Preparation method of piroctone olamine salt

Abstract

The invention discloses a preparation method of piroctone olamine salt, and relates to the technical field of chemical synthesis, and the preparation method comprises the following steps: preparing a reaction kettle I and a reaction kettle II, putting cyclohexane and 4-methyl-6-(2, 4, 4-trimethylpentyl)-2H-pyran-2-ketone into the reaction kettle I, slowly adding hydroxylamine hydrochloride and sodium carbonate in batches in combination with a bubble generation assembly, and reacting for 1-2 hours; bubbles are slowly generated to prevent material flushing; after the reaction is finished, carrying out suction filtration through a washing suction filtration assembly, washing with ethyl acetate, merging filtrates, and transferring the merged filtrates into a reaction kettle II for negative pressure distillation concentration; adding ethyl acetate into the obtained product, stirring and dissolving, heating, adding ethanolamine, crystallizing, carrying out suction filtration and washing by combining with a washing suction filtration assembly, centrifuging by virtue of a centrifugal mechanism, and carrying out vacuum drying by virtue of double-cone reduced-pressure drying equipment, so as to obtain a finished product piroctone ethanolamine salt powder; by means of the steps, the synthesis efficiency and quality of piroctone olamine salt are effectively improved, and the proportion of by-products is greatly reduced.

Description

Technical Field

[0001] The invention relates to the technical field of chemical synthesis, in particular to a method for preparing piroctone olamine salt. Background Art

[0002] Piroctone olamine is a common cosmetic additive that effectively inhibits the Malassezia fungus, which causes dandruff. Overgrowth of Malassezia on the scalp can lead to an imbalance in the scalp's ecology, causing dandruff, itching, and other issues. Piroctone olamine can inhibit the growth and reproduction of Malassezia, thereby reducing dandruff and relieving scalp itching.

[0003] The existing synthesis method of piroctone olamine salt requires frequent temperature adjustment during the synthesis process, while the corresponding synthesis equipment has a weak temperature adjustment capability, thereby affecting the synthesis efficiency and synthesis yield of piroctone olamine salt. Summary of the Invention

[0004] The object of the present invention is to provide a method for preparing piroctone olamine salt to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical solutions: A method for preparing piroctone olamine salt comprises the following steps: S1. Prepare reactors 1 and 2, add cyclohexane and 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-one into reactor 1, and adjust the temperature in reactor 1 to 40° C. using the temperature control component; S2. Combine the bubble generating assembly and slowly add hydroxylamine hydrochloride and sodium carbonate in batches to slowly generate bubbles to prevent material from being washed away; S3. After the reaction is completed, the temperature is adjusted to 70-80°C by the temperature control component and kept warm for 26 hours before sampling and testing. After the reaction is completed, the temperature is lowered to 20-30°C, filtered through the washing and filtration component and washed with ethyl acetate. The filtrates are combined and transferred to the second reactor for vacuum distillation and concentration to obtain intermediate A; S4, adding intermediate A to ethyl acetate and stirring to dissolve, heating to 50 ° C and adding ethanolamine, stirring for 20 minutes, and after crystallization, combining the washing and filtration components to perform suction filtration and washing, centrifuging through a centrifuge, and vacuum drying using a double-cone vacuum drying equipment to obtain a finished product piroctone olamine salt powder; The equipment used in the above preparation method includes reactor 1, a temperature control component, a bubble generating component, a washing and filtration component, reactor 2, a centrifugal mechanism, and a double-cone reduced-pressure drying device; the reactor 1 includes a reaction cylinder 1, the top of the reaction cylinder 1 is sealed with a top cover, the top cover is provided with an exhaust pipe and a feed port, the temperature control component is connected to the outer wall of the reaction cylinder 1, the temperature control component includes a temperature control box sleeved on the outside of the reaction cylinder 1, the top cover is provided with a water temperature controller, a water supply pipe is provided between the temperature control box and the water temperature controller, an annular pipe 1 and an annular pipe 2 are respectively provided at the upper and lower ends of the temperature control box, inclined pipes are evenly distributed between the annular pipe 1 and the annular pipe 2, and water outlet holes are evenly provided on the inclined pipes, the bottom of the temperature control box is connected to a return pipe, the other end of the return pipe is connected to the water temperature controller, and a discharge pipe is provided at the bottom of the reactor 1 and the reactor 2.

