A device for treating organic waste water in the synthesis of p-acetamidobenzenesulfonyl chloride

Abstract

The utility model relates to the technical field of p-acetylaminobenzenesulfonyl chloride synthesis, and disclose a kind of treatment device of organic wastewater in p-acetylaminobenzenesulfonyl chloride synthesis, the treatment device of organic wastewater in p-acetylaminobenzenesulfonyl chloride synthesis, including reaction kettle, the sidewall of the reaction kettle is fixedly connected with waste sulfuric acid input pipe, the inside of the reaction kettle is provided with adsorption component.The treatment device of organic wastewater in p-acetylaminobenzenesulfonyl chloride synthesis, resin bed that inclines and shakes can constantly change liquid flow direction and resin relative position, prevent resin particle gap blockage or deposition, waste sulfuric acid can more evenly soak resin bed, resin particle surface utilization rate improves, waste acid is more evenly distributed in bed layer, adsorption efficiency is greatly improved, organic matter interception is more sufficient, simultaneously, resin bed that swings can make backwash liquid more evenly penetrate resin particle layer, avoid appearing the dead angle of backwash not thoroughly, resin regeneration is more sufficient.

Description

Technical Field

[0001] This utility model relates to the field of p-acetaminobenzenesulfonyl chloride synthesis technology, specifically to a device for treating organic wastewater in the synthesis of p-acetaminobenzenesulfonyl chloride. Background Technology

[0002] The synthesis of p-acetaminobenzenesulfonyl chloride mainly involves the chlorosulfonation reaction of acetanilide with chlorosulfonic acid as a sulfonating agent, followed by hydrolysis to remove excess chlorosulfonic acid, resulting in a dilute sulfuric acid solution of p-acetaminobenzenesulfonyl chloride. The p-acetaminobenzenesulfonyl chloride and organic waste sulfuric acid are then separated by filtration. However, the product p-acetaminobenzenesulfonyl chloride, some unreacted acetanilide raw material, and the reaction intermediate p-acetaminobenzenesulfonic acid dissolve in the dilute sulfuric acid, resulting in a low yield of p-acetaminobenzenesulfonyl chloride. Furthermore, the large amount of organic waste acid generated is difficult to utilize and can only be treated as organic waste acid.

[0003] According to a method for treating organic waste acid in the synthesis of acetaminobenzenesulfonyl chloride (publication number: CN111392697B), organic waste sulfuric acid is pumped into a macroporous resin bed for adsorption and retention of organic matter to obtain a sulfuric acid solution. The sulfuric acid solution is mixed with an oxidant and introduced into an oxidation reactor for oxidative decomposition. After decolorization, purified sulfuric acid is obtained. The organic matter adsorbed by the resin in the macroporous resin bed is backwashed and desorbed using a backwashing solvent to obtain an eluent.

[0004] However, in actual use, the liquid in the bed often flows through the channel of least resistance, and some resin is hardly contacted. The adsorption efficiency of organic waste acid is low, and the residual organic matter in the effluent is high. More resin or longer residence time is required to achieve the same purification effect. In view of this, we propose a treatment device for organic wastewater in the synthesis of acetaminobenzenesulfonyl chloride. Utility Model Content

[0005] The purpose of this invention is to provide a device for treating organic wastewater in the synthesis of acetaminobenzenesulfonyl chloride, so as to solve the problems mentioned in the background art.

[0006] To achieve the above objectives, this utility model provides the following technical solution: a device for treating organic wastewater from the synthesis of p-acetaminobenzenesulfonyl chloride, comprising a reaction vessel, a waste sulfuric acid input pipe fixedly connected to the side wall of the reaction vessel, a sulfuric acid solution output pipe fixedly connected to the bottom end face of the reaction vessel, and an adsorption assembly disposed inside the reaction vessel, the adsorption assembly comprising:

[0007] Motor 1, the output end of which is fixedly connected to a rotating shaft, the top end face of which is fitted with a diagonal rod, and the top end of which is fixedly connected to a resin bed;

[0008] A crossbar, with ring-shaped frames fitted at both ends of the crossbar;

[0009] A ring-shaped spray frame is provided with a cam on its inner wall. The cam is fixedly connected to a rotating rod, and the top end of the rotating rod is fixedly connected to the output end of a second motor.

[0010] Preferably, the motor is fixedly connected to the bottom end face of the reactor, the rotating shaft is sleeved with the reactor, and a shielding cylinder is fixedly connected to the side wall of the resin bed.

