A method for preparing high-purity o-aminothiophenol

Abstract

The invention relates to the technical field of preparation of o-aminothiophenol, in particular to a method for preparing high-purity o-aminothiophenol. The impurity removal equipment involved in the method comprises a fixed frame, a movable loading barrel loaded with an orange-yellow solution is arranged at the inner bottom end of the fixed frame, a plurality of limit bars for limiting the movable loading barrel are arranged near the bottom end of the inner side of the fixed frame, and an impurity removal mechanism is arranged inside the movable loading barrel and rotates, so that the orange-yellow solution inside the movable loading barrel can be driven to rotate, and during the rotation of the solution, an adjusting plate is used to perform turbulence, so that the solution inside the movable loading barrel does not rotate in the form of a vortex, and a connecting piece can be matched to enable the impurity removal mechanism to move in an up-and-down direction during the rotation, so that the activated carbon inside the second filter box can fully contact with the solution at various positions inside the movable loading barrel, so that the impurity removal effect of the activated carbon is better.

Description

Technical Field

[0001] The invention relates to the technical field of o-aminothiophenol preparation, in particular to a method for preparing high-purity o-aminothiophenol. Background Art

[0002] o-Aminothiophenol generally refers to 2-mercaptoaniline, an organic compound with the chemical formula C6H7NS. It is mainly used as a dye raw material, a functional pigment raw material, and a pharmaceutical raw material. When preparing o-aminothiophenol, the required raw materials must first be mixed and heated, and then sodium disulfide is added for a catalytic reaction. The by-products produced during the reaction are removed by distillation to obtain an orange-yellow solution, and then the orange-yellow solution is removed by impurity removal equipment. After toluene phase separation and high-pressure reaction, an o-aminothiophenol mixture is obtained, and finally high-purity o-aminothiophenol is obtained by purification.

[0003] In the process of preparing o-aminothiophenol, when the impurity removal work is performed by the impurity removal equipment, activated carbon is usually added directly to the orange-yellow solution obtained by the reaction. When the activated carbon is added to the solution, the contact between the activated carbon and the solution at various positions inside the container is not sufficient, resulting in the activated carbon being unable to fully play its role, affecting the impurity removal effect on the solution; and when the activated carbon is directly added to the solution, some carbon residues will remain in the solution, resulting in the addition of new impurities during the impurity removal process; at the same time, after the solution is impurity-removed, it needs to be naturally cooled before proceeding to the next step. Since the solution obtained by the reaction is 100° C., it needs to be naturally cooled for a long time after the impurity removal process, which affects the preparation efficiency of high-purity o-aminothiophenol. Summary of the invention

[0004] Therefore, the present invention provides a method for preparing high-purity o-aminothiophenol, which solves the above technical problems.

[0005] The present invention provides a method for preparing high-purity o-aminothiophenol, comprising the following steps:

[0006] S1. Raw material mixing treatment: o-Nitrochlorobenzene, water and Emulsogen are mixed and heated to 70° C. to obtain a mixed solution.

[0007] S2. Catalytic reaction: Add freshly prepared sodium disulfide solution to the mixed solution obtained in step S1 within 4 hours, and heat the reaction mixture at 100° C. for 2 hours.

[0008] S3. Removal of by-products: A small amount of by-product o-chloroaniline generated during the heating reaction in step S2 is removed by steam distillation to obtain an orange-yellow solution.

[0009] S4, impurity removal: the orange-yellow solution obtained in step S3 is subjected to impurity removal by using an impurity removal device in combination with activated carbon.

[0010] S5. Toluene phase separation: the orange-yellow solution after impurity removal is naturally cooled to 20-25°C, toluene is added, and hydrochloric acid is added to adjust the pH value to 6 to separate the toluene phase.

[0011] S6, high pressure reaction: the orange-yellow solution after separation of the toluene phase was added into an autoclave, and water and sodium hydroxide solution were added, and the reaction was carried out at 130°C and a pressure of 3x10 5 The reaction was carried out under 370°C conditions for 4 hours to obtain an o-aminobenzenethiol mixture.

[0012] S7. Purification: Cool the o-aminothiophenol mixture to 20-25° C., adjust the pH value to 5.5 with hydrochloric acid, and distill off the solvent to obtain a yellow oily substance, which is high-purity o-aminothiophenol.

[0013] The impurity removal equipment involved in the above-mentioned step S4 includes a fixed frame, a movable loading bucket loaded with orange-yellow solution is arranged at the inner bottom end of the fixed frame, and a plurality of limit bars for limiting the movable loading bucket are arranged near the bottom end of the inner side of the fixed frame.

[0014] The impurity removal mechanism is used for moving up and down and rotating the orange-yellow solution in the movable loading barrel to remove impurities, and the impurity removal mechanism is arranged on the inner side of the fixed frame.