[0006] As a further solution of the present invention: the bubble generating assembly includes a discharge tray 1 and a discharge tray 2 arranged inside the reaction cylinder 1, the discharge tray 1 is evenly provided with leakage holes 1, the leakage hole 1 is downwardly connected to a discharge pipe 1, the discharge tray 2 is provided with a docking hole at a position corresponding to the discharge pipe 1, the discharge tray 2 is provided with a leakage hole 2 at a position staggered from the docking hole, the leakage hole 2 is downwardly connected to a discharge pipe 2, and a pneumatic telescopic column is provided at the center of the discharge tray 1 and the discharge tray 2, and the pneumatic telescopic column is installed for lifting between the upper side and the top cover.

[0007] As a further solution of the present invention: a lifting rod is inserted into the center of the top cover, a fixing frame is provided on the top cover, a driving gear is horizontally rotatably installed on the fixing frame, the driving gear is connected to a driving motor, a matching rack is provided on the side of the lifting rod, the driving gear and the matching rack are engaged with each other, and the bottom of the lifting rod is connected to a pneumatic telescopic column.

[0008] As a further solution of the present invention: the docking hole is a press-type connecting hole.

[0009] As a further solution of the present invention: the washing and filtration assembly includes a hanging bracket arranged at the bottom of the reaction cylinder, a telescopic motor is arranged on the hanging bracket, the telescopic motor is connected to a plug-in tube, the plug-in tube is sealed and plugged with the discharge pipe at the bottom of the reaction cylinder, the plug-in tube is located at the center of the bottom inner side of the reaction cylinder and is provided with a plugging connector, the outer circle of the plugging connector is evenly distributed with curved tubes, the curved tubes are evenly distributed with filtration ports, the curved tubes are arranged in contact with the bottom surface of the reaction cylinder, the plug-in tube is connected to a telescopic tube, and the telescopic tube is connected to a pump body.

[0010] As a further solution of the present invention: a docking mechanism is provided between the reactor 1 and the reactor 2, and between the reactor 2 and the centrifugal mechanism, the docking mechanism includes a discharge valve connected to the discharge pipe, a fixing frame 2 is provided on the discharge valve, a telescopic motor 2 is provided on the fixing frame 2, the discharge valve is connected to a telescopic tube 2, the telescopic tube 2 is connected to a docking port, a connecting frame is provided on the docking port, the telescopic motor 2 is connected to the connecting frame, a docking valve 1 is provided on the side of the reactor 2, and a docking valve 2 is provided on the side of the centrifugal mechanism.

[0011] As a further solution of the present invention: the centrifugal mechanism includes a centrifugal cylinder, which is rotatably installed around the central axis. The bottom outer ring of the centrifugal cylinder is provided with an outer gear ring, and the outer gear ring is cooperated with the drive gear 2, and the drive gear 2 is connected to the drive motor 2.

[0012] As a further solution of the present invention: a stirring assembly is provided in the second reactor and the centrifugal mechanism, and the stirring assembly includes a stirring motor, and the stirring motor is connected to a stirring rod 1, and the stirring rod 1 extends to the bottom of the reaction cylinder 1 and the centrifugal cylinder.

[0013] As a further solution of the present invention: the inclined tube is spirally arranged, and the water outlet is inclined to point to the side wall of the reaction tube 1.

[0014] Compared with the prior art, the present invention has the following beneficial effects: (1) The raw materials are fed into the reactor 1 in the reactor 1 through the feed port on the top cover. When the reactor 1 is reacting, the temperature inside the reactor 1 is adjusted by combining the temperature control component, and the temperature of the circulating water is adjusted by the water temperature controller. The temperature-adjusted water flow is dispersed and sent into the inclined tube in combination with the water supply pipe and the annular tube 1. The temperature-adjusted water in the inclined tube is sprayed onto the outer wall of the reactor 1, thereby adjusting the reaction temperature in the reactor 1 and continuously keeping it warm.