[0011] Preferably, the crossbar and the diagonal bar are sleeved together, and a rotating shaft is fixedly connected to the inner wall of the reactor, and the rotating shaft is sleeved together with the annular frame.

[0012] Preferably, a limiting frame is fixedly connected to the inner wall of the reactor, and the limiting frame is slidably connected to the annular spray frame, thereby limiting the position of the annular spray frame.

[0013] Preferably, the number of annular spray frames is set to several groups, the axes of the several groups of annular spray frames coincide, and the several groups of annular spray frames are connected by connecting pipes.

[0014] Preferably, a flexible hose is fixedly connected to the top end face of the annular spray frame, and the flexible hose is fixedly connected to the liquid inlet pipe. A solvent outlet pipe is fixedly connected to the bottom end face of the reaction vessel, and the eluent is discharged from the reaction vessel through the solvent outlet pipe.

[0015] Preferably, the second motor is fixedly connected to the top end face of the reactor, and the cam is movably connected to the inner wall of the annular spray frame. When the cam rotates, the annular spray frame continuously generates displacement.

[0016] Preferably, an annular pipe is fixedly connected to the bottom end of the inlet pipe, and a lower spray pipe is fixedly connected to the inner wall of the annular pipe. The output end of the lower spray pipe is located between the resin bed and the annular frame.

[0017] Compared with the prior art, this utility model provides a device for treating organic wastewater in the synthesis of p-acetaminobenzenesulfonyl chloride, which has the following beneficial effects:

[0018] 1. This device for treating organic wastewater from the synthesis of acetaminobenzenesulfonyl chloride utilizes an adsorption assembly. The tilted and swaying resin bed continuously changes the direction of liquid flow and the relative position of the resin, preventing clogging or deposition between resin particles. Waste sulfuric acid can more evenly wet the resin bed, increasing the surface utilization rate of the resin particles. Waste acid is more evenly distributed within the bed, significantly improving adsorption efficiency and ensuring more thorough retention of organic matter. Simultaneously, the swaying resin bed allows the backwash liquid to penetrate the resin particle layer more evenly, avoiding dead zones from incomplete backwashing and ensuring more complete resin regeneration. The annular spray frame continuously changes the spray position, and the direction and impact point of the backwash liquid jet constantly change, disturbing the gaps between resin particles. The backwash liquid covers every area of ​​the resin bed, avoiding cleaning dead zones and ensuring more thorough regeneration of the resin particle layer.

[0019] 2. The organic wastewater treatment device in the synthesis of acetaminobenzenesulfonyl chloride uses a bottom spray pipe to rinse the bottom of the resin bed. The liquid jet from below lifts some resin particles, enhancing the loosening and agitation of the resin. The bottom spray pushes the rinsing liquid into the resin layer from bottom to top, allowing the liquid to penetrate the entire bed evenly, resulting in more uniform rinsing and thorough removal of impurities between resin particles. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the main structure of the present utility model;

[0021] Figure 2 This is a schematic diagram of the main cross-sectional structure of the present utility model;

[0022] Figure 3 This is a schematic diagram of the cross-sectional structure of the reaction vessel of this utility model;

[0023] Figure 4 This is a schematic diagram of the resin bed structure of this utility model;

[0024] Figure 5 This is a schematic diagram of the annular spray frame structure of this utility model.

[0025] In the diagram: 1. Reactor; 2. Waste sulfuric acid input pipe; 3. Sulfuric acid solution output pipe; 4. Adsorption assembly; 401. Motor 1; 402. Rotating shaft; 403. Inclined rod; 404. Resin bed; 405. Crossbar; 406. Annular frame; 407. Rotating shaft; 408. Annular spray frame; 409. Flexible hose; 410. Motor 2; 411. Rotating rod; 412. Cam; 5. Liquid inlet pipe; 6. Limiting frame; 7. Solvent output pipe; 8. Annular pipe; 9. Lower spray pipe. Detailed Implementation

[0026] like Figures 1-5As shown, this utility model provides a technical solution: a device for treating organic wastewater in the synthesis of acetaminobenzenesulfonyl chloride, including a reaction vessel 1, a waste sulfuric acid input pipe 2 fixedly connected to the side wall of the reaction vessel 1, a sulfuric acid solution output pipe 3 fixedly connected to the bottom end face of the reaction vessel 1, and an adsorption assembly 4 arranged inside the reaction vessel 1. The adsorption assembly 4 includes a motor 401, a rotating shaft 402, an inclined rod 403, a resin bed 404, a crossbar 405, an annular frame 406, a rotating shaft 407, an annular spray frame 408, a hose 409, a second motor 410, a rotating rod 411, and a cam 412.

