Preparation method and device of nitrogen heterocyclic corrosion inhibitor

Abstract

The invention relates to the technical field of corrosion inhibitor production, in particular to a preparation method and device of an azacyclo corrosion inhibitor, the preparation device comprises a stirring tank, a storage tank, a compaction feeding mechanism and a stirring mechanism, the stirring tank is fixed on a rack, the storage tank is fixed on the top of the stirring tank, and the compaction feeding mechanism is fixed on the top of the stirring tank. A material falling opening in the bottom of the material storage tank extends into the stirring tank in a penetrating mode, the compaction feeding mechanism is arranged at the material falling opening and used for pressing solid powder materials into cake-shaped materials and then feeding the cake-shaped materials into the stirring tank, and the stirring mechanism is arranged in the stirring tank and used for stirring and mixing the materials. According to the preparation device, the push plate is driven by the first telescopic cylinder to pre-compact powder in the blanking cavity to form a cake body structure, the cake body material vertically sinks to the bottom of a solvent under the action of gravity, liquid level agglomeration caused by powder floating is avoided, and the stirring mechanism forms a blanking area through off-axis stirring, so that the stirring efficiency is improved. The cake body is dispersed along with stirring flow in the process of gradually dissolving in the blanking area, so that the mixing uniformity is improved, and the reaction efficiency is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of corrosion inhibitor production, in particular to a preparation method and a device for a nitrogen heterocyclic corrosion inhibitor. Background Art

[0002] Nitrogen heterocyclic corrosion inhibitors are organic compounds that form chemical adsorption with metal surfaces through some atoms in the molecules, building a dense protective film on the metal surface, thereby inhibiting corrosion reactions. Their mechanism of action mainly relies on the electronic conjugation effect of the heterocyclic structure and the coordination ability of lone pair electrons. They exhibit excellent corrosion inhibition performance, especially in acidic, high-temperature and high-salt environments, with a corrosion inhibition efficiency of more than 90%. This type of corrosion inhibitor is widely used in petrochemicals, seawater environments, pickling processes and drilling fluids. For example, in oil and gas production, they protect metal equipment from carbon dioxide corrosion, or prevent metal and alloy corrosion in seawater media.

[0003] Existing preparation methods for nitrogen heterocyclic corrosion inhibitors often require high-temperature reactions, which not only consumes a lot of energy but also easily lead to the decomposition of sulfur-containing active groups, affecting product stability. In addition, traditional products lack the synergistic effect of long carbon chain hydrophobic groups and multiple active sites, resulting in weak adsorption on metal surfaces, loose film formation, and limited corrosion inhibition efficiency.

[0004] During the preparation process, materials are often ground into powders to ensure uniform mixing between the materials and the solvent before being added to the solvent. However, due to the light weight of the powdered materials, some of the materials tend to float on the surface of the solvent, resulting in uneven mixing between the materials and the solvent. This affects the uniformity and efficiency of the reaction system, and adversely affects the formation and performance of the target product.

[0005] In view of this, the present invention provides a method and device for preparing a nitrogen heterocyclic corrosion inhibitor Summary of the Invention

[0006] The purpose of the present invention is to provide a method for preparing a nitrogen heterocyclic corrosion inhibitor and a device thereof, so as to solve the technical problems raised in the above background technology.

[0007] To achieve the above objectives, the present invention provides the following technical solutions.

[0008] A method for preparing a nitrogen heterocyclic corrosion inhibitor, the specific preparation steps are as follows: Add tetrahydrofuran to the preparation device, then add 2,5-dimercaptothiadiazole to the preparation device, and stir to disperse evenly; Adding n-octyl mercaptan and hydrogen peroxide to the preparation device, heating for reaction, and then leading the mixture to an evaporation device for evaporation to remove the solvent; Add dichloromethane and deionized water to the evaporation equipment, stir and allow to stand to separate, and retain the organic phase; The solvent was removed by filtration and evaporation to obtain a nitrogen heterocyclic corrosion inhibitor.

[0009] The present invention also provides a preparation device for a nitrogen heterocyclic corrosion inhibitor, comprising a stirring tank, a storage tank, a compacting and feeding mechanism, and a stirring mechanism. The stirring tank is fixed on a frame, the storage tank is fixed on the top of the stirring tank, and a feeding port at the bottom of the storage tank extends through the stirring tank. The compacting and feeding mechanism is provided at the feeding port and is used to press solid powder material into a cake-shaped material and then feed it into the stirring tank. The stirring mechanism is provided in the stirring tank and is used to stir the mixed material. Among them, the stirring mechanism is set off-axis relative to the stirring tank to form a vertically extending drop zone between one side of the stirring mechanism and the inner wall of the stirring tank. The cake-shaped material falls into the drop zone from the drop port. A heat dissipation mechanism is provided inside the stirring tank.

[0010] Preferably, the compacting and feeding mechanism includes a sphere, a push plate and a cover plate. The sphere is installed in the blanking port with equal diameter. A shaft is fixed on the outer wall of the sphere. The shaft extends horizontally through the outside of the mixing tank. A driving motor is fixed on the outer wall of the mixing tank. The output shaft of the driving motor is fixed to the end of the shaft. A blanking cavity is provided on the sphere. An installation cavity is provided on the inner end wall of the blanking cavity. A first telescopic cylinder is fixed in the installation cavity to maintain verticality with the shaft. The push plate is matched and installed in the blanking cavity and is fixed to the telescopic end of the first telescopic cylinder. The first telescopic cylinder can drive the push plate to move in the blanking cavity through the telescopic operation to realize the spatial change adjustment in the blanking cavity. A cover plate is installed at the bottom of the blanking port to seal the bottom port of the blanking port, and the cover plate can swing open and close.

