A stirring device for reduction kettle and diaminobenzoic acid reduction method

Abstract

The embodiment of the present application provides a stirring device for a reduction kettle and a diaminobenzoic acid reduction method, which relate to the field of chemical technology. The stirring device for the reduction kettle includes a premixing tank, a connecting tank, a reduction kettle, a driving shaft, a slow injection component and an adjustable stirring component, wherein the slow injection component includes a gear ring, and the driving motor is started to drive the driving shaft to rotate. The premixed additives can be premixed through the slow injection component in the reduction kettle, and can slowly flow into the reduction kettle through the conveying hole for reduction processing, effectively reducing the impact of the violent reaction caused by the reduction reaction on the reduction kettle, providing the practicality of the reduction kettle, and then the adjustable stirring component in the reduction kettle can change the stirring diameter to adjust the mixing effect according to the strength of the reduction reaction, thereby improving the mixing effect of the reduction kettle and the accuracy of the reduction effect.

Description

Technical Field

[0001] The present application relates to the field of chemical technology, and in particular to a stirring device for a reduction kettle and a diaminobenzoic acid reduction method. Background Art

[0002] 3.5-Diaminobenzoic acid is an important chemical intermediate that can be used to synthesize various pharmaceutical and dye products. For example, a series of yellow reactive dyes derived from it can be used as dark yellow dyes or as yellow components in black dyes, and have great market application prospects. 3.5-Diaminobenzoic acid is an important monomer of the new material polyimide film, which is a type of high-temperature resistant new polymer material with excellent comprehensive performance. It is widely used in high-temperature resistant coatings, electromagnetic wires, semiconductor protective layers, flexible printed circuit boards, solar panels and other fields. In addition, 3,5-Diaminobenzoic acid is also an important dye and pharmaceutical intermediate, and a series of yellow reactive dyes can be derived from it.

[0003] The problem with the existing solution is that the existing diaminobenzoic acid needs to be subjected to a reduction reaction during the production process, and most of the reduction reactions require the use of a reduction kettle. The existing reduction kettle pours the mixed material into the reduction kettle at one time during the loading process. Due to the fast pouring speed, the reduction reaction will be too strong, causing damage to the reduction kettle and making subsequent processing inconvenient. Summary of the invention

[0004] The present application aims to solve at least one of the technical problems existing in the prior art. To this end, the present application proposes a stirring device for a reduction kettle and a diaminobenzoic acid reduction method, wherein the reaction materials to be mixed are added into the premixing tank through the top feeding port and the middle feeding port, and then the driving motor is started to drive the driving shaft to rotate, and the premixed additives can be premixed through the slow injection component in the reduction kettle, and can slowly flow into the reduction kettle through the conveying hole for reduction processing, effectively reducing the impact of the violent reaction caused by the reduction reaction on the reduction kettle, providing the practicality of the reduction kettle, and then the adjustable stirring component in the reduction kettle can change the stirring diameter to adjust the mixing effect according to the strength of the reduction reaction, thereby improving the mixing effect of the reduction kettle and the accuracy of the reduction effect.

[0005] The present application provides a stirring device for a reduction kettle, comprising a premixing tank, a connecting tank, a reduction kettle, a driving shaft, a slow injection component and an adjustable stirring component, wherein the slow injection component comprises a gear ring, the gear ring is fixedly connected to the middle part of the inner wall of the premixing tank, the inner side of the gear ring is connected with four evenly distributed driven gears through a latching meshing, the upper and lower ends of each driven gear are fixedly connected with a baffle, the inner side of each driven gear is connected with a driving gear through a latching meshing, the upper and lower surfaces of the driving gear are fixedly connected with a main support plate, the main support plate is located on the inner side of the baffle, and the main support plate and the driving gear are fixedly sleeved on the driving shaft; the adjustable stirring component comprises a fixed transmission plate, movable transmission plates are rotatably installed on both sides of the fixed transmission plate, the fixed transmission plate and the movable transmission plate are rotatably installed together in an X shape, the lower ends of the fixed transmission plate and the movable transmission plate are fixedly connected with L-shaped fixed blocks, and the two side surfaces of each L-shaped fixed block are fixedly connected with L-shaped stirring plates.

[0006] In some technical solutions of the present application, a mounting hole is provided on the upper surface of the connecting tank, a premixing tank is fixedly connected in the mounting hole, and a fixing ring is fixedly connected to the lower end of the premixing tank.

[0007] In some technical solutions of the present application, a middle feeding port is provided on the upper surface of the premixing tank, and a mounting shell is fixedly connected to the upper surface of the premixing tank.