[0015] (2) During the reaction, the internal pressure may increase rapidly. The pressure inside the reaction tube 1 increases rapidly, causing the material soil to rush out of the reaction vessel. By slowly adding hydroxylamine hydrochloride and sodium carbonate into the reaction tube 1, they react and produce bubbles, thereby eliminating the possible material rushing phenomenon in the reaction tube 1. Hydroxylamine hydrochloride and sodium carbonate need to be added slowly in batches to control the continuous generation of bubbles. By setting up a feed tray one and a feed tray two, first, combine the feed port to feed hydroxylamine hydrochloride onto the feed tray one. At this time, the distance between the feed tray one and the feed tray two is adjusted to the maximum. At this time, the docking hole on the feed tray two is closed, and the hydroxylamine hydrochloride leaks through the feed pipe one to the feed tray two. Then, the pneumatic telescopic column is shortened to reduce the distance between the feed tray one and the feed tray two. The feed pipe one is inserted into the docking hole. At this time, sodium carbonate is continued to be fed into the feed tray one. The sodium carbonate will fall evenly along the feed pipe one into the reaction tube one, while the hydroxylamine hydrochloride slowly and evenly falls along the feed pipe two into the reaction tube one. After contact, the hydroxylamine hydrochloride and sodium carbonate react to generate gas, thereby generating bubbles in the reaction tube one, eliminating the hidden danger of material impact. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 Flowchart of the present invention.

[0017] Figure 2 It is a schematic diagram of the overall structure of the present invention.

[0018] Figure 3 It is a schematic diagram of the cross-section structure of the reactor 1 in the present invention.

[0019] Figure 4 Schematic diagram of the structure of the bubble generating component in the present invention.

[0020] Figure 5 for Figure 4 Enlarged structural diagram at point A in the middle.

[0021] Figure 6 for Figure 4 Enlarged structural diagram at point B in the middle.

[0022] Figure 7 This is a schematic diagram of the temperature control component structure of the present invention.

[0023] Figure 8 It is a structural schematic diagram of the washing and filtration component in the present invention.

[0024] Figure 9 It is a structural schematic diagram of the docking mechanism in the present invention.

[0025] Figure 10 It is a schematic diagram of the cross-section structure of the reactor 2 in the present invention.

[0026] Figure 11It is a schematic diagram of the cross-section structure of the centrifugal mechanism in the present invention.

[0027] In the figure: 1. Reactor 1; 10. Reactor 1; 11. Top cover; 12. Exhaust pipe; 13. Feed port; 14. Temperature control assembly; 140. Water temperature controller; 141. Water supply pipe; 142. Temperature control box; 143. Annular pipe 1; 144. Inclined pipe; 145. Annular pipe 2; 146. Return pipe; 15. Bubble generating assembly; 150. Feed tray 1; 1500. Leakage hole 1; 151. Feed tube 1; 152. Feed tray 2; 1520. Leakage hole 2; 1521. Docking hole; 153. Feed tube 2; 154. Lifting rod; 1540. Matching rack; 1541. Fixing frame 1; 1542. Driving gear 1; 1543. Driving Motor 1; 155. Pneumatic telescopic column; 16. Washing and filtration assembly; 160. Hanging frame; 161. Telescopic motor 1; 162. Plug-in tube; 163. Telescopic tube 1; 164. Pump body; 165. Plug connector; 166. Bending tube; 167. Filtration port; 17. Discharge pipe; 2. Docking mechanism; 20. Discharge valve; 21. Telescopic tube 2; 22. Docking port; 23. Fixed frame 2; 24. Telescopic motor 2; 25. Connecting frame; 3. Reactor 2; 31. Stirring motor; 32. Stirring rod 1; 33. Docking valve 1; 4. Centrifugal mechanism; 40. Centrifugal cylinder; 41. Docking valve 2; 42. Outer gear ring; 43. Drive gear 2; 44. Drive motor 2. DETAILED DESCRIPTION

[0028] In the description of the present invention, it should be understood that the terms "longitudinal", "transverse", "up", "down", "top", "bottom", "inside", "outside", 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, 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 should not be understood as a limitation on the present invention.

[0029] Furthermore, the terms "one" and "two" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referenced. Thus, a feature specified with "one" or "two" may explicitly or implicitly include one or more of the features. In the description of the present invention, "plurality" means two or more, unless otherwise specifically defined.

[0030] In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "connect," "fixed," etc. should be understood broadly. For example, they may refer to fixed connection, detachable connection, or integration; mechanical connection or electrical connection; direct connection or indirect connection through an intermediate medium; internal communication between two components or interaction between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0031] The technical solution of the present invention will be further described in detail below in conjunction with specific implementation methods.