[0011] Preferably, a U-shaped seat is fixed on the outer wall of the blanking port, a rotating shaft is rotatably installed on the U-shaped seat, an L-shaped connecting arm and a transmission gear are fixedly mounted on the rotating shaft, the cover plate is fixed on the L-shaped connecting arm, a mounting frame is fixed on the outer wall of the blanking port, a second telescopic cylinder extending vertically is fixed on the mounting frame, a rack is vertically fixed to the telescopic end of the second telescopic cylinder, and the rack is meshed with the transmission gear.

[0012] Preferably, the stirring mechanism includes a rectangular frame, a first stirring rod and a second stirring rod. A suspension is fixed on the inner wall of the stirring tank, and a stirring main shaft is rotatably installed on the suspension. The rectangular frame is fixed on the bottom end of the stirring main shaft, and a plurality of first stirring rods and second stirring rods are evenly distributed on the rectangular frame. A bevel gear A is fixed on the top of the stirring main shaft, and a bevel gear B is fixedly mounted on the shaft, and the bevel gear B is meshed with the bevel gear A.

[0013] Preferably, shafts are rotatably installed on the rectangular frame at the upper and lower parts respectively, and belts that can run around the two shafts are provided on the two shafts through limiting guide pulley sleeves fixed thereon. The first stirring rod is evenly distributed on the belt, and a linkage shaft is vertically fixed on the inner bottom wall of the stirring tank. The linkage shaft passes through the bottom of the rectangular frame and is coaxially arranged with the stirring main shaft. The linkage shaft is rotatably connected to the rectangular frame, and a bevel gear C is fixed on the top of the linkage shaft, and a bevel gear D is fixedly sleeved on the shaft below, and the bevel gear D is correspondingly engaged with the bevel gear C.

[0014] Preferably, U-shaped frames are evenly distributed on the belt, and a rotating rod is rotatably installed in the mounting hole of the U-shaped frame. A spiral spring is provided on the outside of the rotating rod, one end of the spiral spring is fixed to the inner wall of the mounting hole, and the other end is fixed to the outer wall of the rotating rod. The tail of the first stirring rod is fixedly sleeved on the rotating rod, and under the elastic restraining force of the spiral spring, the first stirring rod is set perpendicular to the belt surface. Spherical cavities that pass through the upper and lower sides of the rectangular frame corresponding to the position of the first stirring rod are provided, and a ball is embedded in each spherical cavity, and the ball is correspondingly pressed and fitted with the first stirring rod.

[0015] Preferably, the heat dissipation mechanism includes a coil and a water cooling box. The coil is fixed on the inner wall of the stirring tank and is distributed in a spiral shape around the axis of the stirring tank. The water cooling box is arranged on the frame and is located on one side of the stirring tank. The outlet of the coil is connected to the inlet of the water cooling box, and the inlet of the coil is connected to the outlet of the water cooling box. A temperature sensor is fixed on the inner wall of the stirring tank, and an electrical control box is provided on the frame. The temperature sensor is electrically connected to the control module in the electrical control box.

[0016] Preferably, the preparation device further includes a three-way valve A and a three-way valve B. An electric heating box is installed on the rack on one side of the water cooling box. The outlet of the electric heating box is connected to the first interface of the three-way valve B through a connecting pipe C, and the second interface of the three-way valve B is connected to the outlet of the water cooling box through a connecting pipe B. The third interface of the three-way valve B is connected to the inlet of the coil through the inlet pipe, the inlet of the electric heating box is connected to the first interface of the three-way valve A through the connecting pipe D, the second interface of the three-way valve A is connected to the inlet of the water cooling box through the connecting pipe A, and the third interface of the three-way valve A is connected to the outlet of the coil through the outlet pipe.

[0017] Preferably, the outlet pipe is U-shaped and has two spiral portions on it. The two spiral portions are symmetrically arranged on the left and right and extend vertically. A vertically penetrating rectangular cover is fixed on the outer wall of the frame. The two spiral portions are matched and arranged in the rectangular cover. A cooling fan is installed on one side of the rectangular cover.

[0018] Compared with the prior art, the present invention has the following beneficial effects.

[0019] This preparation method reacts at a low temperature of 50°C, which significantly reduces energy consumption compared to traditional high-temperature reactions and avoids the destruction of sulfur-containing active groups by high temperature, ensuring the structural stability of the product. The 2,5-dimercaptothiadiazole in the raw materials reacts with n-octanethiol, so that the product has the electronic conjugation effect of the heterocyclic structure, the coordination ability of lone pair electrons, and the long carbon chain hydrophobic group, which enhances the chemical adsorption ability and film density on the metal surface, thereby improving the corrosion inhibition efficiency.

[0020] This preparation device uses a first telescopic cylinder to drive a push plate to pre-compact the powder in the blanking chamber to form a cake structure. The cake-shaped material sinks vertically to the bottom of the solvent under the action of gravity, avoiding the aggregation of liquid dough caused by powder floating; The off-axis stirring of the stirring mechanism forms a laminar flow and turbulent flow transition interface with the main body of the solvent. The cake disperses with the stirring flow during the gradual dissolution process, thereby improving the mixing uniformity and the reaction efficiency.

[0021] When the cover is flipped open to the tilted state, its lower end tilts toward the drop zone, and the cake-shaped material can slide along the cover into the drop zone, preventing the stirring parts from directly contacting and impacting the material and causing the cake to break into powder, thereby maintaining the material in block form and gradually sinking into the solvent and dispersing and dissolving.

[0022] During the rotation of the rectangular frame, since the bevel gear C and the linkage shaft are fixedly arranged, under the meshing transmission action of the bevel gear D and the bevel gear C, the bevel gear D is driven in the reverse direction and drives the shaft below to rotate, thereby driving the belt to run around the two shafts. The belt drives each first stirring rod to move up and down in sequence, realizing a dynamic stirring mechanism in the horizontal and vertical directions, effectively reducing material sedimentation and further improving the quality of the mixing reaction.