[0015] A displacement mechanism is used to drive the impurity removal mechanism to move up and down and rotate, the displacement mechanism is arranged on a fixed frame, the bottom end of the displacement mechanism is fixedly connected to a connecting frame, the bottom end of the connecting frame is fixedly connected to the impurity removal mechanism, and a positioning mechanism for limiting the movable loading bucket is arranged on the fixed frame.

[0016] A turbulent cooling mechanism is used for assisting cooling of the orange-yellow solution inside the movable loading barrel. The turbulent cooling mechanism is arranged on the impurity removal mechanism, and an inflation mechanism for conveying cooling gas to the inside of the turbulent cooling mechanism is arranged on the fixed frame.

[0017] The impurity removal mechanism includes a first filter box fixedly connected to the bottom end of the connecting frame, and the four inner walls of the first filter box are fixedly connected to limit baffles, and the second filter box is slidably connected between the four limit baffles. The upper surface of the second filter box is provided with a snap-in groove, and a sealing plate is snap-into the interior of the snap-in groove. The sealing plate slides with the limit baffle on the top inner wall of the second filter box.

[0018] The turbulence cooling mechanism includes two left-right symmetrical transmission parts fixedly connected to the upper surface of the first filter box. A plurality of evenly distributed adjustment plates are hinged on the left, right and rear three sides of the first filter box through hinge shafts. A limiting member is arranged on the second filter box and above the adjustment plate.

[0019] According to an embodiment of the present invention, the displacement mechanism includes an electric slide frame slidably connected to a fixed frame up and down, a drive motor is fixedly connected to the upper surface of the electric slide frame, and a connecting piece is provided on the output shaft of the drive motor.

[0020] According to an embodiment of the present invention, the inflation mechanism includes a cooling gas preparation machine fixedly connected to a fixed frame, an inflation nozzle for replenishing air inside the limiter is arranged on the left side of the rear surface of the cooling gas preparation machine, and an electric telescopic exhaust component for releasing the gas inside the limiter is arranged on the right side of the rear surface of the cooling gas preparation machine.

[0021] According to an embodiment of the present invention, the positioning mechanism includes an electric telescopic rod fixedly connected to a fixed frame, a telescopic end of the electric telescopic rod is provided with a limit push rod that elastically extends forward and backward, a limit sleeve is fixedly connected to the connecting member, and a limit hole corresponding to and adapted to the limit push rod is opened on the circumferential surface of the limit sleeve.

[0022] According to an embodiment of the present invention, the connecting member includes a spline shaft fixedly connected to the output shaft of the driving motor, the bottom end of the spline shaft is slidably connected to a spline sleeve, the top of the spline sleeve is fixedly connected to a cross-shaped adapter frame, and rollers are rotatably connected to the four supporting feet of the cross-shaped adapter frame. An adjustment ring is fixedly connected to the fixed frame and located below the spline shaft, and a plurality of circumferentially distributed limit rods are fixedly connected to the upper surface of the spline sleeve. The top of the limit rod is slidably connected to the spline shaft and is provided with a stop block.

[0023] According to an embodiment of the present invention, the adjustment ring is coaxial with the spline sleeve, the upper surface of the adjustment ring is in an undulating wave shape, and the roller is rollingly connected to the upper surface of the adjustment ring.

[0024] According to an embodiment of the present invention, the transmission member includes a mounting bracket fixedly connected to the upper surface of the first filter box, a valve nozzle is fixedly connected to the upper surface of the mounting bracket, a connecting hose is fixed and penetrated at the bottom end of the valve nozzle, and the connecting hose penetrates the mounting bracket up and down and is fixed and penetrated to an adjustment plate close to the nozzle.

[0025] According to an embodiment of the present invention, the limiting member includes a mounting box fixedly connected to the debris removing mechanism, the top end of the hinge shaft between the adjustment plate and the debris removing mechanism passes through the interior of the mounting box, a transmission box is fixedly connected to the right side of the interior of the mounting box, a rotating disk is rotatably connected to the side of the mounting box, the left side of the transmission box is rotatably connected to two front-and-rear symmetrical bidirectional threaded rods, the left end of the bidirectional threaded rod is rotatably connected to the mounting box, two left-and-right symmetrical limiting arc plates are commonly threadedly connected to the two bidirectional threaded rods, and the hinge shaft of the adjustment plate is located between the two limiting arc plates.

[0026] According to an embodiment of the present invention, the left end of the rotating disk passes through the interior of the installation box and is rotatably connected to the transmission box. The rotating disk drives two bidirectional threaded rods to rotate synchronously and in the same direction on the transmission box through gear transmission inside the transmission box. A connecting pipe is fixed and penetrated between adjacent adjustment plates.

