on the lower portion of the side wall of the blocking cylinder along the blocking cylinder, an annular flow baffle plate 14 is arranged on the upper portion of the side wall of the blocking cylinder, the annular flow baffle plate is positioned above the liquid throwing holes and is arranged in a downward inclined mode, circular arc transition is adopted between the annular flow baffle plate and the blocking cylinder, annular flow guide edges 9 are arranged on the side wall of the blocking cylinder, positioned on the outer side of the liquid throwing holes on the same circumference, are arranged in a downward inclined mode and completely block the liquid throwing holes, a stirring paddle of the stirrer is positioned in the blocking cylinder and is surrounded by the liquid throwing holes, a rotating shaft of the stirrer is connected with a motor shaft of a driving device 22 (a speed reducing motor) fixed on the top of the kettle body through a coupler, the bottom of the kettle body is set to be a concave round bottom, a plurality of inner spinning disks 12 are arranged at intervals along the circumferential direction at the bottom of the kettle body, an inner spinning flow channel 13 is formed in a gap between every two adjacent inner spinning disks, the spinning direction of each inner spinning disk is the same as the rotating direction of the stirrer, an area formed by surrounding the inner ends of the inner spinning disks corresponds to an opening at the lower end of the blocking cylinder, and the height of each inner spinning disk is gradually increased from the outer end to the inner end.
The operation principle of the utility model is as follows: after materials (a mixed material of sulfate generated by the reaction of 2B and concentrated sulfuric acid and an inert organic solvent) are input into the kettle body, heat conduction oil is introduced into a heat conduction oil cavity, the temperature is raised to a required temperature for dehydration, transposition and rearrangement, water generated by the reaction is continuously taken out by the inert organic solvent, the recovered inert organic solvent flows back into the kettle body through a solvent backflow port, after the reaction is finished, the reaction in the kettle body is cooled to below 50 ℃, and the inert organic solvent is recovered through suction filtration, so that a crude product is further purified; during the reaction, the materials in the kettle body are sucked from the bottom of the blocking cylinder under the action of the stirrer and lifted to the blocking cylinder to form tumbling turbulent flow (laminar flow can not be formed), are thrown out from the liquid throwing hole under the centrifugal action, are guided downwards in an inclined mode to the kettle bottom through the forced guiding of the annular flow guide edge, and are finally concentrated below the blocking cylinder along the internal rotation flow channel and ascend to the blocking cylinder, so that the materials are circulated continuously.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the utility model as set forth in the claims.
Claims (10)
1.2B is sour production with sulfonation reaction device, including the cauldron body (1), agitator (2) and set up in the external clamp sleeve (3) of cauldron, the space between clamp sleeve and the cauldron body forms heat conduction oil pocket (4), characterized in that, 2B is sour production with sulfonation reaction device still includes and blocks a section of thick bamboo (5), block a section of thick bamboo and fix in the cauldron body, block a section of thick bamboo and be upper and lower open-ended hollow cylinder structure, block and leave the clearance between the lower extreme of a section of thick bamboo and the cauldron body bottom, this clearance forms return flow channel (6), block the clearance between a section of thick bamboo and the cauldron body inner wall and form circulation channel (7), the lateral wall lower part that blocks a section of thick bamboo is equipped with along blockking a section of thick bamboo axial interval and is the liquid throwing hole (8) that the circumference array distributes, be located on the liquid throwing hole lateral wall outside on same circumference and block all be equipped with annular water conservancy diversion limit (9), annular water conservancy diversion limit sets up and blocks the liquid throwing hole completely, the stirrer is positioned in the blocking cylinder and is surrounded by the liquid throwing hole, and the stirrer is connected with a driving device (22) fixed at the top of the kettle body.
2. The sulfonation reaction device for producing 2B acid, according to claim 1, wherein a plurality of particle boards (10) are arranged on the inner wall of the kettle body at intervals along the circumferential direction of the kettle body, and prismatic particle parts (11) are arranged on the side surfaces of the particle boards facing the blocking cylinder.
3. The sulfonation reaction device for producing 2B acid according to claim 2, wherein the crushed aggregates have a triangular prism shape or a quadrangular prism shape.
4. The sulfonation reaction device for producing 2B acid, according to claim 2, wherein the particle board and the inner wall of the kettle body form a circular arc transition.
5. The sulfonation reaction device for producing 2B acid according to claim 1, wherein a plurality of inner swirling sheets (12) are arranged at intervals along the circumferential direction at the bottom of the kettle body, an inner swirling flow channel (13) is formed in a gap between every two adjacent inner swirling sheets, the swirling direction of each inner swirling sheet is the same as the rotating direction of the stirrer, an area formed by surrounding the inner ends of the inner swirling sheets corresponds to the lower end opening of the blocking cylinder, and the heights of the inner swirling sheets increase from the outer end to the inner end.
6. The sulfonation reaction device for producing 2B acid according to claim 1, wherein an annular flow baffle (14) is provided at an upper portion of a side wall of the barrier cylinder, the annular flow baffle is disposed to be inclined downward, and an arc transition is provided between the annular flow baffle and the barrier cylinder.
7. The sulfonation reaction device for producing 2B acid according to claim 1, wherein a bottom of the kettle body is a concave round bottom.
8. The sulfonation reaction device for producing 2B acid according to claim 1, wherein a discharge port (15) is formed in the bottom of the kettle body, a feed port (16) and a gas phase discharge port (17) are formed in the top of the kettle body, and a solvent return port (18) is formed in the upper portion of the kettle body.
9. The sulfonation reaction device for producing 2B acid according to claim 1, wherein an oil inlet (19) is provided at a lower portion of the jacket, and an oil return port (20) is provided at an upper portion of the jacket.
10. The sulfonation reaction device for producing 2B acid according to claim 1, wherein the blocking cylinder is fixedly connected with the inner wall of the kettle body through connecting plates (21) which are circumferentially distributed.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220146382.9U CN216910299U (en) | 2022-01-19 | 2022-01-19 | Sulfonation reaction device for 2B acid production |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220146382.9U CN216910299U (en) | 2022-01-19 | 2022-01-19 | Sulfonation reaction device for 2B acid production |
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| CN202220146382.9U Active CN216910299U (en) | 2022-01-19 | 2022-01-19 | Sulfonation reaction device for 2B acid production |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114272882A (en) * | 2022-01-19 | 2022-04-05 | 浙江友联化学工业有限公司 | Sulfonation reaction device is used in sour production of 2B |
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- 2022-01-19 CN CN202220146382.9U patent/CN216910299U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114272882A (en) * | 2022-01-19 | 2022-04-05 | 浙江友联化学工业有限公司 | Sulfonation reaction device is used in sour production of 2B |
| CN114272882B (en) * | 2022-01-19 | 2024-05-07 | 浙江友联化学工业有限公司 | Sulfonation reaction device for 2B acid production |
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