[0032] like Figure 1 、 Figure 2 As shown, a method for preparing piroctone olamine salt comprises the following steps: Weigh 340 kg of 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-one, 290 kg of hydroxylamine hydrochloride, 148.4 kg of sodium carbonate, 400 kg of cyclohexane, 880 kg of ethyl acetate, and 103 kg of ethanolamine; S1. Prepare a reactor 1 (3000-5000 L) and a reactor 2 (3) (2000-3000 L). Add cyclohexane and 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-one to the reactor 1. Adjust the temperature of the reactor 1 to 40° C. using the temperature control assembly 14. S2. Combine the bubble generating assembly 15 and slowly add hydroxylamine hydrochloride and sodium carbonate in batches to slowly generate bubbles to prevent material from being washed away; S3. After the reaction is completed, the temperature is adjusted to 70-80°C by the temperature control component 14 and kept warm for 26 hours before sampling and testing. After the reaction is completed, the temperature is lowered to 20-30°C, filtered through the washing and filtration component 16 and washed with ethyl acetate. The filtrates are combined and transferred to the reactor 2 3 for vacuum distillation and concentration to obtain intermediate A; S4, adding ethyl acetate to intermediate A and stirring to dissolve, heating to 50 ° C and adding ethanolamine, stirring for 20 minutes, and after crystallization, combining the washing and filtration assembly 16 to perform suction filtration and washing, centrifuging through the centrifugal mechanism 4, and vacuum drying using a double-cone vacuum drying device to obtain a finished product piroctone olamine salt powder; like Figure 2 、 Figure 3 、 Figure 7As shown, the equipment used in the above preparation method includes a reactor 1, a temperature control component 14, a bubble generating component 15, a washing and filtering component 16, a reactor 2 3, a centrifugal mechanism 4, and a double-cone reduced-pressure drying device; the reactor 1 includes a reaction cylinder 10, the top of the reaction cylinder 10 is sealed with a top cover 11, the top cover 11 is provided with an exhaust pipe 12 and a feed port 13, the temperature control component 14 is connected to the outer wall of the reaction cylinder 10, the temperature control component 14 includes a temperature control box 142 sleeved on the outside of the reaction cylinder 10, and the top cover 11 is provided with a A water temperature controller 140 is provided with a water supply pipe 141 between the temperature control box 142 and the water temperature controller 140. An annular pipe 143 and an annular pipe 2 145 are respectively provided at the upper and lower ends of the temperature control box 142. Inclined pipes 144 are evenly distributed between the annular pipe 143 and the annular pipe 2 145. Water outlet holes are evenly provided on the inclined pipes 144. A return pipe 146 is connected to the bottom of the temperature control box 142. The other end of the return pipe 146 is connected to the water temperature controller 140. A discharge pipe 17 is provided at the bottom of the reactor 1 and the reactor 2 3.

[0033] Specifically, the raw materials are fed into the reactor 1 in the reactor 1 through the feed port 13 on the top cover 11. When the reaction tube 10 is reacting, the temperature inside the reaction tube 10 is adjusted in conjunction with the temperature control component 14, the temperature of the circulating water is adjusted by the water temperature controller 140, and the temperature-adjusted water flow is dispersed and sent into the inclined tube 144 in conjunction with the water supply pipe 141 and the annular tube 143. The temperature-adjusted water in the inclined tube 144 is sprayed onto the outer wall of the reaction tube 10, thereby adjusting the reaction temperature in the reactor 1 and continuously keeping it warm.

[0034] Further, such as Figure 4 、 Figure 5 、 Figure 6 As shown, the bubble generating assembly 15 includes a discharge tray 150 and a discharge tray 152 arranged inside the reaction cylinder 10, the discharge tray 150 is evenly provided with leakage holes 1500, the leakage holes 1500 are downwardly connected to the discharge pipe 151, the discharge tray 152 is provided with a docking hole 1521 at a position corresponding to the discharge pipe 151, the discharge tray 152 is provided with a leakage hole 1520 at a position staggered from the docking hole 1521, the leakage hole 1520 is downwardly connected to the discharge pipe 2 153, and a pneumatic telescopic column 155 is provided at the center of the discharge tray 150 and the discharge tray 152, and the upper side of the pneumatic telescopic column 155 is installed for lifting between the top cover 11.