[0027] Technical solutions of the present invention are as follows: 1. The impurity removal mechanism is arranged inside the movable loading barrel and rotates, so that the orange-yellow solution inside the movable loading barrel can be driven to rotate. During the rotation of the solution, the regulating plate is used to perform turbulence, so that the solution does not rotate in the form of a vortex inside the movable loading barrel, and the impurity removal mechanism can be moved up and down in the process of rotation by cooperating with the connecting piece. The activated carbon inside the second filter box can fully contact with the solution at various positions inside the movable loading barrel, so that the impurity removal effect of the activated carbon is better, and the solution is affected by the turbulence effect, which can speed up the cooling time of the solution.

[0028] 2. By nesting the first filter box and the second filter box together, double filtration can prevent the carbon residue produced by the shaking of the activated carbon inside the second filter box from falling into the solution when the activated carbon inside the first filter box removes impurities from the solution, thereby affecting the impurity removal effect of the solution.

[0029] 3. Through the setting of the adjustment plate, cooling air can be introduced into the interior of the adjustment plate through the inflation mechanism before the impurity removal mechanism enters into the interior of the movable loading barrel. After the adjustment plate enters into the solution, the solution in the movable loading barrel can be cooled down by the heat exchange of the cooling gas, so that after the solution is impurities removed, the natural cooling time is shorter, thereby improving the preparation efficiency of high-purity o-aminobenzenethiol. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0031] Figure 1 The present invention provides a flow chart of a method for preparing high-purity o-aminobenzenethiol.

[0032] Figure 2 It is a schematic diagram of the three-dimensional structure of the impurity removal equipment involved in the preparation method of high-purity o-aminobenzenethiol provided by the present invention.

[0033] Figure 3 It is a three-dimensional structural schematic diagram of the fixed frame structure provided by the present invention.

[0034] Figure 4 It is a three-dimensional structural schematic diagram of the displacement mechanism and the inflation mechanism provided by the present invention.

[0035] Figure 5 It is a three-dimensional structural schematic diagram of the spoiler and cooling mechanism provided by the present invention.

[0036] Figure 6 It is a three-dimensional structural schematic diagram of the impurity removal mechanism provided by the present invention.

[0037] Figure 7 It is a three-dimensional structural schematic diagram of the position coordination of the impurity removal mechanism and the movable loading bucket provided by the present invention.

[0038] Figure 8 It is a schematic diagram of the three-dimensional structure of the limiting member provided by the present invention.

[0039] Fig. 9 The present invention provides Figure 8 main view.

[0040] Fig.10 It is a schematic diagram of the three-dimensional structure of the connecting piece provided by the present invention.

[0041] Reference numerals:

[0042] 1. Fixed frame; 2. Displacement mechanism; 3. Inflating mechanism; 4. Limiting strip; 5. Connecting frame; 6. De-impurity mechanism; 7. Movable loading bucket; 8. Turbine cooling mechanism; 9. Positioning mechanism; 21. Electric sliding frame; 22. Driving motor; 23. Connecting piece; 31. Inflating nozzle; 32. Cooling gas preparation machine; 33. Electric telescopic exhaust piece; 61. First filter box; 62. Second filter box; 63. Limiting baffle; 64. Snap-in groove; 65. Blocking plate; 81. Transmission Transmission piece; 82, adjustment plate; 83, limit piece; 91, electric telescopic rod; 92, limit push rod; 93, limit sleeve; 231, spline shaft; 232, limit pull rod; 233, cross adapter frame; 234, spline sleeve; 235, roller; 236, adjustment ring; 811, valve; 812, mounting bracket; 813, connecting hose; 831, two-way threaded rod; 832, mounting box; 833, limit arc plate; 834, rotating disk; 835, transmission box. DETAILED DESCRIPTION

[0043] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without violating the connotation of the present invention, so the present invention is not limited by the specific embodiments disclosed below.

[0044] like Figure 1 , Figure 2 and Figure 3 As shown, a method for preparing high-purity o-aminobenzenethiol comprises the following steps:

[0045] S1. Raw material mixing treatment: o-Nitrochlorobenzene, water and Emulsogen are mixed and heated to 70° C. to obtain a mixed solution.

[0046] S2. Catalytic reaction: freshly prepared sodium disulfide solution (prepared from sodium sulfide, sulfur, sodium hydroxide solution and water) is added to the mixed solution obtained in step S1 within 4 hours, and the reaction mixture is heated at 100° C. for 2 hours.

[0047] S3. Removal of by-products: A small amount of by-product o-chloroaniline generated during the heating reaction in step S2 is removed by steam distillation to obtain an orange-yellow solution.

[0048] S4, impurity removal: the orange-yellow solution obtained in step S3 is subjected to impurity removal by using an impurity removal device in combination with activated carbon.

[0049] S5. Toluene phase separation: the orange-yellow solution after impurity removal is naturally cooled to 20-25°C, toluene is added, and hydrochloric acid is added to adjust the pH value to 6 to separate the toluene phase.