[0023] The cooling medium in the heat dissipation mechanism is used for both heating the reaction in the stirring tank and dissipating heat and cooling the subsequent heat generation, killing two birds with one stone. At the same time, heating and heat dissipation basically share the same set of piping systems, which optimizes the system structure and improves the compactness and integration of the equipment. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 A schematic flow chart of the preparation method provided by the present invention; Figure 2 A schematic diagram of the overall structure of the preparation device provided by the present invention; Figure 3 This is a cross-sectional schematic diagram of the mixing tank and the storage tank in the present invention; Figure 4 This is a schematic diagram of the structure at the top of the stirring tank in the present invention; Figure 5 It is a schematic diagram of the local structure of the blanking port in the present invention; Figure 6A for Figure 5A schematic partial cross-sectional view of the structure shown; Figure 6B This is a schematic structural diagram of Example 6; Figure 7 for Figure 3 A schematic plan view of the structure shown; Figure 8 It is a schematic diagram of the local structure of the stirring mechanism in the present invention; Figure 9 for Figure 8 A schematic diagram of the structure at center A; Figure 10 for Figure 8 A magnified schematic diagram of the structure at point B in the middle; Figure 11 This is a schematic diagram of the installation of the first stirring rod structure in the present invention; Figure 12 for Figure 11 A magnified schematic diagram of the structure at point C in the middle; Figure 13 Schematic diagram of the heat dissipation and preheating components in the present invention; Figure 14 It is a schematic diagram of the rectangular cover structure layout in the present invention.

[0025] In the figure: 1. frame; 2. mixing tank; 21. blanking area; 3. storage tank; 31. blanking port; 32. discharge port; 321. electric valve; 4. compacting feeding mechanism; 41. sphere; 411. blanking cavity; 412. mounting cavity; 42. push plate; 421. slide hole; 422. forming rod; 43. first telescopic cylinder; 44. shaft; 45. driving motor; 46. cover plate; 461. U-shaped seat; 462. rotating shaft; 463. L-shaped connecting arm; 464. transmission gear; 465. mounting frame; 466. second telescopic cylinder; 467. rack; 5. mixing mechanism; 501. suspension; 51. rectangular frame; 511. spherical cavity; 512. rolling ball; 52. mixing main Shaft; 521, bevel gear A; 522, bevel gear B; 53, first stirring rod; 531, U-shaped frame; 532, mounting hole; 533, rotating rod; 534, scroll spring; 54, second stirring rod; 55, shaft body; 551, limit guide wheel; 56, belt; 57, linkage shaft; 58, bevel gear C; 59, bevel gear D; 6, coil; 61, water cooling box; 62, three-way valve A; 63, three-way valve B; 64, outlet pipe; 641, spiral part; 65, inlet pipe; 66, connecting pipe A; 67, connecting pipe B; 7, electric heating box; 71, connecting pipe C; 72, connecting pipe D; 8, rectangular cover; 81, cooling fan; 9, electric control box; 91, temperature sensor. DETAILED DESCRIPTION

[0026] The embodiments of the present invention are described below with reference to the accompanying drawings.

[0027] In the description of the embodiments of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms, "connection", and "installation" should be understood in a broad sense. For example, "connection" can be a detachable connection or a non-detachable connection; it can be a direct connection or an indirect connection through an intermediate medium. In addition, "communication" can be a direct connection or an indirect connection through an intermediate medium. Here, "fixed" means that the two are connected to each other and the relative position relationship after connection remains unchanged. The directional terms mentioned in the embodiments of the present invention, such as "inside", "outside", "top", "bottom", etc., are only reference to the directions of the accompanying drawings. Therefore, the directional terms used are for better and clearer explanation and understanding of the embodiments of the present invention, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the embodiments of the present invention.

[0028] In the embodiments of the present invention, the terms "first" and "second" are used for descriptive purposes only and should not be understood to indicate or imply relative importance or implicitly specify the number of technical features indicated. Therefore, features defined as "first" or "second" may explicitly or implicitly include one or more of the features.

[0029] In the embodiments of the present invention, "and / or" is simply a description of the association relationship between associated objects, indicating that three possible relationships exist. For example, "A and / or B" can represent three situations: A exists alone, A and B exist simultaneously, and B exists alone. Furthermore, the character " / " in this document generally indicates that the associated objects are in an "or" relationship.

[0030] References to "one embodiment" or "some embodiments" in this specification mean that a particular feature, structure, or characteristic described in connection with that embodiment is included in one or more embodiments of the present invention. Thus, phrases such as "in one embodiment," "in some embodiments," "in other embodiments," and "in yet other embodiments" appearing in various places in this specification do not necessarily refer to the same embodiment, but rather mean "one or more, but not all, embodiments," unless otherwise specifically emphasized. The terms "including," "comprising," "having," and variations thereof mean "including but not limited to," unless otherwise specifically emphasized. Example 1

[0031] See also Figure 1 The present invention provides a method for preparing a nitrogen heterocyclic corrosion inhibitor, and the specific preparation steps are as follows: Add 100 L of tetrahydrofuran to the preparation device, then add 45.07 kg of 2,5-dimercaptothiadiazole to the preparation device, and stir to disperse evenly; Add 87.78 kg of n-octyl mercaptan and 23.80 kg of hydrogen peroxide to the preparation device, heat to 50°C and react for 3 hours, then lead to an evaporation device to evaporate and remove the solvent; Add 50 L of dichloromethane and 300 L of deionized water to the evaporation equipment, stir for 30 minutes, and then let it stand to separate the layers, retaining the organic phase; The solvent was removed by filtration and evaporation to obtain a nitrogen heterocyclic corrosion inhibitor.