[0008] In some technical solutions of the present application, top feeding ports are provided on both sides of the installation shell, a driving motor is fixedly connected to the upper end of the installation shell, and a partition is fixedly connected to the upper inner wall of the installation shell.

[0009] In some technical solutions of the present application, the output shaft of the driving motor is fixedly connected to a driving shaft, and the driving shaft passes through the premixing tank and extends to the interior of the reduction kettle.

[0010] In some technical solutions of the present application, an adjustable stirring assembly is installed at the lower end of the driving shaft, and the adjustable stirring assembly is located in the reduction kettle.

[0011] In some technical solutions of the present application, delivery holes are provided on both sides of the lower side of the premixing tank, a slow injection assembly is installed inside the lower side of the premixing tank, and the slow injection assembly is connected to the adjustable stirring assembly.

[0012] In some technical solutions of the present application, a reduction kettle is installed below the fixing ring, a water injection hole is arranged on the surface of the reduction kettle, and a water injection ring is arranged outside the water injection hole.

[0013] In some technical solutions of the present application, the water injection ring is fixedly connected to the outer surface of the reduction kettle, and a sealing ring is arranged above the water injection ring.

[0014] In some technical schemes of the present application, each baffle plate has a fixed seat fixedly connected to the upper surface, each fixed seat has a rotating roller fixedly connected to the upper surface, each rotating roller has a stirring plate fixedly connected to both sides, a bearing is installed at the center of the bottom of the premixing tank, a driving shaft is installed in the bearing, an upper short plate is fixedly connected to the lower end of the driving shaft, a limiting shaft is fixedly connected to one side of the lower surface of the upper short plate, a lower long plate is fixedly connected to the lower end of the limiting shaft, a mounting plate is rotatably mounted on the limiting shaft, fixing rods are fixedly connected to both ends of the upper surface of the mounting plate, a sealing plate is fixed to the upper end of each fixing rod, each sealing plate is located outside the conveying hole, and a limiting rod is fixedly connected to the four corners on the inner side of each sealing plate, and each limiting rod is movably mounted on the premixing tank.

[0015] In some technical solutions of the present application, a central shaft is rotatably installed on the upper end of the movable transmission plate, and mounting sheet metals are fixedly connected at both ends of the central shaft. A side extension shaft is installed inside the mounting sheet metal, and an electric push rod output shaft is arranged in the middle of the side extension shaft. A heat-insulating shell is arranged on the outer side of the electric push rod, and the heat-insulating shell is fixedly connected to the lower surface of the lower long plate.

[0016] In some technical solutions of the present application, a diaminobenzoic acid reduction method, specifically the diaminobenzoic acid reduction method comprises the following steps:

[0017] S1. First, prepare 3,5-dinitrobenzoic acid with a percentage content of 99% and a feed amount of 820KG, a percentage content of 95%, a feed amount of 1800KG reduced iron powder, 48KG glacial acetic acid, 24KG alcohol, 280KG soda ash, a percentage content of 70%, a feed amount of 30KG sodium hydrosulfide, 10KG hydrosulfite, a percentage content of 30%, and a feed amount of 600KG hydrochloric acid;

[0018] S2. Add 2000L of clean water into a 20-ton reduction kettle (8) and start stirring. Add 1800KG of reduced iron powder, 48KG of glacial acetic acid and 24KG of alcohol and heat to 90-95°C and keep stirring for 15 minutes. Perform a seepage circle test to obtain an iron powder solution for later use.

[0019] S3, add 3200L of iron sludge washing water to the 6300L reduction kettle (8), start stirring, add 820KG of 3,5-dinitrobenzoic acid, stir for half an hour, measure the pH, adjust the pH in the reduction kettle (8) to 4-5, and obtain 3,5-dinitrobenzoic acid liquid for standby use;

[0020] S4, then start the circulating water, slowly add the 3,5-dinitrobenzoic acid solution prepared in S2 to the iron powder solution in S1 at 93-97°C for 3-4 hours, keep warm for 1 hour after the addition is completed, and take a sample of the reaction solution for testing;

[0021] S5. After passing the test, slowly add 280KG of soda ash, adjust the reaction solution to pH = 9-10, then add 30KG of sodium hydrosulfide, heat to 93-97℃ and keep stirring for 1 hour, then filter the mixture, slowly add the filtrate to the acidification kettle, and repeatedly open the air compressor to dry the iron mud after the filter press is completed, and the filtrate is prepared for neutralization and crystallization;