[0050] S6, high pressure reaction: the orange-yellow solution after separation of the toluene phase was added into an autoclave, and water and sodium hydroxide solution were added, and the reaction was carried out at 130°C and a pressure of 3x10 5 The reaction was carried out under 370°C conditions for 4 hours to obtain an o-aminobenzenethiol mixture.

[0051] S7. Purification: Cool the o-aminothiophenol mixture to 20-25° C., adjust the pH value to 5.5 with hydrochloric acid, and distill off the solvent to obtain a yellow oily substance, which is high-purity o-aminothiophenol.

[0052] The impurity removal equipment involved in the above-mentioned step S4 includes a fixed frame 1, a movable loading barrel 7 loaded with orange-yellow solution is arranged at the inner bottom end of the fixed frame 1, and a plurality of limit bars 4 for limiting the movable loading barrel 7 are arranged near the bottom end of the inner side of the fixed frame 1.

[0053] The impurity removal mechanism 6 is used for moving up and down and rotating the orange-yellow solution in the movable loading bucket 7 to remove impurities. The impurity removal mechanism 6 is arranged on the inner side of the fixed frame 1.

[0054] A displacement mechanism 2 is used to drive the impurity removing mechanism 6 to move up and down and rotate. The displacement mechanism 2 is arranged on a fixed frame 1. The bottom end of the displacement mechanism 2 is fixedly connected with a connecting frame 5. The bottom end of the connecting frame 5 is fixedly connected to the impurity removing mechanism 6. A positioning mechanism 9 for limiting the movable loading bucket 7 is arranged on the fixed frame 1.

[0055] The turbulent cooling mechanism 8 is used for assisting in cooling the orange-yellow solution inside the movable loading barrel 7. The turbulent cooling mechanism 8 is arranged on the impurity removal mechanism 6. The fixed frame 1 is provided with an inflation mechanism 3 for conveying cooling gas to the inside of the turbulent cooling mechanism 8.

[0056] like Figure 5 and Figure 6 As shown, the impurity removal mechanism 6 includes a first filter box 61 fixedly connected to the bottom end of the connecting frame 5, and the four inner walls of the first filter box 61 are fixedly connected with limit baffles 63, and the second filter box 62 is slidably connected between the four limit baffles 63. The upper surface of the second filter box 62 is provided with a snap-in groove 64, and the inside of the snap-in groove 64 is snap-connected with a sealing plate 65, and the sealing plate 65 is slidably matched with the limit baffle 63 on the top inner wall of the second filter box 62.

[0057] like Figure 5 and Figure 6As shown, the first filter box 61 and the second filter box 62 can be kept relatively fixed by limiting bolts (not shown in the figure). When the second filter box 62 slides to the inside of the first filter box 61, the limiting baffle 63 on the inner wall of the top end of the first filter box 61 presses the sealing plate 65 into the inside of the snap-in groove 64.

[0058] like Figure 5 As shown, the turbulence cooling mechanism 8 includes two left-right symmetrical transmission parts 81 fixedly connected to the upper surface of the first filter box 61, and a plurality of evenly distributed adjustment plates 82 are hinged on the left and right rear three sides of the first filter box 61 through hinge shafts, and a limiting part 83 is arranged on the second filter box 62 and above the adjustment plate 82.

[0059] like Figure 4 As shown, the inflation mechanism 3 includes a cooling gas preparation machine 32 fixedly connected to the fixed frame 1, and an inflation nozzle 31 for replenishing air inside the limiter 83 is arranged on the left side of the rear surface of the cooling gas preparation machine 32, and an electric telescopic exhaust member 33 for releasing the gas inside the limiter 83 is arranged on the right side of the rear surface of the cooling gas preparation machine 32.

[0060] like Figure 4 As shown, the transmission member 81 includes a mounting bracket 812 fixedly connected to the upper surface of the first filter box 61, the upper surface of the mounting bracket 812 is fixedly connected to a valve mouth 811, the bottom end of the valve mouth 811 is fixed and penetrated with a connecting hose 813, the connecting hose 813 penetrates the mounting bracket 812 up and down and is fixed and penetrated with an adjustment plate 82 close to the mouth.

[0061] During specific use, the preparation work is first started. The cooling gas preparation machine 32 transports cooling gas to the interior of the adjustment plate 82 through the inflation nozzle 31 and the valve nozzle 811 through the connecting hose 813. Since a connecting pipe is provided between adjacent adjustment plates 82, the cooling gas can be transported to the interior of multiple adjustment plates 82. While transporting cooling gas to the interior of the adjustment plate 82, the first filter box 61 is taken out from the interior of the second filter box 62, the sealing plate 65 on the snap-in groove 64 is removed, and a certain amount of activated carbon is filled into the interior of the second filter box 62 from the position of the snap-in groove 64.