[0027] In one embodiment of this utility model, a motor 401 is fixedly connected to the bottom end face of a reaction vessel 1, and a rotating shaft 402 is fixedly connected to the output end of the motor 401. A diagonal rod 403 is sleeved on the top end face of the rotating shaft 402, and a resin bed 404 is fixedly connected to the top end of the diagonal rod 403. The resin bed 404 is a frame divided into many small compartments, and the small compartments are filled with resin particles. The top and bottom of the frame are set with a dense mesh, so that the solution can pass through the dense mesh and contact the resin particles filled in the small compartments, and then fall into the inner bottom of the reaction vessel 1 through the dense mesh at the bottom of the frame. The rotating shaft 402 is sleeved with the reaction vessel 1. A shielding cylinder is fixedly connected to the side wall of the resin bed 404. A ring frame 406 is sleeved at both ends of a crossbar 405, and the crossbar 405 is sleeved with the diagonal rod 403. A rotating shaft 407 is fixedly connected to the inner wall of the reaction vessel 1, and the rotating shaft 407 is sleeved with the ring frame 406.

[0028] A limiting frame 6 is fixedly connected to the inner wall of the reactor 1. The limiting frame 6 is slidably connected to the annular spray frame 408, and the limiting frame 6 limits the movement of the annular spray frame 408. A cam 412 is provided on the inner wall of the annular spray frame 408. The cam 412 is fixedly connected to the rotating rod 411. The top end of the rotating rod 411 is fixedly connected to the output end of the motor 410. Several sets of annular spray frames 408 are provided, and the axes of the several sets of annular spray frames 408 coincide. 408 is connected by a connecting pipe. A hose 409 is fixedly connected to the top end face of the annular spray frame 408. The hose 409 is fixedly connected to the liquid inlet pipe 5. A solvent outlet pipe 7 is fixedly connected to the bottom end face of the reactor 1. The eluent is discharged into the reactor 1 through the solvent outlet pipe 7. The motor 410 is fixedly connected to the top end face of the reactor 1. The cam 412 is movably connected to the inner wall of the annular spray frame 408. When the cam 412 rotates, the annular spray frame 408 continuously moves.

[0029] Organic waste sulfuric acid is fed into reactor 1, causing it to fall onto resin bed 404. Resin bed 404 adsorbs organic matter, while the waste sulfuric acid is discharged from reactor 1 through sulfuric acid solution outlet pipe 3. Motor 401 drives shaft 402 to rotate, causing inclined rod 403 and resin bed 404 to oscillate continuously. Annular frame 406 supports inclined rod 403, ensuring the stability of resin bed 404's oscillation. The tilting and swaying resin bed 404 continuously changes the direction of liquid flow and the relative position of the resin, preventing clogging or deposition between resin particles. Waste sulfuric acid can more evenly wet resin bed 404, improving the surface utilization rate of resin particles, resulting in a more uniform distribution of waste acid within the bed, significantly improving adsorption efficiency, and more thorough retention of organic matter.

[0030] Simultaneously, the oscillating resin bed 404 continuously tilts and agitates the bed layer, causing the liquid path to constantly change. This allows for coverage of more resin particles, enabling the backwash liquid to penetrate the resin particle layer more evenly, avoiding dead zones caused by incomplete backwashing, resulting in more complete resin regeneration and extending resin life. The motor 410 drives the rotating rod 411 and cam 412 to rotate. When the cam 412 rotates, it pushes the annular spray frame 408 to continuously shift. As the annular spray frame 408 is driven by the cam 412, it continuously changes the spray position, causing the backwash liquid jet direction and impact point to constantly change. This disturbs the gaps between resin particles, ensuring that the backwash liquid covers every area of ​​the resin bed 404, avoiding cleaning dead zones, and resulting in more thorough regeneration of the resin particle layer.

[0031] In addition, an annular pipe 8 is fixedly connected to the bottom end of the inlet pipe 5, and a lower spray pipe 9 is fixedly connected to the inner wall of the annular pipe 8. The output end of the lower spray pipe 9 is located between the resin bed 404 and the annular frame 406. The lower spray pipe 9 rinses the bottom of the resin bed 404. The liquid jet from below lifts some resin particles, causing local agitation and enhancing the loosening and agitation of the resin. The bottom spray pushes the rinsing liquid into the resin layer from bottom to top, so that the liquid penetrates the entire bed layer evenly, making the rinsing more uniform. Impurities between the resin particles can be completely removed. With the liquid jetting from both top and bottom, impurities are not easy to remain, and the resin regeneration is more thorough.