[0022] S6, then slowly add S4 filtrate under vacuum, add 10 kg of sodium hypochlorite after adding, stir for half an hour, then slowly add 500 L of hydrochloric acid at 50-60 degrees and adjust the pH of the reduction kettle (8) to 3.8-4.0, cool to 25°C after adjustment, re-measure the pH and adjust the pH to 3.8-4.0, then let it stand for 1 hour for filter pressing and air-dry the filter cake, then use 600 L of water for circulating washing, pressing and drying to obtain the finished product;

[0023] S7, put 20 tons of the finished product obtained in S5 into a reduction kettle, add 3300 liters of water and raise the temperature to 60 degrees, adjust the pH in the reduction kettle (8) to 8-9 and stir for half an hour, then filter press and collect the filtrate to obtain iron mud washing water for use, and after washing, bag the iron mud for treatment;

[0024] S8. The pre-mixed additives can be pre-mixed through the slow injection assembly (12) in the reduction kettle (8), and can be slowly flowed into the reduction kettle (8) through the conveying hole (11) for reduction processing, thereby effectively reducing the impact of the violent reaction caused by the reduction reaction on the reduction kettle (8), thereby improving the practicality of the reduction kettle (8);

[0025] S9. The adjustable stirring assembly (15) in the reduction kettle (8) can change the stirring diameter, thereby adjusting the mixing effect according to the strength of the reduction reaction, thereby improving the mixing effect of the reduction kettle (8) and the accuracy of the reduction effect.

[0026] The beneficial effects of the present application are as follows: the reaction materials to be mixed are added into the premixing tank through the top feeding port and the middle feeding port, and then the driving motor is started to drive the driving shaft to rotate. The premixed additives can be premixed through the slow injection component in the reduction kettle, and can slowly flow into the reduction kettle through the conveying hole for reduction processing, thereby effectively reducing the impact of the violent reaction caused by the reduction reaction on the reduction kettle, improving the practicality of the reduction kettle, and then the adjustable stirring component in the reduction kettle can change the stirring diameter to adjust the mixing effect according to the strength of the reduction reaction, thereby improving the mixing effect of the reduction kettle and the accuracy of the reduction effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the embodiments of the present application will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present application and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.

[0028] Figure 1 is a schematic three-dimensional diagram of the overall structure according to an embodiment of the present application;

[0029] Figure 2 is a schematic three-dimensional diagram of the cross-sectional structure of a reduction kettle according to an embodiment of the present application;

[0030] Figure 3 is a schematic three-dimensional diagram of a partial structure of a premixing tank section according to an embodiment of the present application;

[0031] Figure 4 is a schematic three-dimensional diagram of the detailed structure of a reduction kettle according to an embodiment of the present application;

[0032] Figure 5 is a schematic three-dimensional diagram of the combined structure of a slow injection component and an adjustable stirring component according to an embodiment of the present application;

[0033] Figure 6 is a schematic three-dimensional diagram of the overall structure of a slow injection assembly according to an embodiment of the present application;

[0034] Figure 7 is a schematic three-dimensional diagram of the local structure of a slow injection assembly according to an embodiment of the present application;

[0035] Figure 8 It is a schematic three-dimensional diagram of the structure of the slow injection component according to an embodiment of the present application.

[0036] Icons: 1. Drive motor; 2. Mounting shell; 3. Top feeding port; 4. Premixing tank; 5. Middle feeding port; 6. Connecting tank; 7. Fixing ring; 8. Reduction kettle; 9. Water injection ring; 10. Sealing ring; 11. Conveying hole; 12. Slow injection assembly; 13. Water injection hole; 14. Driving shaft; 15. Adjustable stirring assembly; 16. Partition; 17. Mounting hole; 201. Gear ring; 202. Driven gear; 203. Baffle; 204. Fixing seat; 205. Rotating roller; 206 , stirring plate; 207, main support plate; 208, driving gear; 209, bearing; 210, upper short plate; 211, limiting shaft; 212, lower long plate; 213, mounting plate; 214, fixing rod; 215, sealing plate; 216, limiting rod; 501, thermal insulation shell; 502, electric push rod; 503, side extension shaft; 504, mounting sheet metal; 505, center shaft; 506, fixed transmission plate; 507, movable transmission plate; 508, L-shaped fixing block; 509, L-shaped stirring plate. DETAILED DESCRIPTION

[0037] The technical solutions in the embodiments of the present application will be described below in conjunction with the drawings in the embodiments of the present application.