[0032] The synthesis process is carried out at 50°C, which consumes less energy than high-temperature reactions and avoids damage to the reactant structure caused by high temperature, facilitating the stable production of the target product. Tetrahydrofuran is used as the reaction solvent, which has good solubility for raw materials such as 2,5-dimercaptothiadiazole and n-octyl mercaptan, ensuring a uniform reaction. Post-processing involves extraction with dichloromethane, resulting in clear separation from the aqueous phase, facilitating separation and purification. Hydrogen peroxide is used as an oxidant, and the reaction generates water without any harmful byproducts. This is in line with the concept of green chemistry. The post-processing process of stirring, stratification, filtration, and evaporation effectively removes impurities. The operation steps are simple and conducive to industrial production. The 2,5-dimercaptothiadiazole in the raw material contains a nitrogen heterocyclic ring and a thiol group, and n-octyl mercaptan introduces a long carbon chain alkyl group. The two react to form a product containing multiple active sites and hydrophobic groups, which enhances the adsorption capacity and film-forming properties on the metal surface and improves the corrosion inhibition efficiency. Example 2

[0033] See also Figure 2-Figure 14 The difference between this embodiment and embodiment 1 is that: The present invention also provides a preparation device for a nitrogen heterocyclic corrosion inhibitor, comprising a stirring tank 2, a storage tank 3, a compacting and feeding mechanism 4, and a stirring mechanism 5. The stirring tank 2 is fixed on a frame 1, the storage tank 3 is fixed on the top of the stirring tank 2, and a feeding port 31 at the bottom of the storage tank 3 extends through the stirring tank 2. The storage tank 3 serves as a solid material feeding portion, and the fixed powder material is fed into the storage tank 3, and the powder material can fall into the stirring tank 2 through the feeding port 31. Secondly, a liquid feeding port (not shown in the figure) is further provided on the stirring tank 2 for feeding liquid materials. The structure and use principle of the liquid feeding port are consistent with those in the prior art and will not be described in detail. In addition, Figure 3 As shown, the bottom of the stirring tank 2 is further provided with a discharge port 32 for discharging the reaction liquid, and an electric valve 321 is further installed on the discharge port 32 to control the discharge on and off.

[0034] like Figure 3-Figure 7 As shown, the compacting and feeding mechanism 4 is provided at the blanking port 31. The compacting and feeding mechanism 4 includes a sphere 41, a push plate 42 and a cover plate 46. The sphere 41 is installed in the blanking port 31 with equal diameter, that is, the outer diameter of the sphere 41 is adapted to the inner diameter of the blanking port 31. A shaft 44 is fixed on the outer wall of the sphere 41, and the shaft 44 extends horizontally through the outside of the mixing tank 2. A driving motor 45 is fixed on the outer wall of the mixing tank 2, and the output shaft of the driving motor 45 is fixed to the end of the shaft 44. A blanking cavity 411 is provided on the sphere 41, and a mounting cavity 412 is provided on the inner end wall of the blanking cavity 411. A first telescopic cylinder 43 that is perpendicular to the shaft 44 is fixed in the mounting cavity 412. When the driving motor 45 works, its output shaft can drive the sphere 41 to rotate and adjust under the connection with the shaft 44. During the rotation of the sphere 41, when the opening of the sphere 41 rotates to an upward state, the material in the storage tank 3 can fall into the blanking cavity 411. As the sphere 41 continues to rotate, when the opening of the blanking cavity 411 faces downward, the material therein can fall into the mixing tank 2 from the lower end of the blanking port 31. The push plate 42 is matchedly installed in the blanking cavity 411 and is fixed to the telescopic end of the first telescopic cylinder 43, that is, the push plate 42 slides and fits against the inner wall of the blanking cavity 411. The first telescopic cylinder 43 telescopically works to drive the push plate 42 to move in the blanking cavity 411, thereby adjusting the size of the space for temporarily storing materials in the blanking cavity 411. In addition, a cover plate 46 for sealing the bottom port of the blanking cavity 31 is installed at the bottom of the blanking port 31, wherein the cover plate 46 can be swung open and closed.

[0035] When the cover plate 46 is closed and the material falls into the blanking cavity 411, the adjusting ball 41 is rotated until the opening of the blanking cavity 411 faces downward. Then, the first telescopic cylinder 43 is extended to push the push plate 42 toward the end of the blanking cavity 411. Under the blocking effect of the cover plate 46, the powdered material temporarily stored in the blanking cavity 411 can be compacted into a cake shape. Subsequently, the cover plate 46 is rotated to open, and the first telescopic cylinder 43 continues to extend to push the cake-shaped material out of the blanking cavity 411 and fall into the solvent in the mixing tank 2 through the bottom opening of the blanking port 31. The powder material is compacted into a cake shape and put into the solvent to increase the material density. The cake-shaped material can sink into the solvent, avoiding uneven mixing caused by the floating of the powder material. In addition, the cake structure sinks in the solvent and gradually disperses and dissolves, ensuring that the upper and lower positions of the material in the solvent are evenly distributed. Secondly, the gradual dispersion and dissolution of the cake makes the concentration gradient of the reaction system tend to balance, thereby effectively improving the quality of the target product.

[0036] In addition, by the extension and retraction of the first telescopic cylinder 43, the push plate 42 is pushed to move and adjust accordingly, and the temporary storage space of the material in the blanking cavity 411 can be adjusted to achieve quantitative delivery of different amounts of material; Secondly, when the first telescopic cylinder 43 is extended to the limit position, it pushes the push plate 42 to move to the end of the blanking cavity 411, blocking the end of the blanking cavity 411, thereby preventing the material from entering the blanking cavity 411 and stopping the feeding.

