Hundred-kilogram continuous production device of o-toluidine sulfone

Abstract

The utility model discloses a hundred-kilogram continuous production device of o-toluidine sulfone, and belongs to the technical field of o-toluidine sulfone production devices. In order to solve the problem that in the existing dibenzothiophene sulfone compound preparation process, acid waste gas generated in the high-temperature reaction and quenching reaction process is not treated, and large pressure is caused to environmental protection work, the production device comprises a feeding device, a reaction device, a quenching device, a product post-treatment device and a tail gas treatment device. The feeding device comprises a material bottle, a feeding pipeline, a feeding valve, a vacuum pipeline, a discharging pipeline, a discharging valve, a vacuum valve, a head tank, a dropwise adding pipeline, a valve, a vacuum pump and a vacuum pump acid gas absorption device; the reaction device is a reaction kettle, the quenching device is a quenching kettle, and the product post-treatment device comprises a material pipe, a valve, a diaphragm pump, a filter press and an air compressor; and the tail gas treatment device comprises a tail gas pipeline, a valve, a spray tower, a fan and a circulating pump.

Description

Technical Field

[0001] The utility model belongs to the technical field of o-tolidine sulfone production equipment, and specifically relates to a 100-kilogram continuous production equipment of o-tolidine sulfone. Specifically, it relates to a kilogram-level to 100-kilogram-level continuous production equipment of 3,7-diamino-2,8-dimethyldibenzothiophene sulfone (including 2,6-dimethyl isomer), especially an acid gas absorption and recovery device in the production process. Background Art

[0002] The raw materials for synthesizing 3,7-diamino-2,8-dimethyldibenzothiophene sulfone (including 2,6-dimethyl isomer) include o-o-toluidine and sulfuric acid or fuming sulfuric acid or chlorosulfonic acid. Acidic gases such as sulfur trioxide or hydrogen chloride are released during the reaction. After the reaction is completed, the reaction system is quenched. In this stage, a large amount of acidic waste gases such as hydrogen chloride or sulfur trioxide are still generated.

[0003] At present, the methods for preparing dibenzothiophene sulfone compounds from biphenyl compounds are reported in patents CN116041363A, CN1528760A and Japanese patent JP 5668333, all of which use fuming sulfuric acid as a sulfonation reagent, use a small amount of reaction raw materials, and only synthesize gram-level products; and none of them treat the acidic waste gas generated during the high-temperature reaction and quenching reaction, which puts great pressure on environmental protection work.

[0004] Therefore, it is necessary to provide a production device that can produce products of kilogram level or above and can recover and treat the acid waste gas generated in the entire production process. Summary of the invention

[0005] Aiming at the problem that the acidic waste gas generated in the high-temperature reaction and quenching reaction process is not treated in the current preparation process of dibenzothiophene sulfone compounds, which causes great pressure on environmental protection work, and there is no production process and device for o-tolidine sulfone above kilogram level, the utility model provides a 100-kilogram continuous production device for o-tolidine sulfone.

[0006] In order to achieve the above purpose, the utility model adopts the following technical solutions:

[0007] A 100 kg continuous production device for o-tolidine sulfone, the production device comprising a feeding device, a reaction device, a quenching device, a product post-processing device and an exhaust gas treatment device;

[0008] The feeding device includes: a material bottle, a feeding pipeline, a feeding valve A, a feeding valve B, a feeding valve C, a feeding valve D, a vacuum pipeline, a discharging pipeline, a discharging valve E, a discharging valve F, a vacuum valve G, a vacuum valve H, a vacuum valve I, a vacuum valve J, and a vacuum valve K; a high-level tank, a dripping pipeline, a valve L, a valve M, a valve N, a vacuum pump, and a vacuum pump acid gas absorption device;

[0009] The reaction device comprises: a reaction kettle;

[0010] The quenching device comprises: a quenching kettle;

[0011] The product post-processing device includes: a material pipe, a valve O, a diaphragm pump, a filter press and an air compressor;

[0012] Furthermore, the exhaust gas treatment device includes: an exhaust gas pipeline, a valve P, a spray tower, a fan and a circulation pump.