[0038] In order to make the purpose, technical solutions and advantages of the implementation methods of this application clearer, the technical solutions in the implementation methods of this application will be clearly and completely described below in conjunction with the drawings in the implementation methods of this application. Obviously, the described implementation methods are part of the implementation methods of this application, not all of the implementation methods. Based on the implementation methods in this application, all other implementation methods obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0039] Therefore, the following detailed description of the embodiments of the present application provided in the accompanying drawings is not intended to limit the scope of the present application for protection, but merely represents the selected embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present application.

[0040] It should be noted that similar reference numerals and letters denote similar items in the following drawings, and therefore, once an item is defined in one drawing, further definition and explanation thereof is not required in subsequent drawings.

[0041] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise" and the like indicating orientations or positional relationships are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present application.

[0042] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of this application, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0043] In this application, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected or indirectly connected through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0044] In the present application, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may include that the first and second features are in direct contact, or may include that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, a first feature being "above", "above" and "above" a second feature includes that the first feature is directly above and obliquely above the second feature, or simply indicates that the first feature is higher in level than the second feature. A first feature being "below", "below" and "below" a second feature includes that the first feature is directly below and obliquely below the second feature, or simply indicates that the first feature is lower in level than the second feature.

[0045] A stirring device for a reduction kettle according to an embodiment of the present application is described below with reference to the accompanying drawings.

[0046] like Figure 1-Figure 8As shown, a stirring device for a reduction kettle comprises a premixing tank 4, a connecting tank 6, a reduction kettle 8, a driving shaft 14, a slow injection assembly 12 and an adjustable stirring assembly 15, wherein the slow injection assembly 12 comprises a gear ring 201, wherein the gear ring 201 is fixedly connected to the middle of the inner wall of the premixing tank 4, wherein the inner side of the gear ring 201 is connected to four evenly distributed driven gears 202 through a snap-tooth meshing, wherein the upper and lower ends of each driven gear 202 are fixedly connected to a baffle 203, wherein the inner side of each driven gear 202 is connected to a driving gear 208 through a snap-tooth meshing, wherein the upper and lower surfaces of the driving gear 208 are fixedly connected to the driving gear 208. A main support plate 207 is fixedly connected, and the main support plate 207 is located on the inner side of the baffle 203. The main support plate 207 and the driving gear 208 are fixedly sleeved on the driving shaft 14; the adjustable stirring assembly 15 includes a fixed transmission plate 506, and movable transmission plates 507 are rotatably installed on both sides of the fixed transmission plate 506. The fixed transmission plate 506 and the movable transmission plate 507 are rotatably installed together in an X shape. The lower ends of the fixed transmission plate 506 and the movable transmission plate 507 are fixedly connected with L-shaped fixed blocks 508, and each of the two side surfaces of the L-shaped fixed blocks 508 are fixedly connected with L-shaped stirring plates 509.

[0047] According to some embodiments of the present application, Figure 1-Figure 5As shown, a mounting hole 17 is provided on the upper surface of the connecting tank 6, a premixing tank 4 is fixedly connected in the mounting hole 17, a fixing ring 7 is fixedly connected at the lower end of the premixing tank 4, a middle feeding port 5 is provided on the upper surface of the premixing tank 4, a mounting shell 2 is fixedly connected to the upper surface of the premixing tank 4, top feeding ports 3 are provided on both sides of the mounting shell 2, a driving motor 1 is fixedly connected to the upper end of the mounting shell 2, a partition 16 is fixedly connected to the upper inner wall of the mounting shell 2, an output shaft of the driving motor 1 is fixedly connected to a driving shaft 14, the driving shaft 14 passes through the premixing tank 4 and extends to the inside of the reduction kettle 8, an adjustable stirring assembly 15 is installed at the lower end of the driving shaft 14, and the adjustable stirring assembly 15 is located in the reduction kettle 8, conveying holes 11 are provided on both sides below the premixing tank 4, a slow injection assembly 12 is installed inside the lower part of the premixing tank 4, the slow injection assembly 12 is connected to the adjustable stirring assembly 15, the fixing ring A reduction kettle 8 is installed below 7, and a water injection hole 13 is arranged on the surface of the reduction kettle 8. A water injection ring 9 is arranged outside the water injection hole 13, and the water injection ring 9 is fixedly connected to the outer surface of the reduction kettle 8. A sealing ring 10 is arranged above the water injection ring 9. First, the reaction materials to be mixed are added into the premixing tank 4 through the top feeding port 3 and the middle feeding port 5, and then the driving motor 1 is started to drive the driving shaft 14 to rotate. The premixed additives can be premixed through the slow injection component 12 in the reduction kettle 8, and can slowly flow into the reduction kettle 8 through the conveying hole 11 for reduction processing, which effectively reduces the impact of the violent reaction caused by the reduction reaction on the reduction kettle 8, and provides the practicality of the reduction kettle 8. Then, the adjustable stirring component 15 in the reduction kettle 8 can change the stirring diameter, so as to adjust the mixing effect according to the strength of the reduction reaction, thereby improving the mixing effect of the reduction kettle 8 and the accuracy of the reduction effect.