[0037] like Figure 3 and Figure 7 As shown, the stirring mechanism 5 is arranged in the stirring tank 2, and is used to stir the mixed materials to improve the reaction quality, wherein the stirring mechanism 5 is eccentrically arranged relative to the stirring tank 2, that is, the stirring mechanism 5 is in the stirring tank 2 and deviates to one side of the stirring tank 2, thereby forming a vertically extending blanking area 21 between one side of the stirring mechanism 5 and the inner wall of the stirring tank 2, that is, the stirring part in the stirring mechanism 5 will not directly enter the blanking area 21.

[0038] like Figure 7 As shown, when the cover plate 46 is flipped open to the tilted state, its lower end tilts toward the drop zone 21, and the cake-shaped material can slide along the cover plate 46 into the drop zone 21, preventing the stirring component from directly contacting and impacting the material and causing the cake to break into powder, thereby maintaining the material in a block form and gradually sinking into the solvent for dispersion and dissolution; This design can not only utilize the density characteristics of the cake itself to ensure that it sinks stably to the bottom of the frame 1, but also reduce the damage to the shape of the cake material caused by external mechanical forces, and avoid the generation of powder after crushing that floats or partially agglomerates on the liquid surface; In addition, the material gradually dissolves and disperses after falling into the drop zone 21. Combined with the stirring action of the stirring mechanism 5, the solvent flows continuously, and the dissolved and dispersed material is subjected to wave stirring, forming an orderly dispersion process from the edge to the center, which significantly improves the uniformity of the material distribution in the solvent.

[0039] Combine Figure 5 and Figure 6A A U-shaped seat 461 is fixed on the outer wall of the blanking port 31, and a rotating shaft 462 is rotatably installed on the U-shaped seat 461. An L-shaped connecting arm 463 and a transmission gear 464 are fixed on the rotating shaft 462. The cover plate 46 is fixed on the L-shaped connecting arm 463. A mounting bracket 465 is fixed on the outer wall of the blanking port 31. A vertically extending second telescopic cylinder 466 is fixed on the mounting bracket 465. A rack 467 is vertically fixed at the telescopic end of the second telescopic cylinder 466, and the rack 467 is engaged with the transmission gear 464.

[0040] The cover plate 46 is hingedly installed by using the U-shaped seat 461, the rotating shaft 462 and the L-shaped connecting arm 463. The second telescopic cylinder 466 is telescopically operated to drive the rack 467 to move up and down accordingly. The moving rack 467 engages the drive gear 464 and drives the rotating shaft 462 to rotate. Under the connection action of the L-shaped connecting arm 463, the cover plate 46 can be driven to perform a swinging opening and closing adjustment. Example 3

[0041] See also Figure 3 、 Figure 4 as well as Figures 8 to 12 The difference between this embodiment and embodiment 2 is that: The stirring mechanism 5 includes a rectangular frame 51, a first stirring rod 53 and a second stirring rod 54. A suspension 501 is fixed on the inner wall of the stirring tank 2. A stirring main shaft 52 is rotatably installed on the suspension 501. The rectangular frame 51 is fixed on the bottom end of the stirring main shaft 52. Several first stirring rods 53 and second stirring rods 54 are evenly distributed on the rectangular frame 51. Among them, a bevel gear A521 is fixed on the top of the stirring main shaft 52, and a bevel gear B522 is fixedly mounted on the shaft 44. The bevel gear B522 is meshed with the bevel gear A521.

[0042] During the rotation of the shaft 44, the bevel gear B522 can be driven to rotate. The rotating bevel gear B522 engages with the driving bevel gear A521 and drives the stirring main shaft 52 to rotate, thereby driving the rectangular frame 51 to rotate. The first stirring rod 53 and the second stirring rod 54 rotate along with the rectangular frame 51 to achieve stirring of the material and solvent mixture. Through the linkage cooperation of the bevel gear A521 and the bevel gear B522, the rotational force of the driving motor 45 driving the shaft 44 is converted into the rotational force of the rectangular frame 51, and there is no need to set an additional driving source separately for the stirring mechanism 5.

[0043] Axles 55 are rotatably mounted on the upper and lower sides of the rectangular frame 51. Belts 56 that can run around the two axles 55 are sleeved on the two axles 55 via limiting guide wheels 551 fixed thereon. The first stirring rods 53 are evenly mounted on the belts 56, that is, the first stirring rods 53 are evenly distributed on the belts 56, and the second stirring rods 54 are evenly distributed on both sides of the rectangular frame 51. Two belts 56 are provided. A linkage shaft 57 is vertically fixed on the inner bottom wall of the mixing tank 2. The linkage shaft 57 passes through the bottom of the rectangular frame 51 and is coaxially arranged with the mixing main shaft 52. The linkage shaft 57 is rotatably connected to the rectangular frame 51. A bevel gear C58 is fixed on the top of the linkage shaft 57, and a bevel gear D59 is fixedly mounted on the shaft body 55 below. The bevel gear D59 is meshed with the bevel gear C58.

[0044] During the rotation of the rectangular frame 51, since the bevel gear C58 and the linkage shaft 57 are fixedly arranged, the bevel gear D59 is driven in reverse by the meshing transmission of the bevel gear C58, and the shaft 55 below is driven to rotate, thereby driving the belt 56 to run around the two shafts 55. The belt 56 drives each first stirring rod 53 to move up and down in a circular motion in sequence, realizing a dynamic stirring mechanism in both horizontal and vertical directions, effectively reducing material sedimentation and further improving the quality of the mixing reaction. The operation of the belt 56 depends on the meshing transmission of the bevel gear C58 and the bevel gear D59, and no additional driving source is required. Example 4

[0045] See also Figure 10 and Figure 11The difference between this embodiment and embodiment 3 is that: U-shaped frames 531 are evenly distributed on the belt 56. A rotating rod 533 is rotatably installed in the mounting hole 532 on the U-shaped frame 531. A spiral spring 534 is sleeved on the outside of the rotating rod 533. One end of the spiral spring 534 is fixed to the inner wall of the mounting hole 532, and the other end is fixed to the outer wall of the rotating rod 533. The tail of the first stirring rod 53 is fixedly sleeved on the rotating rod 533.