[0013] The material bottle is connected to the high-level tank, the reactor and the quenching kettle respectively through the feeding pipeline, and a feeding valve A is installed on the feeding pipeline near one end of the material bottle, a feeding valve B is installed on the feeding pipeline near one end of the high-level tank, a feeding valve C is installed on the feeding pipeline near one end of the reactor, and a feeding valve D is installed on the feeding pipeline near one end of the quenching kettle;

[0014] The vacuum pump is connected to the vacuum pump acid gas absorption device through a pipeline, and the vacuum pump acid gas absorption device is connected to the high-level tank, the reaction kettle and the quenching kettle through vacuum pipelines, and a vacuum valve K is installed on the vacuum pipeline near one end of the vacuum pump acid gas absorption device, a vacuum valve G is installed on the vacuum pipeline between the vacuum valve K and the reaction kettle, a vacuum valve I is installed on the vacuum pipeline near one end of the high-level tank, a vacuum valve H is installed on the vacuum pipeline near one end of the reaction kettle, and a vacuum valve J is installed on the vacuum pipeline near one end of the quenching kettle;

[0015] The reactor is connected to the high-level tank through a discharge pipeline. A discharge valve E is installed on the discharge pipeline near one end of the reactor, and a discharge valve F is installed on the discharge pipeline near one end of the high-level tank.

[0016] The header tank is connected to the reactor and the quenching kettle through a dripping pipeline, a valve L is installed on the dripping pipeline near one end of the reactor, a valve N is installed on the dripping pipeline near one end of the quenching kettle, a valve M is installed on the dripping pipeline between the valve L and the valve N, and the position of the valve M is close to the header tank;

[0017] The quenching kettle is connected to the diaphragm pump through a material pipe, and a valve O is installed on the material pipe between the quenching kettle and the diaphragm pump. The diaphragm pump is connected to the filter press and the air compressor through pipelines respectively.

[0018] Furthermore, the spray tower is connected to the reaction kettle and the quenching kettle respectively through the tail gas pipeline. A valve P is installed on the tail gas pipeline near one end of the spray tower. A circulating pump is provided at the bottom of the spray tower and a fan is provided at the top of the spray tower.

[0019] Furthermore, one side of the reaction kettle is connected to the heating and cooling circulation kettle through a two-way pipeline.

[0020] Furthermore, one side of the quenching kettle is connected to the cooling circulation kettle through a two-way pipeline.

[0021] Furthermore, the reactor is a 30L~500L reactor with stirring function and temperature control and heating function.

[0022] Furthermore, the quenching kettle is a quenching kettle of 100L~500L with stirring and cooling functions.

[0023] Furthermore, the vacuum valve K is a three-way valve.

[0024] Furthermore, the valve M is a three-way valve.

[0025] Compared with the prior art, the utility model has the following advantages:

[0026] (1) It can realize the production of o-tolidine sulfone with high selectivity in the range of kilograms to hundreds of kilograms;

[0027] (2) The acidic waste gases sulfur trioxide and hydrogen chloride released during the reaction in the 30~500L reactor and 100~500L quenching reactor can be effectively recovered and treated.

[0028] (3) In the product production process, all equipment used meets the requirements of scale-up production and plays a guiding role in scale-up production. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 The utility model is a schematic diagram of the structure of an experimental device for producing o-tolidine sulfone.

[0030] Figure numerals: 1, material bottle; 2, high-level tank; 3, reaction kettle; 4, quenching kettle; 5, vacuum pump; 6, vacuum pump acid gas absorption device; 7, diaphragm pump; 8, filter press; 9, air compressor; 10, spray tower; 11, fan; 12, circulation pump; 13, feeding pipeline; 14, vacuum pipeline; 15, discharge pipeline; 16, tail gas pipeline; 17, dripping pipeline; 18, material pipe; 19, feeding valve A; 2 0. Feeding valve B; 21. Feeding valve C; 22. Feeding valve D; 23. Discharging valve E; 24. Discharging valve F; 25. Vacuum valve G; 26. Vacuum valve H; 27. Vacuum valve I; 28. Vacuum valve J; 29. ​​Vacuum valve K; 30. Valve L; 31. Valve M; 32. Valve N; 33. Valve O; 34. Valve P; 35. Heating and cooling circulation kettle; 36. Cooling circulation kettle. DETAILED DESCRIPTION

[0031] In order to further illustrate the technical solution of the present utility model, the present utility model is further described below in conjunction with the accompanying drawings and embodiments. Example 1

[0032] A 100 kg continuous production device for o-tolidine sulfone, the production device comprising a feeding device, a reaction device, a quenching device, a product post-processing device and an exhaust gas treatment device;