[0048] According to some embodiments of the present application, Figure 6-Figure 7As shown, each baffle 203 is fixedly connected to a fixing seat 204 on the upper surface, each fixing seat 204 is fixedly connected to a rotating roller 205 on the upper surface, each rotating roller 205 is fixedly connected to stirring plates 206 on both sides, a bearing 209 is installed at the center of the bottom of the premixing tank 4, a driving shaft 14 is installed in the bearing 209, an upper short plate 210 is fixedly connected to the lower end of the driving shaft 14, and a limited axis 211 is fixedly connected to one side of the lower surface of the upper short plate 210, the The lower end of the limiting shaft 211 is fixedly connected to a lower long plate 212, and a mounting plate 213 is rotatably mounted on the limiting shaft 211. Both ends of the upper surface of the mounting plate 213 are fixedly connected to fixing rods 214, and a sealing plate 215 is fixed to the upper end of each fixing rod 214. Each sealing plate 215 is located outside the conveying hole 11, and each of the four corners of the inner side of each sealing plate 215 is fixedly connected to a limiting rod 216. Each limiting rod 216 is movably mounted on the premixing tank 4. When the driving shaft 14 rotates, When the driving gear 208 is rotated, the driving gear 208 is connected to the driven gear 202 through the engagement of the teeth, and the driven gear 202 is connected to the gear ring 201 through the engagement of the teeth. When the driving gear 208 rotates, it can drive the driven gear 202 to make a circular motion along the gear ring 201 and to rotate on its own circumference. The driven gear 202 can drive the rotating roller 205 and the stirring plate 206 to rotate to stir and mix the reaction materials in the premixing tank 4. At the same time, the upper short plate 210, the limit shaft 211 and The lower long plate 212 rotates around the driving shaft 14. Since a mounting plate 213 is rotatably mounted on the limiting shaft 211, the mounting plate 213 is connected to a sealing plate 215 via a fixing rod 214. The sealing plate 215 is movably mounted below the premixing tank 4 via a limiting rod 216. This allows the conveying hole 11 on one side to be sealed while the conveying hole 11 on the other side to be exposed, thereby slowing down the discharge of materials into the premixing tank 4, effectively reducing the impact of the violent reaction caused by the reduction reaction on the reduction kettle 8, and providing the reduction kettle 8 with practicality.

[0049] According to some embodiments of the present application, Figure 8As shown, the upper end of the movable transmission plate 507 is rotatably mounted with a central shaft 505, and both ends of the central shaft 505 are fixedly connected with mounting sheet metal 504, and a side extension shaft 503 is installed in the mounting sheet metal 504, and an electric push rod 502 output shaft is arranged in the middle of the side extension shaft 503, and a heat-insulating shell 501 is arranged on the outer side of the electric push rod 502, and the heat-insulating shell 501 is fixedly connected to the lower surface of the lower long plate 212, and when the driving shaft 14 rotates, the lower long plate 212 can be driven. 12 rotates, starts the electric push rod 502 to push the side extension shaft 503 located in the installation sheet metal 504 to move, and can drive the movable transmission plate 507 to rotate around the middle of the fixed transmission plate 506, so as to achieve the effect of adjusting the distance between the L-shaped fixed block 508 and the L-shaped stirring plate 509 at the lower end of the fixed transmission plate 506 and the movable transmission plate 507, and then the dinitrobenzoic acid in the reduction kettle 8 can be stirred and reduced by the L-shaped fixed block 508 and the L-shaped stirring plate 509.