[0035] Specifically, during the reaction process, the internal pressure may increase rapidly, and the pressure in the reaction tube 10 may increase rapidly, causing the material soil to rush out of the reaction container. By slowly adding hydroxylamine hydrochloride and sodium carbonate into the reaction tube 10, a reaction occurs to produce bubbles, thereby eliminating the material rushing phenomenon that may occur in the reaction tube 10. Hydroxylamine hydrochloride and sodium carbonate need to be added slowly in batches to control the continuous generation of bubbles. By setting the feed tray 150 and the feed tray 2 152, first, the feed port 13 is combined to feed hydroxylamine hydrochloride to the feed tray 150. At this time, the distance between the feed tray 150 and the feed tray 2 152 is adjusted to the maximum. At this time, the docking hole 1521 on the feed tray 2 152 is closed, and the hydroxylamine hydrochloride leaks through the feed pipe 151 to the feed tray 2 152, and then combined with the pneumatic telescopic column 15 5 is shortened, so that the distance between the lower material tray 150 and the lower material tray 2 152 is reduced, and the lower material tray 151 is inserted into the docking hole 1521. At this time, sodium carbonate is continued to be fed into the lower material tray 150. The sodium carbonate will fall evenly along the lower material tray 151 into the reaction tube 10, while the hydroxylamine hydrochloride will fall slowly and evenly along the lower material tray 2 153 into the reaction tube 10. After the hydroxylamine hydrochloride and the sodium carbonate come into contact, they react to generate gas, thereby generating bubbles in the reaction tube 10, eliminating the risk of material impact.

[0036] Further, such as Figure 4 、 Figure 5 As shown, a lifting rod 154 is inserted into the center of the top cover 11, and a fixing frame 1541 is provided on the top cover 11. A driving gear 1542 is horizontally rotatably mounted on the fixing frame 1541. The driving gear 1542 is connected to a driving motor 1543. A mating rack 1540 is provided on the side of the lifting rod 154. The driving gear 1542 and the mating rack 1540 are engaged with each other. The bottom of the lifting rod 154 is connected to a pneumatic telescopic column 155.

[0037] Specifically, the driving motor 1543 and the driving gear 1542 drive the matching rack 1540 to move up and down, thereby adjusting the height of the bubble generating assembly 15 connected to the bottom, and adjusting the bubble generating position in real time in combination with the height of the raw materials inside the reaction tube 10, thereby ensuring the bubble generating effect.

[0038] Furthermore, the docking hole 1521 is a press-type connecting hole.

[0039] Specifically, the docking hole 1521 is set as a press-type connecting hole. When the lower feeding tube 151 is separated from the docking hole 1521, the docking hole 1521 is closed, and the hydroxylamine hydrochloride falls through the lower feeding tray 150, the leakage hole 1500, and the lower feeding tube 151 to the lower feeding tray 2 152, and then falls into the reaction tube 10 through the leakage hole 2 1520 and the lower feeding tube 2 153. When the lower feeding tube 151 is plugged into the docking hole 1521, the sodium carbonate falls directly into the bottom of the reaction tube 10 along the leakage hole 1500 and the lower feeding tube 151, thereby completing the filling of hydroxylamine hydrochloride and sodium carbonate.

[0040] Further, such as Figure 8 As shown, the washing and filtration assembly 16 includes a hanging bracket 160 arranged at the bottom of the reaction barrel 10, and a telescopic motor 161 is provided on the hanging bracket 160. The telescopic motor 161 is connected to a plug-in tube 162, and the plug-in tube 162 is sealed and plugged with the discharge pipe 17 at the bottom of the reaction barrel 10. The plug-in tube 162 is located at the center of the bottom inner side of the reaction barrel 10 and is provided with a plugging connector 165. The outer circle of the plugging connector 165 is evenly distributed with curved tubes 166, and the curved tubes 166 are evenly distributed with filtration ports 167. The curved tube 166 is arranged to fit the bottom surface of the reaction barrel 10, and the plug-in tube 162 is connected to a telescopic tube 163, and the telescopic tube 163 is connected to a pump body 164.

[0041] Specifically, when the reactants at the bottom of reaction tube 10 need to be filtered, pump body 164, curved tube 166, and filtration port 167 are used to perform the filtration. After the filtration is complete, pump body 164 pumps ethyl acetate into reaction tube 10 for washing. During the filtration and washing process, telescopic motor 161 controls plug connector 165 to seal against the bottom of reaction tube 10 to prevent the product from entering discharge pipe 17. After the filtration is complete, plug connector 165 is controlled to rise, opening discharge pipe 17 and delivering the product to reactor 3 for further reaction.

[0042] Further, such as Figure 2 、 Figure 9 As shown, a docking mechanism 2 is provided between the reactor 1 and the reactor 2 3, as well as between the reactor 2 3 and the centrifugal mechanism 4. The docking mechanism 2 includes a discharge valve 20 connected to the discharge pipe 17, a fixing frame 23 is provided on the discharge valve 20, a telescopic motor 24 is provided on the fixing frame 23, the discharge valve 20 is connected to the telescopic tube 21, the telescopic tube 21 is connected to the docking port 22, a connecting frame 25 is provided on the docking port 22, the telescopic motor 24 is connected to the connecting frame 25, a docking valve 1 33 is provided on the side of the reactor 2 3, and a docking valve 2 41 is provided on the side of the centrifugal mechanism 4.