[0033] The feeding device includes: a material bottle 1, a feeding pipeline 13, a feeding valve A19, a feeding valve B20, a feeding valve C21, a feeding valve D22, a vacuum pipeline 14, a discharge pipeline 15, a discharge valve E23, a discharge valve F24, a vacuum valve G25, a vacuum valve H26, a vacuum valve I27, a vacuum valve J28, and a vacuum valve K29; a high-level tank 2, a dripping pipeline 17, a valve L30, a valve M31, a valve N32, a vacuum pump 5, and a vacuum pump acid gas absorption device 6;

[0034] The reaction device comprises: a reaction kettle 3;

[0035] The quenching device comprises: a quenching kettle 4;

[0036] The product post-processing device includes: a material pipe 18, a valve O33, a diaphragm pump 7, a filter press 8 and an air compressor 9;

[0037] The tail gas treatment device includes: a tail gas pipeline 16 , a valve P34 , a spray tower 10 , a fan 11 and a circulation pump 12 .

[0038] The material bottle 1 is connected to the high-level tank 2, the reaction kettle 3 and the quenching kettle 4 respectively through the feeding pipeline 13, and a feeding valve A19 is installed on the feeding pipeline 13 near one end of the material bottle 1, a feeding valve B20 is installed on the feeding pipeline 13 near one end of the high-level tank 2, a feeding valve C21 is installed on the feeding pipeline 13 near one end of the reaction kettle 3, and a feeding valve D22 is installed on the feeding pipeline 13 near one end of the quenching kettle 4;

[0039] The vacuum pump 5 is connected to the vacuum pump acid gas absorption device 6 through a pipeline, and the vacuum pump acid gas absorption device 6 is connected to the high-level tank 2, the reaction kettle 3 and the quenching kettle 4 through a vacuum pipeline 14, and a vacuum valve K29 is installed on the vacuum pipeline 14 near one end of the vacuum pump acid gas absorption device 6, a vacuum valve G25 is installed on the vacuum pipeline 14 between the vacuum valve K29 and the reaction kettle 3, a vacuum valve I27 is installed on the vacuum pipeline 14 near one end of the high-level tank 2, a vacuum valve H26 is installed on the vacuum pipeline 14 near one end of the reaction kettle 3, and a vacuum valve J28 is installed on the vacuum pipeline 14 near one end of the quenching kettle 4;

[0040] The reactor 3 is connected to the high-level tank 2 through a discharge pipe 15. A discharge valve E23 is installed on the discharge pipe 15 near one end of the reactor 3, and a discharge valve F24 is installed on the discharge pipe 15 near one end of the high-level tank 2.

[0041] The header tank 2 is connected with the reactor 3 and the quenching reactor 4 through a dripping line 17. A valve L30 is installed on the dripping line 17 near one end of the reactor 3, a valve N32 is installed on the dripping line 17 near one end of the quenching reactor 4, and a valve M31 is installed on the dripping line 17 between the valve L30 and the valve N32, and the position of the valve M31 is close to the header tank 2;

[0042] The quenching kettle 4 is connected to the diaphragm pump 7 through a material pipe 18, and a valve O33 is installed on the material pipe 18 between the quenching kettle 4 and the diaphragm pump 7. The diaphragm pump 7 is connected to the filter press 8 and the air compressor 9 through pipelines respectively.

[0043] Furthermore, the spray tower 10 is connected to the reactor 3 and the quenching reactor 4 respectively through the tail gas pipeline 16. A valve P34 is installed on the tail gas pipeline 16 near one end of the spray tower 10. A circulating pump 12 is provided at the bottom of the spray tower 10, and a fan 11 is provided at the top of the spray tower 10.

[0044] Furthermore, one side of the reaction kettle 3 is connected to the heating and cooling circulation kettle 35 through a two-way pipeline.

[0045] Furthermore, one side of the quenching kettle 4 is connected to the cooling circulation kettle 36 through a two-way pipeline.

[0046] Furthermore, the reactor 3 is a 30L-500L reactor with stirring function and temperature control and heating function.

[0047] Furthermore, the quenching kettle 4 is a quenching kettle of 100L to 500L with stirring and cooling functions.

[0048] Furthermore, the vacuum valve K29 is a three-way valve.

[0049] Furthermore, the valve M31 is a three-way valve.