[0050] According to some embodiments of the present application, Figure 1-Figure 8 As shown, a diaminobenzoic acid reduction method, the specific diaminobenzoic acid reduction method comprises the following steps:

[0051] S1. First, prepare 3,5-dinitrobenzoic acid (99% / 820KG), reduced iron powder (95% / 1800KG), glacial acetic acid (48KG), alcohol (24KG), soda ash (280KG), sodium hydrosulfide (70% / 30KG), hydrosulfite (10KG) and hydrochloric acid (30% / 600KG);

[0052] S2, add 2000L of clean water into a 20-ton reduction kettle 8 and start stirring, add 1800KG of reduced iron powder, 48KG of glacial acetic acid and 24KG of alcohol and heat up, heat to 90-95°C and keep stirring for a quarter of an hour, perform a seepage circle test (there is black substance at the intersection of the activation liquid and the sodium hydrosulfide aqueous solution seepage circle in the kettle), and obtain an iron powder solution for standby use;

[0053] S3, add 3200L of iron mud washing water to the 6300L reduction kettle 8, start stirring and add 820KG of 3,5-dinitrobenzoic acid, stir for half an hour and measure the pH, adjust the pH in the reduction kettle 8 to 4-5, and obtain 3,5-dinitrobenzoic acid liquid for standby use;

[0054] S4, then start the circulating water, slowly add the prepared 3,5-dinitrobenzoic acid solution in S2 to the iron powder solution in S1 at 93-97°C for about 3-4 hours, keep warm for 1 hour after the addition is completed, and sample the reaction solution for testing (requirement: use high performance liquid chromatography to determine the content, the main content is more than 94% and there is no nitro compound);

[0055] S5. After passing the test, slowly add 280KG of soda ash, adjust the reaction solution to pH = 9-10, then add 30KG of sodium hydrosulfide, heat to 93-97℃ and keep stirring for 1 hour, then filter the mixture, slowly add the filtrate to the acidification kettle, and repeatedly open the air compressor to dry the iron mud after the filter press is completed, and the filtrate is prepared for neutralization and crystallization;

[0056] S6, then slowly add S4 filtrate under vacuum, add 10KG of sodium hypochlorite after adding, stir for half an hour (the reaction mixture is measured by high performance liquid chromatography, the main content is more than 97%), then slowly add about 500L of hydrochloric acid at 50-60 degrees and adjust the pH of reduction kettle 8 to 3.8-4.0, cool to 25°C after adjustment, re-measure the pH and adjust the pH to 3.8-4.0, then stand for 1 hour for filter pressing and air pressure drying the filter cake, then use 600L of water to circulate, wash, press and dry to obtain the finished product (industrial weight of about 470KG, reduction yield of 80%, total yield of 58%);

[0057] S7, put 20 tons of the finished product obtained in S5 into the reduction kettle, add 3300 liters of water and heat it to 60 degrees, adjust the pH in the reduction kettle 8 to 8-9 and stir for half an hour, perform pressure filtration and collect the filtrate to obtain iron mud washing water for use, and after washing, bag the iron mud for treatment;

[0058] S8. The premixed additives can be premixed through the slow injection assembly 12 in the reduction kettle 8, and can slowly flow into the reduction kettle 8 through the conveying hole 11 for reduction processing, effectively reducing the impact of the violent reaction caused by the reduction reaction on the reduction kettle 8, and improving the practicality of the reduction kettle 8;

[0059] S9. The adjustable stirring assembly 15 in the reduction kettle 8 can change the stirring diameter to adjust the mixing effect according to the strength of the reduction reaction, thereby improving the mixing effect of the reduction kettle 8 and the accuracy of the reduction effect.

[0060] The working principle of this embodiment is:

[0061] First, the reaction materials to be mixed are added into the premixing tank 4 through the top feeding port 3 and the middle feeding port 5, and then the driving motor 1 is started to drive the driving shaft 14 to rotate. When the driving shaft 14 rotates, the driving gear 208 is driven to rotate. The driving gear 208 is connected to the driven gear 202 through the engagement of the latch gears, and the driven gear 202 is connected to the gear ring 201 through the engagement of the latch gears. When the driving gear 208 rotates, the driven gear 202 can be driven to make a circular motion along the gear ring 201 and to rotate on its own. The driven gear 202 can drive the rotating roller 205 and the stirring plate 206 to rotate to stir and mix the reaction materials in the premixing tank 4. At the same time, the upper short plate 210, the limiting shaft 211 and the lower long plate 212 rotate with the driving shaft 14 as the center. Since a mounting plate 213 is rotatably installed on the limiting shaft 211, the mounting plate 213 is connected to the seal through the fixing rod 214 The plate 215 and the sealing plate 215 are movably installed under the premixing tank 4 through the limiting rod 216, so that the conveying hole 11 on one side can be sealed, while the conveying hole 11 on the other side is exposed, so that the material in the premixing tank 4 is discharged slowly, effectively reducing the impact of the violent reaction caused by the reduction reaction on the reduction kettle 8, and providing the practicality of the reduction kettle 8. When the driving shaft 14 rotates, the lower long plate 212 can be driven to rotate, and the electric push rod 502 is started to push the side extension shaft 503 located in the installation sheet metal 504 to move, so that the movable transmission plate 507 can be driven to rotate with the middle part of the fixed transmission plate 506 as the center, so as to achieve the effect of adjusting the distance between the L-shaped fixed block 508 and the L-shaped stirring plate 509 at the lower end of the fixed transmission plate 506 and the movable transmission plate 507, and then the dinitrobenzoic acid in the reduction kettle 8 can be stirred and reduced by the L-shaped fixed block 508 and the L-shaped stirring plate 509.