[0043] Specifically, the docking port 22 is driven to move by the telescopic motor 24 and connected to the docking valve 1 33 or the docking valve 2 41 respectively, thereby connecting the reactor 1 1, the reactor 2 3, and the centrifugal mechanism 4, and the reaction product is circulated among the reactor 1 1, the reactor 2 3, and the centrifugal mechanism 4, thereby realizing streamlined processing and improving synthesis efficiency and synthesis quality.

[0044] Further, such as Figure 11 As shown, the centrifugal mechanism 4 includes a centrifugal cylinder 40, which is rotatably installed around the central axis. The bottom outer ring of the centrifugal cylinder 40 is provided with an outer gear ring 42, and the outer gear ring 42 is cooperated with the drive gear 2 43, and the drive gear 2 43 is connected to the drive motor 2 44.

[0045] Specifically, the docking mechanism 2 sends the filtered and washed product into the centrifuge cylinder 40, and then the docking mechanism 2 is separated from the centrifuge cylinder 40. At this time, the drive motor 2 44 and the drive gear 2 43 are combined to drive the centrifuge cylinder 40 to rotate, thereby centrifuging the product in the centrifuge cylinder 40 to obtain a wet product, and finally send it to a double-cone vacuum drying device for drying to obtain piroctone ethanolamine salt powder.

[0046] Further, such as Figure 10 As shown, a stirring assembly is provided in the reactor 2 3 and the centrifugal mechanism 4 , and the stirring assembly includes a stirring motor 31 , and the stirring motor 31 is connected to a stirring rod 1 32 , and the stirring rod 1 32 extends to the bottom of the reaction cylinder 10 and the centrifugal cylinder 40 .

[0047] Further, such as Figure 7 As shown, the inclined tube 144 is spirally arranged, and the water outlet is inclined to point to the side wall of the reaction tube 10.

[0048] The working principle of the embodiment of the present invention is: like Figures 1-11As shown, raw materials are fed into Reactor 1 through feed port 13 on top cover 11. While Reactor 10 is reacting, the temperature inside Reactor 10 is adjusted using temperature control assembly 14. The temperature of the circulating water is adjusted using water temperature controller 140. The temperature-adjusted water is dispersed and fed into inclined tube 144 using water supply pipe 141 and annular tube 143. The temperature-adjusted water in inclined tube 144 is sprayed onto the outer wall of Reactor 10, thereby adjusting the reaction temperature within Reactor 1 and maintaining heat. During the reaction, internal pressure may increase rapidly, causing the pressure inside Reactor 10 to rise rapidly, causing the material to rush upward out of the reaction vessel. By slowly adding hydroxylamine hydrochloride and sodium carbonate to Reactor 10, causing them to react and generate bubbles, this phenomenon can be eliminated. Hydroxylamine hydrochloride and sodium carbonate need to be added slowly in batches to control the continuous generation of bubbles. By setting the unloading tray 150 and the unloading tray 2 152, first, the hydroxylamine hydrochloride is fed to the unloading tray 1 150 in conjunction with the feed port 13. At this time, the distance between the unloading tray 150 and the unloading tray 2 152 is adjusted to the maximum. At this time, the docking hole 1521 on the unloading tray 2 152 is closed, and the hydroxylamine hydrochloride leaks from the unloading pipe 151 to the unloading tray 2 152. Then, the pneumatic telescopic column 15 is combined with the pneumatic telescopic column 15 5 is shortened, reducing the distance between lower tray 150 and lower tray 2 152. Lower tube 151 is inserted into docking hole 1521. Sodium carbonate is then fed into lower tray 150. It will evenly fall along lower tube 151 into reaction tube 10, while hydroxylamine hydrochloride slowly and evenly falls along lower tube 2 153 into reaction tube 10. Hydroxylamine hydrochloride and sodium carbonate react to form gas, generating bubbles within reaction tube 10 and eliminating the risk of material impact. Drive motor 1543 and drive gear 1542 drive the mating rack 1540 up and down, adjusting the height of the bubble generating assembly 15 connected to the bottom. The bubble generating position is adjusted in real time based on the height of the raw materials within reaction tube 10, ensuring effective bubble generation. Docking hole 1521 is configured as a push-type connecting hole. When lower feed tube 151 is separated from docking hole 1521, docking hole 1521 is sealed, and hydroxylamine hydrochloride falls through discharge tray 150, leak hole 1500, and discharge tube 151 onto discharge tray 2 152. It then falls into reaction tube 10 through leak hole 2 1520 and discharge tube 2 153. When lower feed tube 151 is plugged into docking hole 1521, sodium carbonate falls directly into the bottom of reaction tube 10 along leak hole 1500 and discharge tube 151, completing the filling of hydroxylamine hydrochloride and sodium carbonate. When the reactants at the bottom of reaction tube 10 need to be filtered, pump body 164, curved tube 166, and filter port 167 are used to perform the filtration. After the filtration is completed, pump body 164 pumps ethyl acetate into reaction tube 10 for washing.In the process of suction filtration and washing, it is necessary to control the blocking connector 165 by telescopic motor 161 and cooperate with the bottom seal of reaction drum 10 to avoid product from entering discharge pipe 17. After suction filtration ends, control the blocking connector 165 to rise, open discharge pipe 17, and send product into reactor 2 3 and continue to react. Drive docking port 22 to move by telescopic motor 2 24, be connected with docking valve 1 33 or docking valve 2 41 respectively, thereby reactor 1, reactor 2 3, centrifugal mechanism 4 are connected, reaction product is circulated between reactor 1, reactor 2 3, centrifugal mechanism 4, thereby realize streamlining processing, improve synthesis efficiency and synthesis quality. Docking mechanism 2 sends the product after suction filtration washing into centrifugal drum 40, and docking mechanism 2 is separated from centrifugal drum 40 subsequently, now drives centrifugal drum 40 to rotate in conjunction with drive motor 2 44, drive gear 2 43, thereby the product in centrifugal drum 40 is centrifuged to obtain wet product, finally sends into biconical decompression drying equipment and is dried, obtains piroctone olamine salt powder.