[0046] Under the elastic restraining force of the vortex spring 534, the first stirring rod 53 is set perpendicular to the surface of the belt 56. During stirring, as the belt 56 runs, the first stirring rod 53 will conflict with the rectangular frame 51. When the first stirring rod 53 is squeezed by the rectangular frame 51, the first stirring rod 53 will overcome the elastic force of the vortex spring 534 and swing to avoid motion interference. After the first stirring rod 53 is separated from the rectangular frame 51, the elastic force of the vortex spring 534 can be used to drive the first stirring rod 53 to gradually return to its original position, and the overall structural layout is reasonable.

[0047] In addition, the restraining force provided by the spiral spring 534 to the first stirring rod 53 is greater than the resistance of the solvent to the first stirring rod 53, that is, during stirring, the first stirring rod 53 will not swing due to the resistance of the solvent, ensuring that the stirring state of the first stirring rod 53 is stably maintained.

[0048] Spherical cavities 511 are provided at the upper and lower sides of the rectangular frame 51 corresponding to the position of the first stirring rod 53, and each spherical cavity 511 is embedded with a ball 512. The ball 512 is in contact and extruded with the first stirring rod 53, that is, the first stirring rod 53 is directly in contact and extruded with the ball 512. In the process of the first stirring rod 53 being pressed and gradually swinging, the ball 512 rolls, reducing the friction between the ball 512 and the first stirring rod 53, thereby ensuring that the belt 56 can run smoothly and stably. Example 5

[0049] Since a large amount of heat will be generated in the later stage of the reaction, if the heat is excessively accumulated in the stirring tank 2, it will have an adverse effect. In order to solve the heat dissipation problem in the later stage of the reaction, please refer to Figure 1 、 Figure 3 、 Figure 7 and Figure 13 The difference between this embodiment and embodiment 4 is that: The preparation device also includes a heat dissipation mechanism, which includes a coil 6 and a water cooling box 61. The coil 6 is fixed on the inner wall of the stirring tank 2 and is distributed in a spiral shape around the axis of the stirring tank 2. The water cooling box 61 is arranged on the frame 1 and is located on one side of the stirring tank 2. The outlet of the coil 6 is connected to the inlet of the water cooling box 61, and the inlet of the coil 6 is connected to the outlet of the water cooling box 61.

[0050] A temperature sensor 91 is fixed on the inner wall of the mixing tank 2, and an electric control box 9 is provided on the frame 1. The temperature sensor 91 is electrically connected to the control module in the electric control box 9. The temperature in the mixing tank 2 is monitored by the temperature sensor 91. When the temperature in the mixing tank 2 is too high, the electric control box 9 controls the water pump in the water cooling box 61 to pump the cooling medium in the coil 6 into the water cooling box 61. At the same time, the cooling medium in the water cooling box 61 flows back to the coil 6, thereby realizing the circulation of the cooling medium. When the cooling medium flows in the coil 6, it can absorb the temperature generated by the reaction in the stirring tank 2. After the cooling medium flows into the water cooling box 61, it is cooled by heat exchange and then flows back to the coil 6. This cycle of cooling ensures that the temperature in the stirring tank 2 is stable.

[0051] The coil 6 is arranged in a spiral shape, which ensures a large cooling coverage in the mixing tank 2 and improves the cooling efficiency.

[0052] Secondly, the preparation device also includes a three-way valve A62 and a three-way valve B63. An electric heating box 7 is installed on the frame 1 on one side of the water cooling box 61. The outlet of the electric heating box 7 is connected to the first interface of the three-way valve B63 through the connecting pipe C71, and the second interface of the three-way valve B63 is connected to the outlet of the water cooling box 61 through the connecting pipe B67. The third interface of the three-way valve B63 is connected to the inlet of the coil 6 through the inlet pipe 65. The inlet of the electric heating box 7 is connected to the first interface of the three-way valve A62 through the connecting pipe D72, the second interface of the three-way valve A62 is connected to the inlet of the water cooling box 61 through the connecting pipe A66, and the third interface of the three-way valve A62 is connected to the outlet of the coil 6 through the outlet pipe 64.

[0053] Since heating treatment is required in the initial stage of the reaction, the three-way valve A62 is adjusted to the state where the outlet pipe 64 is connected only to the connecting pipe D72, and the three-way valve B63 is adjusted to the state where the inlet pipe 65 is connected only to the connecting pipe C71. The water pump in the electric heating box 7 is operated to suck the cooling medium in the coil 6 into the electric heating box 7 through the outlet pipe 64 and the connecting pipe D72 in turn, and the cooling medium is heated by the electric heater in the electric heating box 7. The heated cooling medium is then discharged into the coil 6 through the connecting pipe C71 and the inlet pipe 65, so that heating treatment can be performed in the initial stage of the reaction.

[0054] After the heating is completed, as the reaction continues, the heat generated gradually accumulates and can provide the required heat for subsequent reactions. In particular, when the heat generated is greater than the actual requirement, there is no need to use the electric heating box 7 for heating. The three-way valve A62 is adjusted to the outlet pipe 64 only connected to the connecting pipe A66, and the three-way valve B63 is adjusted to the inlet pipe 65 only connected to the connecting pipe B67. At this time, the heat dissipation mechanism can be used to dissipate excess heat.