[0062] After filling, the sealing plate 65 is re-engaged in the engaging groove 64, and the second filter box 62 is re-inserted into the interior of the first filter box 61. The second filter box 62 can be limited by cooperating with a plurality of limiting baffles 63, and at the same time, a certain distance of gap is created between the second filter box 62 and the first filter box 61, so that the subsequent solution can smoothly pass through the interior of the first filter box 61 and the second filter box 62. At the same time, the limiting baffle 63 on the inner wall of the top of the first filter box 61 cooperates with the sealing plate 65 to be pressed inside the engaging groove 64 after the second filter box 62 is inserted into the interior of the first filter box 61, and finally the second filter box 62 is fixed to the interior of the first filter box 61 by the limiting bolts.

[0063] like Figure 4 As shown, the displacement mechanism 2 includes an electric sliding frame 21 slidably connected to the fixed frame 1 up and down, a driving motor 22 is fixedly connected to the upper surface of the electric sliding frame 21, and a connecting member 23 is provided on the output shaft of the driving motor 22.

[0064] like Figure 4 and Figure 7 As shown, the positioning mechanism 9 includes an electric telescopic rod 91 fixedly connected to the fixed frame 1, and a limit push rod 92 that can elastically extend and retract forward and backward is provided on the telescopic end of the electric telescopic rod 91. A limit sleeve 93 is fixedly connected to the connecting member 23, and a limit hole (not shown in the figure) corresponding to and adapted to the limit push rod 92 is opened on the circumferential surface of the limit sleeve 93.

[0065] During specific use, after the preparation work is completed, the electric slide frame 21 moves downward on the fixed frame 1, and at the same time, the electric telescopic rod 91 contracts to cancel the limit on the connecting piece 23. The electric slide frame 21 drives the first filter box 61 to move downward through the connecting piece 23 until the first filter box 61 moves to the middle position of the solution inside the movable loading bucket 7. Then, the movement of the electric slide frame 21 is stopped. At this time, the driving motor 22 rotates through the connecting piece 23 to drive the first filter box 61 to rotate inside the movable loading bucket 7, while performing up and down displacements.

[0066] After the first filter box 61 enters into the solution, the adjustment plate 82 exchanges heat with the solution through the internal cooling gas, and assists in cooling the solution inside the movable loading barrel 7. At the same time, the adjustment plate 82 is limited by the limit member 83 so that the adjustment plate 82 can be in a deflection direction, so that when the first filter box 61 rotates, the adjustment plate 82 can disturb the solution inside the movable loading barrel 7 during the rotation process, so that the solution can fully contact the activated carbon inside the second filter box 62.

[0067] like Figure 8 and Fig. 9As shown, the limiting member 83 includes an installation box 832 fixedly connected to the impurity removing mechanism 6, the top end of the hinge shaft between the adjusting plate 82 and the impurity removing mechanism 6 passes through the interior of the installation box 832, a transmission box 835 is fixedly connected to the right side of the interior of the installation box 832, a rotating disk 834 is rotatably connected to the side of the installation box 832, and two front-to-back symmetrical bidirectional threaded rods 831 are rotatably connected to the left side of the transmission box 835, the left end of the bidirectional threaded rod 831 is rotatably connected to the installation box 832, and two left-right symmetrical limiting arc plates 833 are commonly threadedly connected to the two bidirectional threaded rods 831, the hinge shaft of the adjusting plate 82 is located between the two limiting arc plates 833, the left end of the rotating disk 834 passes through the interior of the installation box 832 and is rotatably connected to the transmission box 835, and the rotating disk 834 drives the two bidirectional threaded rods 831 to rotate synchronously in the same direction on the transmission box 835 through the gear transmission inside the transmission box 835 (not shown in the figure), and a connecting pipe is fixed and penetrated between adjacent adjusting plates 82.

[0068] During specific use, when limiting the adjustment plate 82 by the limiting member 83, first adjust the deflection position of the adjustment plate 82, and then rotate the rotating disk 834 to cooperate with the gear transmission inside the transmission box 835 to drive the two bidirectional threaded rods 831 to rotate synchronously, so that the two limiting arc plates 833 move toward each other. With the continuous movement of the two limiting arc plates 833, the hinge axis between the adjustment plate 82 and the first filter box 61 can be limited, so that the position of the adjustment plate 82 can remain unchanged after adjustment.

[0069] It should be noted that, according to different usage requirements, different deflection positions of the adjustment plates 82 can be adjusted. When all the adjustment plates 82 are in a vertical state with the first filter box 61, the rotation of the first filter box 61 can drive the solution inside the movable loading barrel 7 to the greatest extent. The solution inside the movable loading barrel 7 rotates synchronously with the first filter box 61. This situation is suitable for assisting in mixing the solution more evenly during the process of removing impurities from the solution; when the adjustment plates 82 on the left and right sides of the first filter box 61 are deflected in opposite directions, the first filter box 61 drives the adjustment plates 82 to rotate inside the movable loading barrel 7, and the adjustment plates 82 play a turbulent role. This situation is suitable for higher-precision impurity removal work, and can make the solution more fully contact with the activated carbon.