[0050] The operating procedures of the utility model o-tolidine sulfone production device are as follows:

[0051] Step 1, mixed liquid: open the feeding valve A19, feeding valve B20, vacuum valve G25 and vacuum valve H26, vacuum valve K29 is not connected to the atmosphere, open the vacuum pump 5, make the reactor 3 slightly vacuum through the vacuum line 14, the concentrated sulfuric acid in the material bottle 1 flows into the reactor 3 through the feeding line 13, after the addition is complete, close the feeding valve B20 and vacuum valve H26, open the feeding valve C21 and vacuum valve I27, make the header tank 2 slightly vacuum, the chlorosulfonic acid in the material bottle 1 flows into the header tank 2 through the feeding line 13, after the addition is complete, close all valves. Open valve P34, open the circulating pump 12 of the spray tower 10, vacuum valve K29 is connected to the atmosphere, open vacuum valve G25, vacuum valve I27 and vacuum valve K29, valve M31 connects the header tank 2 with the reactor 3, and the chlorosulfonic acid in the header tank 2 drips into the reactor 3 via the dripping line 17 and mixes with the concentrated sulfuric acid. After mixing is completed, close all valves, open vacuum valve G25, vacuum valve I27, discharge valve E23 and discharge valve F24, and disconnect vacuum valve K29 from the atmosphere. Turn on vacuum pump 5 to make high-level tank 2 slightly vacuumed, and the mixed liquid in reactor 3 flows into high-level tank 2 through discharge pipeline 15. After all transfers are completed, close all valves.

[0052] Step 2, dripping the mixed liquid: first add the raw materials to the reactor 3. Open the vacuum valve G25, vacuum valve I27, valve L30 and valve P34, vacuum valve K29 connects to the air, open the circulation pump 12 and fan 11 of the spray tower 10, valve M31 connects the high-level tank 2 and the 30~500L reactor 3, the liquid in the high-level tank 2 is dripped into the reactor 3 through the dripping pipeline 17, after the dripping is completed, close all valves except valve P34, open the heating and cooling circulation kettle 35, set the specified temperature, start the 30~500L reactor 3 for stirring, start the reaction, and the waste gas generated during the reaction is absorbed by the spray tower 10 for alkali solution.

[0053] Step 3, the reaction liquid is removed: after the reaction is completed, the heating and cooling circulating kettle 35 is set to the cooling mode. After the reaction liquid drops to the specified temperature, the discharge valve E23, the discharge valve F24, the vacuum valve I27, and the vacuum valve G25 are opened, and the vacuum valve K29 is not connected to the atmosphere. The vacuum pump 5 is turned on, and the high-level tank 2 is slightly vacuumed through the vacuum pipeline 14. The reaction liquid in the 30-500L reactor 3 flows to the high-level tank 2 through the discharge pipeline 15. After the reaction liquid is completely transferred, the vacuum valve K29 is connected to the atmosphere, the vacuum pump 5 is turned off, and all valves are closed.

[0054] Step 4, quenching of the reaction liquid: open valve N32 and valve P34, valve M31 connects the high-level tank 2 and the quenching kettle 4, open the cooling circulation kettle 36, and the reaction liquid flows from the high-level tank 2 into the quenching kettle 4 through the dripping pipeline 17, and is quenched in the quenching kettle 4. The quenching exhaust gas is absorbed by the alkaline solution through the spray tower 10. After the quenching is completed, the cooling circulation kettle 36 is closed and all valves are closed.

[0055] Step 5, filter pressing operation: turn on the air compressor 9, open the valve O33, adjust the air inlet pressure of the diaphragm pump 7, and the material is sent to the diaphragm pump 7 through the material pipe 18. The diaphragm pump 7 enters the filter press 8 through the pipeline for filter pressing. After the filter pressing is completed, turn off the air compressor 9 and close the valve O33.

[0056] Further, the reactor 3 is a 30L to 500L reactor with stirring and temperature control heating functions; the quenching kettle 4 is a 100L to 500L quenching kettle with stirring and cooling functions. In this embodiment, a 30L reactor 3 and a 100L quenching kettle 4 are selected.

[0057] The above shows and describes the main features and advantages of the utility model. For those skilled in the art, it is obvious that the utility model is not limited to the details of the above exemplary embodiments, and the utility model can be implemented in other specific forms without departing from the spirit or basic features of the utility model. Therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the utility model is limited by the attached claims rather than the above description, and it is intended that all changes that fall within the meaning and scope of the equivalent elements of the claims are included in the utility model.