[0032] In this invention, during use, organic waste sulfuric acid falls onto the resin bed 404, where it adsorbs the organic matter. The waste sulfuric acid then exits the reactor 1 through the sulfuric acid solution output pipe 3 via the resin bed 404. The resin bed 404 continuously oscillates, constantly changing the direction of liquid flow and the relative position of the resin particles to prevent clogging or deposition between resin particles. This allows the waste sulfuric acid to more evenly wet the resin bed 404, resulting in more thorough retention of organic matter. The oscillating resin bed 404 continuously tilts and agitates the bed, enabling the backwash liquid to penetrate the resin particle layer more evenly and avoiding dead zones where backwashing is incomplete. The annular spray frame 408, driven by the cam 412, continuously changes its spray position, causing the backwash liquid jet direction and impact point to constantly change, resulting in more thorough regeneration of the resin particle layer.

[0033] The present invention has been described in detail above. However, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, any modifications or improvements that do not depart from the spirit of the present invention are within the protection scope of the present invention.

Claims

1. A device for treating organic wastewater from the synthesis of acetaminobenzenesulfonyl chloride, comprising a reactor (1), wherein a waste sulfuric acid input pipe (2) is fixedly connected to the side wall of the reactor (1), and a sulfuric acid solution output pipe (3) is fixedly connected to the bottom end face of the reactor (1), characterized in that: The reactor (1) is equipped with an adsorption assembly (4), which includes: Motor 1 (401), the output end of which is fixedly connected to a rotating shaft (402), the top end face of which is sleeved with a diagonal rod (403), and the top end of the diagonal rod (403) is fixedly connected to a resin bed (404); A crossbar (405), with ring frames (406) sleeved at both ends of the crossbar (405); A ring-shaped spray frame (408) is provided with a cam (412) on its inner wall. The cam (412) is fixedly connected to a rotating rod (411), and the top end of the rotating rod (411) is fixedly connected to the output end of a second motor (410).

2. The device for treating organic wastewater from the synthesis of p-acetaminobenzenesulfonyl chloride according to claim 1, characterized in that: The motor (401) is fixedly connected to the bottom end face of the reactor (1), the rotating shaft (402) is sleeved with the reactor (1), and the side wall of the resin bed (404) is fixedly connected with a shielding cylinder.

3. The device for treating organic wastewater from the synthesis of p-acetaminobenzenesulfonyl chloride according to claim 1, characterized in that: The crossbar (405) is sleeved with the diagonal bar (403), and the inner wall of the reactor (1) is fixedly connected with a rotating shaft (407), which is sleeved with the annular frame (406).

4. The device for treating organic wastewater from the synthesis of p-acetaminobenzenesulfonyl chloride according to claim 1, characterized in that: The inner wall of the reactor (1) is fixedly connected to a limiting frame (6), and the limiting frame (6) is slidably connected to the annular spray frame (408).

5. The device for treating organic wastewater from the synthesis of p-acetaminobenzenesulfonyl chloride according to claim 1, characterized in that: The number of annular spray racks (408) is set in several groups, the axes of the several groups of annular spray racks (408) coincide, and the several groups of annular spray racks (408) are connected by connecting pipes.

6. The device for treating organic wastewater from the synthesis of p-acetaminobenzenesulfonyl chloride according to claim 1, characterized in that: A flexible hose (409) is fixedly connected to the top end face of the annular spray frame (408), and the flexible hose (409) is fixedly connected to the liquid inlet pipe (5). A solvent outlet pipe (7) is fixedly connected to the bottom end face of the reactor (1).

7. The device for treating organic wastewater from the synthesis of p-acetaminobenzenesulfonyl chloride according to claim 1, characterized in that: The second motor (410) is fixedly connected to the top end face of the reactor (1), and the cam (412) is movably connected to the inner wall of the annular spray frame (408).

8. The apparatus for treating organic wastewater from the synthesis of p-acetaminobenzenesulfonyl chloride according to claim 6, characterized in that: The bottom end of the liquid inlet pipe (5) is fixedly connected to an annular pipe (8), and the inner wall of the annular pipe (8) is fixedly connected to a lower spray pipe (9). The output end of the lower spray pipe (9) is located between the resin bed (404) and the annular frame (406).

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