[0070] like Fig.10As shown, the connecting member 23 includes a spline shaft 231 fixedly connected to the output shaft of the driving motor 22, the bottom end of the spline shaft 231 is slidably connected to a spline sleeve 234, the top of the spline sleeve 234 is fixedly connected to a cross-shaped adapter frame 233, and rollers 235 are rotatably connected to the four supporting feet of the cross-shaped adapter frame 233. An adjusting ring 236 is fixedly connected to the fixed frame 1 and located below the spline shaft 231. A plurality of circumferentially distributed limiting rods 232 are fixedly connected to the upper surface of the spline sleeve 234. The top of the limiting rod 232 is slidably connected to the spline shaft 231 and is provided with a stopper. The adjusting ring 236 is coaxial with the spline sleeve 234, and the upper surface of the adjusting ring 236 is wavy and undulating. The roller 235 is rollingly connected to the upper surface of the adjusting ring 236.

[0071] During specific use, when the driving motor 22 drives the first filter box 61 to rotate through the connecting piece 23, when the electric slide frame 21 moves to the specified position, the roller 235 contacts the upper surface of the adjusting ring 236. At this time, as the driving motor 22 rotates, the spline shaft 231 is driven to rotate synchronously. The spline shaft 231 drives the first filter box 61 to rotate synchronously through the spline sleeve 234. When the spline sleeve 234 starts to rotate, the cross-shaped adapter frame 233 on the spline sleeve 234 cooperates with the roller 235 to rotate in contact with the upper surface of the adjusting ring 236. Since the upper surface of the adjusting ring 236 is a wavy setting that undulates up and down, during the rotation of the spline sleeve 234.

[0072] When the cross-shaped adapter frame 233 moves from a high position to a low position on the upper surface of the adjustment ring 236, the spline sleeve 234 is displaced downward during the rotation, and vice versa, the spline sleeve 234 is displaced upward during the rotation, thereby achieving repeated up and down displacement during the rotation of the spline sleeve 234. At the same time, the setting of the roller 235 can make the sliding between the cross-shaped adapter frame 233 and the adjustment ring 236 smoother.

[0073] When the impurity removal work is completed, the drive of the drive motor 22 is stopped, and the electric slide frame 21 moves upward. At this time, the drive motor 22 drives the spline sleeve 234 to move upward through the spline shaft 231, and the spline shaft 231 generates an upward pulling force on the spline sleeve 234 through the setting of the limit pull rod 232, so as to lift the first filter box 61 upward. At this time, the first filter box 61 continues to rotate under the action of inertia. When the lower surface of the second filter box 62 leaves the solution, the movement of the electric slide frame 21 is stopped, and the first filter box 61 rotating under the action of inertia throws out the solution inside it.

[0074] When the first filter box 61 stops rotating, the electric sliding frame 21 continues to move upward to its original position, and then the staff member turns and rotates, and at the same time extends the electric telescopic rod 91, and the limit push rod 92 contacts the circumferential surface of the limit sleeve 93 until the limit push rod 92 is compressed into the inside of the electric telescopic rod 91. As the staff member continues to turn, when the limit hole on the limit sleeve 93 rotates to the overlapping position with the limit push rod 92, since the limit push rod 92 and the telescopic end of the electric telescopic rod 91 are elastically slidably connected, the limit push rod 92 is elastically slidably connected to the telescopic end of the electric telescopic rod 91. 2 is pushed into the limiting hole of the limiting sleeve 93 to limit the spline sleeve 234, and the first filter box 61 is restored to its original position. While the air filling nozzle 31 is refilling the cooling gas into the adjusting plate 82, the electric telescopic exhaust member 33 is extended to the right side of the valve 811 (the principle of the valve 811 is the same as that of the existing automobile valve) to release the gas inside the adjusting plate 82. At the same time, the solution that has been cleaned is transferred to the next process through the movable loading barrel 7. The above steps can be repeated to carry out the next solution cleansing work.