[0055] In addition, the outlet pipe 64 is U-shaped and has two spiral portions 641 on the outlet pipe 64. The two spiral portions 641 are symmetrically arranged on the left and right and extend vertically. A vertically penetrating rectangular cover 8 is fixed on the outer wall of the frame 1. The two spiral portions 641 are matched and arranged in the rectangular cover 8. A cooling fan 81 is installed on one side of the rectangular cover 8. When cooling and heat dissipation is performed, the cooling fan 81 works to draw external air into the rectangular cover 8, so that a positive pressure is formed in the rectangular cover 8. Since the upper and lower ends of the rectangular cover 8 are connected, the air in the rectangular cover 8 is discharged from the two ends of the rectangular cover 8 to form a flowing airflow, which can take away part of the heat in the outlet pipe 64. Before the cooling medium enters the water cooling box 61, pre-heating can be performed to accelerate the cooling of the medium and improve the cooling efficiency of the medium.

[0056] In addition, there are two spiral portions 641 on the outlet pipe 64, and the spiral portions 641 are both located inside the rectangular cover 8. The spiral portions 641 extend the travel of the cooling medium inside the rectangular cover 8, allowing it to have a longer contact time and a larger contact area with the flowing airflow, further improving the medium's pre-heat dissipation cooling efficiency.

[0057] In addition, the cooling medium is used for both heating the reaction in the stirring tank 2 and dissipating the heat generated in the later stage, killing two birds with one stone. At the same time, heating and heat dissipation basically share the same set of piping systems, which optimizes the system structure and improves the compactness and integration of the equipment. Example 6

[0058] See also Figure 6B The difference between this embodiment and embodiment 5 is that: The aperture of the mounting cavity 412 is slightly smaller than that of the blanking cavity 411. The push plate 42 is evenly distributed with a number of through sliding holes 421 around its axis. A forming rod 422 is slidably inserted into each sliding hole 421. One end of each forming rod 422 is fixed to the inner end wall of the mounting cavity 412. When the sphere 41 rotates to the point where the end of the blanking cavity 411 faces directly downward, and the cover plate 46 is closed to block the bottom end of the blanking port 31, the ends of each forming rod 422 are in contact with and fit against the cover plate 46.

[0059] When the port of the blanking cavity 411 faces upward, the powder will fall into the blanking cavity 411 and be distributed in places other than the forming rod 422; When the powder is compacted, as the first telescopic cylinder 43 extends, it pushes the push plate 42 toward the cover plate 46. The push plate 42 slides along the forming rod 422, and finally compacts the powder into a cake. The forming rod 422 forms a plurality of through holes in the cake-shaped material. After the cake-shaped material is put into the solvent, the hole structure on it can increase the contact area with the solvent, thereby accelerating the dissolution and dispersion of the cake structure and improving the dispersion and mixing efficiency.

[0060] In addition, it is worth mentioning that the first telescopic cylinder 43 and the second telescopic cylinder 466 in the present application are electric push cylinders.

[0061] The control method of the present invention is automatic control through a controller. The control circuit of the controller can be implemented by simple programming by technicians in this field. The provision of power is also common knowledge in this field, so the present invention will no longer explain the control method and circuit connection in detail.

[0062] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention.

Claims

1. A method for preparing a nitrogen heterocyclic corrosion inhibitor, characterized in that: The specific preparation steps are as follows: Add tetrahydrofuran to the preparation device, then add 2,5-dimercaptothiadiazole to the preparation device, and stir to disperse evenly; adding n-octyl mercaptan and hydrogen peroxide to the preparation device, heating for reaction, and then leading the mixture to an evaporation device for evaporation to remove the solvent; Add dichloromethane and deionized water to the evaporation equipment, stir and allow to stand for stratification, and retain the organic phase; The solvent was removed by filtration and evaporation to obtain a nitrogen heterocyclic corrosion inhibitor.

2. A device for preparing a nitrogen heterocyclic corrosion inhibitor, applied to the above-mentioned method for preparing a nitrogen heterocyclic corrosion inhibitor, characterized in that: It comprises a stirring tank (2), wherein the stirring tank (2) is fixed on the frame (1); A material storage tank (3), the material storage tank (3) is fixed on the top of the mixing tank (2), and the material drop opening (31) at the bottom of the material storage tank (3) extends through and into the mixing tank (2); A compacting and feeding mechanism (4), the compacting and feeding mechanism (4) being arranged at the feeding port (31) and used for pressing the solid powder material into a cake-shaped material and then feeding it into the mixing tank (2); A stirring mechanism (5), the stirring mechanism (5) is arranged in the stirring tank (2) and is used to stir the mixed material; The stirring mechanism (5) is arranged eccentrically relative to the stirring tank (2) to form a vertically extending drop zone (21) between one side of the stirring mechanism (5) and the inner wall of the stirring tank (2); The cake-shaped material falls from the drop opening (31) into the drop area (21); A heat dissipation mechanism is provided inside the stirring tank (2).

3. The preparation device of a nitrogen heterocyclic corrosion inhibitor according to claim 2, characterized in that: The compacting and feeding mechanism (4) comprises a sphere (41), a push plate (42) and a cover plate (46); The sphere (41) is installed in the blanking opening (31) with equal diameter; A shaft (44) is fixed on the outer wall of the sphere (41), and the shaft (44) extends horizontally through the outside of the mixing tank (2); A driving motor (45) is fixed on the outer wall of the stirring tank (2), and an output shaft of the driving motor (45) is fixed to the end of the shaft (44); The sphere (41) is provided with a blanking cavity (411), an inner end wall of the blanking cavity (411) is provided with a mounting cavity (412), and a first telescopic cylinder (43) is fixed in the mounting cavity (412) and is kept perpendicular to the shaft (44); The push plate (42) is matchedly mounted in the blanking cavity (411) and fixed to the telescopic end of the first telescopic cylinder (43); The first telescopic cylinder (43) can be used to telescope and move the push plate (42) within the blanking cavity (411), thereby achieving spatial change adjustment within the blanking cavity (411); A cover plate (46) for blocking the bottom port of the blanking opening (31) is installed at the bottom of the blanking opening (31), and the cover plate (46) can be opened and closed in a swinging manner.