[0049] The foregoing description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention. Any reference numerals in the claims shall not be construed as limiting the claims involved.

[0050] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A method for preparing piroctone olamine salt, characterized in that, The steps include: S1. Prepare reactor 1 (1) and reactor 2 (3), add cyclohexane and 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-one into reactor 1 (1), and adjust the temperature in reactor 1 (1) to 40°C using the temperature control component (14); S2, slowly adding hydroxylamine hydrochloride and sodium carbonate in batches in combination with the bubble generating assembly (15), slowly generating bubbles to prevent material from being washed away; S3. After the reaction is completed, the temperature is adjusted to 70-80°C by using the temperature control component (14) and kept warm for 26 hours before sampling and testing. After the reaction is completed, the temperature is lowered to 20-30°C, and the mixture is filtered through the washing and filtration component (16) and washed with ethyl acetate. The filtrates are combined and transferred to the second reactor (3) for vacuum distillation and concentration to obtain intermediate A. S4, adding intermediate A to ethyl acetate and stirring to dissolve, heating to 50°C and adding ethanolamine, stirring for 20 minutes, and after crystallization, filtering and washing with a washing and filtration assembly (16), centrifuging through a centrifuge (4), and vacuum drying using a double-cone vacuum drying apparatus to obtain a finished product of piroctone ethanolamine salt powder; The equipment used in the above preparation method includes a reactor (1), a temperature control component (14), a bubble generating component (15), a washing and filtering component (16), a reactor (3), a centrifugal mechanism (4), and a double-cone vacuum drying device; the reactor (1) includes a reaction barrel (10), the top of the reaction barrel (10) is sealed with a top cover (11), the top cover (11) is provided with an exhaust pipe (12) and a feed port (13), the temperature control component (14) is connected to the outer wall of the reaction barrel (10), the temperature control component (14) includes a temperature control box (142) sleeved on the outside of the reaction barrel (10), the top cover (11) is provided with a water A temperature controller (140) is provided, a water supply pipe (141) is provided between the temperature control box (142) and the water temperature controller (140), an annular pipe 1 (143) and an annular pipe 2 (145) are provided at the upper and lower ends of the temperature control box (142), inclined pipes (144) are evenly distributed between the annular pipe 1 (143) and the annular pipe 2 (145), and water outlet holes are evenly provided on the inclined pipes (144), the bottom of the temperature control box (142) is connected to a return pipe (146), the other end of the return pipe (146) is connected to the water temperature controller (140), and a discharge pipe (17) is provided at the bottom of the reactor 1 (1) and the reactor 2 (3).