[0075] Working principle: During specific use, the orange-yellow solution obtained by removing the by-products is first transferred to the bottom of the first filter box 61 through the movable loading barrel 7, and the movable loading barrel 7 is limited by a plurality of limit bars 4, so that the movable loading barrel 7 is located directly below the first filter box 61 after being clamped between the plurality of limit bars 4, and then the cooling gas is filled into the interior of the adjustment plate 82 through the inflation nozzle 31 in cooperation with the transmission member 81, and a certain amount of activated carbon is put into the interior of the second filter box 62, and then the first filter box 61 is pushed downward to the middle position of the solution in the movable loading barrel 7 by the electric slide frame 21, and the driving motor 22 drives the impurity removal mechanism 6 to rotate in the movable loading barrel 7 through the connecting member 23, and starts to remove impurities from the solution in the movable loading barrel 7, and at the same time, during the rotation of the impurity removal mechanism 6, the adjustment plate 82 exchanges heat with the solution through the cooling gas inside it, thereby assisting in cooling the solution.

[0076] When the impurity removal work is completed, the driving of the driving motor 22 is stopped, and the impurity removal mechanism 6 is lifted up by the electric slide frame 21. At this time, the impurity removal mechanism 6 continues to rotate under the action of inertia. When the lower surface of the second filter box 62 leaves the solution, the movement of the electric slide frame 21 is stopped. The impurity removal mechanism 6 rotating under the action of inertia throws out the solution inside it. When the impurity removal mechanism 6 stops rotating, it continues to move upward to its original position through the electric slide frame 21, and then the staff turns it to rotate and cooperates with the positioning mechanism 9 to restore the impurity removal mechanism 6 to its original position. At the same time, the solution that has completed impurity removal is transferred to the next process through the movable loading bucket 7. Repeating the above steps can carry out the next solution impurity removal work.

[0077] In the description of the present invention, it is to be understood that the terms “center”, “longitudinal”, “lateral”, “length”, “width”, “thickness”, “up”, “down”, “front”, “back”, “left”, “vertical”, “horizontal”, “top”, “bottom”, “inside”, “outside”, “clockwise”, “counterclockwise”, “axial”, “radial”, “circumferential”, etc., 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 invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0078] In addition, the terms "first", "second", "number one", "number two" 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. Therefore, the features defined as "first", "second", "number one", "number two" may explicitly or implicitly include at least one of the features. In the description of the present invention, the meaning of "multiple" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0079] In the present invention, 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 a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0080] The embodiments of this specific implementation method are all preferred embodiments of the present invention, and are not intended to limit the protection scope of the present invention. Therefore, any equivalent changes made based on the structure, shape, and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing high-purity o-aminothiophenol, characterized in that: The following steps are involved: S1. Raw material mixing treatment: o-nitrochlorobenzene, water and Emulsogen are mixed and heated to 70° C. to obtain a mixed solution; S2, catalytic reaction: the mixed solution obtained in step S1 is added with a freshly prepared sodium disulfide solution within 4 hours, and the mixture is heated at 100° C. for 2 hours; S3, by-product removal: a small amount of by-product o-chloroaniline generated during the heating reaction in step S2 is removed by steam distillation to obtain an orange-yellow solution; S4, impurity removal: the orange-yellow solution obtained in step S3 is subjected to impurity removal by using an impurity removal device in combination with activated carbon; S5, toluene phase separation: the orange-yellow solution after impurity removal is naturally cooled to 20-25°C, toluene is added, and hydrochloric acid is added to adjust the pH value to 6 to separate the toluene phase; S6, high pressure reaction: the orange-yellow solution after separation of the toluene phase was added into an autoclave, and water and sodium hydroxide solution were added, and the reaction was carried out at 130°C and a pressure of 3x10 5 The reaction was carried out under the condition of Pa for 4 hours to obtain an o-aminobenzenethiol mixture; S7, purification: cooling the o-aminothiophenol mixture to 20-25° C., adjusting the pH value to 5.5 with hydrochloric acid, and distilling off the solvent to obtain a yellow oily substance, which is high-purity o-aminothiophenol; The impurity removal equipment involved in the above step S4 includes a fixed frame, a movable loading bucket loaded with orange-yellow solution is arranged at the inner bottom of the fixed frame, and a plurality of limit bars for limiting the movable loading bucket are arranged near the inner bottom of the fixed frame; A cleaning mechanism for removing impurities from the orange-yellow solution in the movable loading barrel by moving it up and down and rotating it, the cleaning mechanism being arranged on the inner side of the fixed frame; A displacement mechanism for driving the impurity removal mechanism to move up and down and rotate, the displacement mechanism is arranged on a fixed frame, the bottom end of the displacement mechanism is fixedly connected to a connecting frame, the bottom end of the connecting frame is fixedly connected to the impurity removal mechanism, and a positioning mechanism for limiting the movable loading bucket is arranged on the fixed frame; A turbulent cooling mechanism for assisting cooling of the orange-yellow solution in the movable loading barrel, which is arranged on the impurity removal mechanism, and an air charging mechanism for conveying cooling gas to the interior of the turbulent cooling mechanism is arranged on the fixed frame; The impurity removal mechanism includes a first filter box fixedly connected to the bottom end of the connecting frame, and the four inner walls of the first filter box are fixedly connected to the limit baffles, and the four limit baffles are slidably connected to the second filter box, and the upper surface of the second filter box is provided with a clamping groove, and the sealing plate is clamped inside the second filter box, and the sealing plate is slidably matched with the limit baffle on the inner wall of the top end of the second filter box; The turbulence cooling mechanism includes a limiter disposed on the first filter box and above the adjustment plate; The displacement mechanism comprises an electric sliding frame connected to the fixed frame in an up-and-down sliding manner, a driving motor is fixedly connected to the upper surface of the electric sliding frame, and a connecting piece is arranged on the output shaft of the driving motor; The inflation mechanism includes a cooling gas preparation machine fixedly connected to the fixed frame, a gas filling nozzle for replenishing gas inside the limiter is arranged on the left side of the rear surface of the cooling gas preparation machine, and an electric telescopic exhaust member for releasing gas inside the limiter is arranged on the right side of the rear surface of the cooling gas preparation machine; The impurity removal mechanism is arranged inside the movable loading barrel and rotates, so that the orange-yellow solution inside the movable loading barrel can be driven to rotate. During the rotation of the solution, the regulating plate is used to perform turbulence, so that the solution inside the movable loading barrel does not rotate in the form of a vortex. The connecting part includes a spline shaft fixedly connected to the output shaft of the driving motor, the bottom end of the spline shaft is connected to a spline sleeve for sliding up and down, the top end of the spline sleeve is fixedly connected to a cross-shaped adapter frame, the four supporting feet of the cross-shaped adapter frame are all rotatably connected to rollers, an adjustment ring is fixedly connected to the fixed frame and located below the spline shaft, and a plurality of circumferentially distributed limit pull rods are fixedly connected to the upper surface of the spline sleeve.