4. The preparation device of a nitrogen heterocyclic corrosion inhibitor according to claim 3, characterized in that: A U-shaped seat (461) is fixed on the outer wall of the blanking port (31), a rotating shaft (462) is rotatably mounted on the U-shaped seat (461), and an L-shaped connecting arm (463) and a transmission gear (464) are fixedly mounted on the rotating shaft (462); The cover plate (46) is fixed on the L-shaped connecting arm (463); A mounting frame (465) is fixed on the outer wall of the blanking port (31), and a second telescopic cylinder (466) extending vertically is fixed on the mounting frame (465); A rack (467) is vertically fixed to the telescopic end of the second telescopic cylinder (466), and the rack (467) is correspondingly engaged with the transmission gear (464).

5. The preparation device of a nitrogen heterocyclic corrosion inhibitor according to claim 3, characterized in that: The stirring mechanism (5) comprises a rectangular frame (51), a first stirring rod (53) and a second stirring rod (54); A suspension (501) is fixed on the inner wall of the stirring tank (2), and a stirring main shaft (52) is rotatably installed through the suspension (501); The rectangular frame (51) is fixed to the bottom end of the stirring main shaft (52); A plurality of the first stirring rods (53) and the second stirring rods (54) are evenly distributed on the rectangular frame (51); A bevel gear A (521) is fixed to the top of the stirring main shaft (52), and a bevel gear B (522) is fixedly sleeved on the shaft (44), and the bevel gear B (522) is correspondingly meshed with the bevel gear A (521).

6. The preparation device of a nitrogen heterocyclic corrosion inhibitor according to claim 5, characterized in that: Axles (55) are rotatably mounted on the rectangular frame (51) at the upper and lower sides respectively, and belts (56) capable of running around the two axles (55) are sleeved on the two axles (55) via limiting guide wheels (551) fixed thereon. The first stirring rods (53) are evenly distributed on the belt (56); A linkage shaft (57) is vertically fixed on the inner bottom wall of the stirring tank (2), and the linkage shaft (57) passes through the bottom of the rectangular frame (51) and is coaxially arranged with the stirring main shaft (52); The linkage shaft (57) is rotatably connected to the rectangular frame (51), a bevel gear C (58) is fixed on the top of the linkage shaft (57), and a bevel gear D (59) is fixedly sleeved on the shaft body (55) below, and the bevel gear D (59) is correspondingly engaged with the bevel gear C (58).

7. The device for preparing a nitrogen heterocyclic corrosion inhibitor according to claim 6, characterized in that: U-shaped frames (531) are evenly distributed on the belt (56), and a rotating rod (533) is rotatably installed in the mounting hole (532) on the U-shaped frame (531); A scroll spring (534) is sleeved on the outside of the rotating rod (533); one end of the scroll spring (534) is fixed to the inner wall of the mounting hole (532), and the other end is fixed to the outer wall of the rotating rod (533); The tail of the first stirring rod (53) is fixedly sleeved on the rotating rod (533); Under the elastic restraining force of the volute spring (534), the first stirring rod (53) is arranged perpendicular to the surface of the belt (56); Spherical cavities (511) that penetrate vertically are provided at the upper and lower sides of the rectangular frame (51) at positions corresponding to the positions of the first stirring rod (53); A rolling ball (512) is embedded in each of the spherical cavities (511); The rolling ball (512) and the first stirring rod (53) are correspondingly pressed and fitted.

8. The device for preparing a nitrogen heterocyclic corrosion inhibitor according to claim 2, characterized in that: The heat dissipation mechanism includes a coil (6) and a water cooling box (61); The coil (6) is fixed on the inner wall of the stirring tank (2) and is distributed in a spiral shape around the axis of the stirring tank (2); The water cooling box (61) is arranged on the frame (1) and is located on one side of the stirring tank (2); The outlet of the coil (6) is in communication with the inlet of the water cooling box (61), and the inlet of the coil (6) is in communication with the outlet of the water cooling box (61); A temperature sensor (91) is fixed on the inner wall of the stirring tank (2), an electric control box (9) is provided on the frame (1), and the temperature sensor (91) is electrically connected to a control module in the electric control box (9).

9. The device for preparing a nitrogen heterocyclic corrosion inhibitor according to claim 8, characterized in that: The preparation device further includes a three-way valve A (62) and a three-way valve B (63); An electric heating box (7) is installed on the frame (1) at one side of the water cooling box (61); The outlet of the electric heating box (7) is connected to the first interface of the three-way valve B (63) through the connecting pipe C (71), the second interface of the three-way valve B (63) is connected to the outlet of the water cooling box (61) through the connecting pipe B (67), and the third interface of the three-way valve B (63) is connected to the inlet of the coil (6) through the inlet pipe (65); The inlet of the electric heating box (7) is connected to the first interface of the three-way valve A (62) through a connecting pipe D (72); The second interface of the three-way valve A (62) is connected to the inlet of the water cooling box (61) through the connecting pipe A (66), and the third interface of the three-way valve A (62) is connected to the outlet of the coil (6) through the outflow pipe (64).

10. The device for preparing a nitrogen heterocyclic corrosion inhibitor according to claim 9, characterized in that: The outlet pipe (64) is U-shaped, and has two spiral portions (641) on the outlet pipe (64); The two spiral portions (641) are arranged symmetrically on the left and right, and both extend vertically; A vertically penetrating rectangular cover (8) is fixed on the outer wall of the frame (1); The two spiral portions (641) are both matched and arranged in the rectangular cover (8); A cooling fan (81) is installed on one side of the rectangular cover (8).

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