[0058] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A 100 kg continuous production device of o-tolidine sulfone, characterized in that: The production device includes a feeding device, a reaction device, a quenching device, a product post-processing device and a tail gas treatment device; The feeding device comprises: a material bottle (1), a feeding pipeline (13), a feeding valve A (19), a feeding valve B (20), a feeding valve C (21), a feeding valve D (22), a vacuum pipeline (14), a discharge pipeline (15), a discharge valve E (23), a discharge valve F (24), a vacuum valve G (25), a vacuum valve H (26), a vacuum valve I (27), a vacuum valve J (28), and a vacuum valve K (29); a high-level tank (2), a dripping pipeline (17), a valve L (30), a valve M (31), a valve N (32), a vacuum pump (5), and a vacuum pump acid gas absorption device (6); The reaction device comprises: a reaction kettle (3); The quenching device comprises: a quenching kettle (4); The product post-processing device comprises: a material pipe (18), a valve O (33), a diaphragm pump (7), a filter press (8) and an air compressor (9); The exhaust gas treatment device comprises: an exhaust gas pipeline (16), a valve P (34), a spray tower (10), a fan (11) and a circulation pump (12); The material bottle (1) is connected to the high-level tank (2), the reaction kettle (3) and the quenching kettle (4) respectively through a feeding pipeline (13), and a feeding valve A (19) is installed on the feeding pipeline (13) near one end of the material bottle (1), a feeding valve B (20) is installed on the feeding pipeline (13) near one end of the high-level tank (2), a feeding valve C (21) is installed on the feeding pipeline (13) near one end of the reaction kettle (3), and a feeding valve D (22) is installed on the feeding pipeline (13) near one end of the quenching kettle (4); The vacuum pump (5) is connected to the vacuum pump acid gas absorption device (6) through a pipeline. The vacuum pump acid gas absorption device (6) is connected to the high-level tank (2), the reaction kettle (3) and the quenching kettle (4) through a vacuum pipeline (14), and a vacuum valve K (29) is installed on the vacuum pipeline (14) near one end of the vacuum pump acid gas absorption device (6), a vacuum valve G (25) is installed on the vacuum pipeline (14) between the vacuum valve K (29) and the reaction kettle (3), a vacuum valve I (27) is installed on the vacuum pipeline (14) near one end of the high-level tank (2), a vacuum valve H (26) is installed on the vacuum pipeline (14) near one end of the reaction kettle (3), and a vacuum valve J (28) is installed on the vacuum pipeline (14) near one end of the quenching kettle (4); The reaction kettle (3) is connected to the high-level tank (2) via a discharge pipeline (15); a discharge valve E (23) is installed on the discharge pipeline (15) near one end of the reaction kettle (3); and a discharge valve F (24) is installed on the discharge pipeline (15) near one end of the high-level tank (2); The high-level tank (2) is connected to the reaction kettle (3) and the quenching kettle (4) via a dripping pipe (17); a valve L (30) is installed on the dripping pipe (17) near one end of the reaction kettle (3); a valve N (32) is installed on the dripping pipe (17) near one end of the quenching kettle (4); a valve M (31) is installed on the dripping pipe (17) between the valve L (30) and the valve N (32); and the valve M (31) is located near the high-level tank (2); The quenching kettle (4) is connected to the diaphragm pump (7) through a material pipe (18), and a valve O (33) is installed on the material pipe (18) between the quenching kettle (4) and the diaphragm pump (7). The diaphragm pump (7) is connected to the filter press (8) and the air compressor (9) through pipelines.

2. The 100 kg continuous production device of o-tolidine sulfone according to claim 1, characterized in that: The spray tower (10) is connected to the reaction kettle (3) and the quenching kettle (4) respectively through an exhaust gas pipeline (16); a valve P (34) is installed on the exhaust gas pipeline (16) near one end of the spray tower (10); a circulation pump (12) is provided at the bottom of the spray tower (10); and a fan (11) is provided at the top of the spray tower (10).

3. The 100 kg continuous production device of o-tolidine sulfone according to claim 1, characterized in that: One side of the reaction kettle (3) is connected to the heating and cooling circulation kettle (35) through a two-way pipeline.

4. The 100 kg continuous production device of o-tolidine sulfone according to claim 1, characterized in that: One side of the quenching kettle (4) is connected to the cooling circulation kettle (36) through a two-way pipeline.

5. The 100 kg continuous production device of o-tolidine sulfone according to claim 1, characterized in that: The reactor (3) is a 30L to 500L reactor with stirring function and temperature control and heating function.

6. The 100 kg continuous production device of o-tolidine sulfone according to claim 1, characterized in that: The quenching kettle (4) is a quenching kettle of 100L to 500L, with stirring and cooling functions.

7. The 100 kg continuous production device of o-tolidine sulfone according to claim 1, characterized in that: The vacuum valve K (29) is a three-way valve.

8. The 100 kg continuous production device of o-tolidine sulfone according to claim 1, characterized in that: The valve M (31) is a three-way valve.

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