2. The method for preparing high-purity o-aminothiophenol according to claim 1, characterized in that: The positioning mechanism (9) comprises an electric telescopic rod (91) fixedly connected to a fixed frame (1); a front-rear elastically telescopic limit rod (92) is provided on the telescopic end of the electric telescopic rod (91); a limit sleeve (93) is fixedly connected to the displacement mechanism (2); a limit hole corresponding to and matching the limit rod (92) is provided on the circumferential surface of the limit sleeve (93).

3. The method for preparing high-purity o-aminothiophenol according to claim 1, characterized in that: The top end of the limit pull rod (232) is slidably connected to the spline shaft (231) up and down and is provided with a stopper.

4. The method for preparing high-purity o-aminothiophenol according to claim 3, characterized in that: The adjusting ring (236) is coaxial with the spline sleeve (234); the upper surface of the adjusting ring (236) is arranged in a wave shape that rises and falls; and the roller (235) is rollingly connected to the upper surface of the adjusting ring (236).

5. The method for preparing high-purity o-aminothiophenol according to claim 1, characterized in that: The turbulence cooling mechanism (8) comprises two left-right symmetrical transmission members (81) fixedly connected to the upper surface of the first filter box (61); a plurality of evenly distributed adjustment plates (82) are hingedly connected to the left, right and rear three sides of the first filter box (61) via hinge shafts; the transmission member (81) further comprises a mounting bracket (812) fixedly connected to the upper surface of the first filter box (61); a valve (811) is fixedly connected to the upper surface of the mounting bracket (812); a connecting hose (813) is fixedly connected to and penetrated by the bottom end of the valve (811); the connecting hose (813) penetrates the mounting bracket (812) from top to bottom and is fixedly connected to and penetrated by the adjustment plate (82) close to the valve.

6. The method for preparing high-purity o-aminothiophenol according to claim 1, characterized in that: The limiting member (83) comprises a mounting box (832) fixedly connected to the impurity removing mechanism (6); the top end of the hinge shaft between the adjusting plate (82) and the impurity removing mechanism (6) passes through the interior of the mounting box (832); a transmission box (835) is fixedly connected to the right side of the interior of the mounting box (832); a rotating disk (834) is rotatably connected to the side of the mounting box (832); two front-to-rear symmetrical bidirectional threaded rods (831) are rotatably connected to the left side of the transmission box (835); the left end of the bidirectional threaded rod (831) is rotatably connected to the mounting box (832); two left-to-right symmetrical limiting arc plates (833) are commonly threadedly connected to the two bidirectional threaded rods (831); and the hinge shaft of the adjusting plate (82) is located between the two limiting arc plates (833).

7. The method for preparing high-purity o-aminothiophenol according to claim 6, characterized in that: The left end of the rotating disk (834) passes through the interior of the installation box (832) and is rotatably connected to the transmission box (835). The rotating disk (834) drives the two bidirectional threaded rods (831) to rotate synchronously in the same direction on the transmission box (835) through the gear transmission inside the transmission box (835). A connecting pipe is fixed and penetrated between adjacent adjustment plates (82).

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