2. a preparation method of piroctone olamine salt according to claim 1, is characterized in that, The bubble generating assembly (15) includes a feed tray 1 (150) and a feed tray 2 (152) arranged inside the reaction cylinder 1 (10), wherein leakage holes 1 (1500) are evenly arranged in the feed tray 1 (150), and the leakage holes 1 (1500) are downwardly connected to the feed tube 1 (151), and a docking hole (1521) is arranged at a position corresponding to the feed tube 1 (151) on the feed tray 2 (152), and a leakage hole 2 (1520) is arranged at a position staggered from the docking hole (1521) on the feed tray 2 (152), and the leakage hole 2 (1520) is downwardly connected to the feed tube 2 (153), and a pneumatic telescopic column (155) is arranged at the center of the feed tray 1 (150) and the feed tray 2 (152), and the upper side of the pneumatic telescopic column (155) is installed to be lifted and lowered between the top cover (11).

3. a preparation method of piroctone olamine salt according to claim 2, is characterized in that, A lifting rod (154) is inserted into the center of the top cover (11), a fixing frame (1541) is provided on the top cover (11), a driving gear (1542) is horizontally rotatably mounted on the fixing frame (1541), the driving gear (1542) is connected to a driving motor (1543), a matching rack (1540) is provided on the side of the lifting rod (154), the driving gear (1542) and the matching rack (1540) are meshed with each other, and the bottom of the lifting rod (154) is connected to a pneumatic telescopic column (155).

4. a preparation method of piroctone olamine salt according to claim 2, is characterized in that, The docking hole (1521) is a press-type communicating hole.

5. A method for preparing a piroctone olamine salt according to claim 1, wherein The washing and filtration assembly (16) includes a hanging frame (160) arranged at the bottom of the reaction barrel (10), a telescopic motor (161) is arranged on the hanging frame (160), and the telescopic motor (161) is connected to a plug-in pipe (162), and the plug-in pipe (162) is sealed and plugged with the discharge pipe (17) at the bottom of the reaction barrel (10). The plug-in pipe (162) is located at the center of the bottom inner side of the reaction barrel (10) and is provided with a plugging connector (165). The outer circle of the plugging connector (165) is evenly distributed with curved tubes (166), and the curved tube (166) is evenly distributed with filtration ports (167). The curved tube (166) is arranged in contact with the bottom surface of the reaction barrel (10), the plug-in pipe (162) is connected to a telescopic tube (163), and the telescopic tube (163) is connected to a pump body (164).

6. A method for preparing a piroctone olamine salt according to claim 1, characterized in that, A docking mechanism (2) is provided between the reactor 1 (1) and the reactor 2 (3), and between the reactor 2 (3) and the centrifugal mechanism (4). The docking mechanism (2) includes a discharge valve (20) connected to the discharge pipe (17). A fixing frame 2 (23) is provided on the discharge valve (20). A telescopic motor 2 (24) is provided on the fixing frame 2 (23). The discharge valve (20) is connected to a telescopic tube 2 (21). The telescopic tube 2 (21) is connected to a docking port (22). A connecting frame (25) is provided on the docking port (22). The telescopic motor 2 (24) is connected to the connecting frame (25). A docking valve 1 (33) is provided on the side of the reactor 2 (3), and a docking valve 2 (41) is provided on the side of the centrifugal mechanism (4).

7. A method for preparing a piroctone olamine salt according to claim 1, characterized in that, The centrifugal mechanism (4) includes a centrifugal cylinder (40), which is rotatably mounted around a central axis. An outer gear ring (42) is provided on the bottom outer ring of the centrifugal cylinder (40), and a second drive gear (43) is mounted on the outer gear ring (42). The second drive gear (43) is connected to a second drive motor (44).

8. A method for preparing a piroctone olamine salt according to claim 6, characterized in that, A stirring assembly is provided in the reactor 2 (3) and the centrifugal mechanism (4), and the stirring assembly includes a stirring motor (31). The stirring motor (31) is connected to a stirring rod 1 (32), and the stirring rod 1 (32) extends to the bottom of the reaction cylinder 1 (10) and the centrifugal cylinder (40).

9. A method for preparing a piroctone olamine salt according to claim 2, characterized in that, The inclined tube (144) is arranged in a spiral shape, and the water outlet is inclined to point to the side wall of the reaction cylinder (10).

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