[0062] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0063] The above description is only an embodiment of the present application and is not intended to limit the scope of protection of the present application. For those skilled in the art, the present application may have various changes and variations. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present application should be included in the scope of protection of the present application. It should be noted that similar reference numerals and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further defined and explained in the subsequent drawings.

[0064] The above is only a specific implementation of the present application, but the protection scope of the present application is not limited thereto. Any technician familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed in the present application, which should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the claims.

Claims

1. A stirring device for a reduction kettle, comprising a premixing tank (4), a connecting tank (6), a reduction kettle (8), a driving shaft (14), a slow injection component (12) and an adjustable stirring component (15), characterized in that: The slow injection assembly (12) comprises a gear ring (201), the gear ring (201) being fixedly connected to the middle of the inner wall of the premixing tank (4), the inner side of the gear ring (201) being connected to four evenly distributed driven gears (202) through a tooth meshing engagement, the upper and lower ends of each driven gear (202) being fixedly connected to a baffle (203), the inner side of each driven gear (202) being connected to a driving gear (208) through a tooth meshing engagement, the upper and lower surfaces of the driving gear (208) being fixedly connected to a main support plate (207), the main support plate (207) being located on the inner side of the baffle (203), and the main support plate (207) and the driving gear (208) being fixedly sleeved on the driving shaft (14); The adjustable stirring assembly (15) comprises a fixed transmission plate (506), movable transmission plates (507) are rotatably mounted on both sides of the fixed transmission plate (506), the fixed transmission plate (506) and the movable transmission plate (507) are rotatably mounted together in an X-shape, the lower ends of the fixed transmission plate (506) and the movable transmission plate (507) are fixedly connected with L-shaped fixing blocks (508), and the two side surfaces of each L-shaped fixing block (508) are fixedly connected with L-shaped stirring plates (509); A fixing seat (204) is fixedly connected to the upper surface of each baffle (203), a rotating roller (205) is fixedly connected to the upper surface of each fixing seat (204), stirring plates (206) are fixedly connected to both sides of each rotating roller (205), a bearing (209) is installed at the center of the bottom of the premixing tank (4), a driving shaft (14) is installed in the bearing (209), an upper short plate (210) is fixedly connected to the lower end of the driving shaft (14), a limiting shaft (211) is fixedly connected to one side of the lower surface of the upper short plate (210), a lower long plate (212) is fixedly connected to the lower end of the limiting shaft (211), a mounting plate (213) is rotatably mounted on the limiting shaft (211), and fixing rods (214) are fixedly connected to both ends of the upper surface of the mounting plate (213), A sealing plate (215) is fixed to the upper end of each fixing rod (214), each sealing plate (215) is located outside the conveying hole (11), and a limiting rod (216) is fixedly connected to the four corners of the inner side of each sealing plate (215), and each limiting rod (216) is movably mounted on the premixing tank (4). A central shaft (505) is rotatably mounted on the upper end of the movable transmission plate (507), and mounting sheet metal (504) is fixedly connected to both ends of the central shaft (505), and a side extension shaft (503) is mounted inside the mounting sheet metal (504), and an output shaft of an electric push rod (502) is arranged in the middle of the side extension shaft (503), and a heat-insulating shell (501) is arranged on the outer side of the electric push rod (502), and the heat-insulating shell (501) is fixedly connected to the lower surface of the lower long plate (212).

2. A stirring device for a reduction kettle according to claim 1, characterized in that: The upper surface of the connecting tank (6) is provided with a mounting hole (17), a premixing tank (4) is fixedly connected in the mounting hole (17), and a fixing ring (7) is fixedly connected at the lower end of the premixing tank (4).

3. A stirring device for a reduction kettle according to claim 2, characterized in that: The upper surface of the premixing tank (4) is provided with a middle feeding port (5), and the upper surface of the premixing tank (4) is fixedly connected to a mounting shell (2).

4. A stirring device for a reduction kettle according to claim 3, characterized in that: Top feeding ports (3) are provided on both sides of the installation shell (2), a driving motor (1) is fixedly connected to the upper end of the installation shell (2), and a partition plate (16) is fixedly connected to the upper inner wall of the installation shell (2).

5. A stirring device for a reduction kettle according to claim 4, characterized in that: The output shaft of the driving motor (1) is fixedly connected to a driving rotating shaft (14), and the driving rotating shaft (14) passes through the premixing tank (4) and extends into the interior of the reduction kettle (8).

6. A stirring device for a reduction kettle according to claim 5, characterized in that: An adjustable stirring assembly (15) is mounted at the lower end of the driving shaft (14), and the adjustable stirring assembly (15) is located in the reduction kettle (8).

7. A stirring device for a reduction kettle according to claim 6, characterized in that: Delivery holes (11) are provided on both sides of the lower part of the premixing tank (4), and a slow injection assembly (12) is installed inside the lower part of the premixing tank (4), and the slow injection assembly (12) is connected to the adjustable stirring assembly (15).

8. A diaminobenzoic acid reduction method, characterized in that: The reduction kettle according to any one of claims 1 to 7 is used with a stirring device, and the specific diaminobenzoic acid reduction method comprises the following steps: S1. First, prepare 3,5-dinitrobenzoic acid with a percentage content of 99% and a feed amount of 820KG, a percentage content of 95%, a feed amount of 1800KG reduced iron powder, 48KG glacial acetic acid, 24KG alcohol, 280KG soda ash, a percentage content of 70%, a feed amount of 30KG sodium hydrosulfide, 10KG hydrosulfite, a percentage content of 30%, and a feed amount of 600KG hydrochloric acid; S2. Add 2000L of clean water into the reduction kettle (8) and start stirring. Add 1800KG of reduced iron powder, 48KG of glacial acetic acid and 24KG of alcohol and heat to 90-95°C and keep stirring for 15 minutes. Perform a seepage circle test to obtain an iron powder solution for later use. S3, add 3200L of iron sludge washing water to the reduction kettle (8), start stirring, add 820KG of 3,5-dinitrobenzoic acid, stir for half an hour, measure the pH, adjust the pH in the reduction kettle (8) to 4-5, and obtain 3,5-dinitrobenzoic acid liquid for standby use; S4, then start the circulating water, slowly add the 3,5-dinitrobenzoic acid solution prepared in S2 to the iron powder solution in S1 at 93-97°C for 3-4 hours, keep warm for 1 hour after the addition is completed, and take a sample of the reaction solution for testing; S5. After passing the test, slowly add 280KG of soda ash, adjust the reaction solution to pH = 9-10, then add 30KG of sodium hydrosulfide, heat to 93-97℃ and keep stirring for 1 hour, then filter the mixture, slowly add the filtrate to the acidification kettle, and repeatedly open the air compressor to dry the iron mud after the filter press is completed, and the filtrate is prepared for neutralization and crystallization; S6, then slowly add S4 filtrate under vacuum, add 10 kg of sodium hypochlorite after adding, stir for half an hour, then slowly add 500 L of hydrochloric acid at 50-60 degrees and adjust the pH of the reduction kettle (8) to 3.8-4.0, cool to 25°C after adjustment, re-measure the pH and adjust the pH to 3.8-4.0, then let it stand for 1 hour for filter pressing and air-dry the filter cake, then use 600 L of water for circulating washing, pressing and drying to obtain the finished product; S7, put 20 tons of the finished product obtained in S5 into a reduction kettle, add 3300 liters of water and raise the temperature to 60 degrees, adjust the pH in the reduction kettle (8) to 8-9 and stir for half an hour, then filter press and collect the filtrate to obtain iron mud washing water for use, and after washing, bag the iron mud for treatment; S8. The pre-mixed additives can be pre-mixed through the slow injection assembly (12) in the reduction kettle (8), and can be slowly flowed into the reduction kettle (8) through the conveying hole (11) for reduction processing, thereby effectively reducing the impact of the violent reaction caused by the reduction reaction on the reduction kettle (8), thereby improving the practicality of the reduction kettle (8); S9. The adjustable stirring assembly (15) in the reduction kettle (8) can change the stirring diameter, thereby adjusting the mixing effect according to the strength of the reduction reaction, thereby improving the mixing effect of the reduction kettle (8) and the accuracy of the reduction effect.

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