Purification processing technology of lactulose oral solution

Abstract

The invention belongs to the technical field of purification equipment, and particularly discloses a lactulose oral solution purification processing technology. According to the lactulose oral solution purification processing technology, a reaction kettle is adopted, a tank cover is arranged at the top of the reaction kettle, and feeding assemblies are arranged in the tank cover and the reaction kettle; the feeding assembly comprises a feeding port, a protective cover, a feeding pipe, a guide pipe and a supporting and limiting assembly, and the feeding port is formed in the top of the tank cover. The feeding pipe is limited through the supporting and limiting structure, so that the bottom end of the feeding pipe is always inserted below the liquid level of the reaction kettle, a solution is prevented from entraining a large amount of air to enter the kettle to form dense bubbles, and the feeding pipe is prevented from vibrating due to the stability of connection between the feeding pipe and the guide pipe and is prevented from being influenced by vibration; and meanwhile, the bottom of the feeding pipe can be shielded through the effect of the dispersing plate, the materials are prevented from being sprayed out from a pipe opening and directly impacting the liquid level to form splashing bubbles, and the material conveying effect is conveniently improved.

Description

Technical Field

[0001] This invention belongs to the field of purification equipment technology, and specifically relates to a purification process for lactulose oral solution. Background Technology

[0002] Lactulose is an important medicinal ingredient widely used in the pharmaceutical industry. It is a disaccharide (4-O-β-D-galactopyranosyl-D-fructose) formed by the isomerization of lactose under alkaline conditions. Its oral solution is mainly used to treat chronic or habitual constipation, hepatic encephalopathy, etc. Under alkaline catalysis, the intramolecular glucose units of lactose (α-D-galactopyranosyl-(1→4)-D-glucose) undergo isomerization, converting to fructose units to produce lactulose. Subsequent steps such as neutralization, decolorization, desalting, and chromatographic separation remove unreacted lactose, byproducts (galactose, mannose), and impurities, ultimately resulting in a clear and stable oral solution.

[0003] In the existing technology, it is necessary to transfer the clarified lactose solution into the reaction vessel for reaction. However, during use, when the clarified lactose solution is transported through the feed pipe, bubbles are easily generated, and the feed pipe is easily vibrated in the reaction vessel, resulting in low stability and affecting the efficiency of solution transfer.

[0004] Therefore, it is necessary to invent a purification and processing technology for lactulose oral solution to solve the above problems. Summary of the Invention

[0005] To address the aforementioned problems, this invention provides a purification and processing technology for lactulose oral solution, thereby resolving the issues raised in the background section.

[0006] To achieve the above objectives, the present invention provides the following technical solution: A process for purifying lactulose oral solution, using a reaction vessel with a lid on top and a feeding assembly inside the reaction vessel. The feeding assembly includes a feed inlet, a protective cover, a feed pipe, a guide pipe, and a support and limiting component. The feed inlet is located on the top of the can lid, and a protective cover is installed on the top of the feed inlet. The protective cover is hinged to the top of the can lid. A guide pipe is installed at the bottom of the feed inlet. One end of the guide pipe is fixedly connected to the bottom of the can lid, and the feed pipe is fixedly connected to the bottom of the guide pipe. Support and limiting components are installed at both ends of the feed pipe.

[0007] Furthermore, a stirring assembly is provided on the tank cover and the reactor. The stirring assembly includes a motor, a mounting base, a rotating rod, and a stirring rod. The mounting base is fixedly connected to the top of the tank cover, and the motor is fixedly connected to the top of the mounting base. The rotating rod is fixedly connected to the output end of the motor. One end of the rotating rod passes through the mounting base and extends into the reactor. Multiple stirring rods are fixedly connected to the outside of the rotating rod.

[0008] Further, the guide pipe is located in the tank cover, the feeding pipe is located in the reaction kettle, the feeding pipe is located at the end of the stirring rod away from the rotating rod, the outer side of the end of the feeding pipe close to the tank cover is fixedly connected with the connecting pipe, the connecting pipe is provided with a slot on the outer side, the connecting pipe is provided with a sliding block on both sides, the sliding block is fixedly connected with a plug rod on the side close to the connecting pipe.

[0009] Further, the support limiting assembly comprises a guide block, a fixed block, a dispersion plate, a first telescopic rod, a connecting spring and a clamping structure, the guide block is arranged on the outer side of the bottom end of the feeding pipe, the bottom of the guide block is fixedly connected with the fixed block, the bottom of the fixed block is provided with a groove, the inner wall of the groove is provided with the dispersion plate, the top of the dispersion plate is fixedly connected with two first telescopic rods, the two first telescopic rods are provided with the connecting spring inside, the guide block and the fixed block are provided with a mounting groove inside, and the mounting groove is provided with the clamping structure.

[0010] Further, the guide block and the fixed block are fixedly connected with the inner wall of the reaction kettle on one side, the bottom end of the feeding pipe extends through the guide block to the mounting groove on the top of the fixed block, one end of the connecting spring is fixedly connected with the inner wall of the top of the groove, and the other end is fixedly connected with the dispersion plate, and the clamping structure is symmetrically arranged on both sides of the feeding pipe.

[0011] Further, the side close to the feeding pipe of the guide block is a slope, the radius of the dispersion plate is greater than the radius of the feeding pipe, the clamping structure comprises a clamping plate, a moving block and a compression spring, the clamping block is slidably connected with the inner wall of the mounting groove on both sides, the moving block is fixedly connected with the clamping block on one side, the other side is attached to the outer side of the feeding pipe, the compression spring is fixedly connected with the moving block on the side away from the feeding pipe, and one end of the compression spring is fixedly connected with the inner wall of the mounting groove.

[0012] Further, the support limiting assembly further comprises a fixed plate, a support plate and a second telescopic rod, the fixed plate is arranged at the bottom of the connecting pipe, the middle of the fixed plate is fixedly connected with the feeding pipe, the top of the fixed plate is fixedly connected with the support plate on both sides, the top end of the support plate is fixedly connected with the bottom of the tank cover, the side close to the sliding block of the support plate is fixedly connected with the second telescopic rod, and one end of the second telescopic rod is fixedly connected with the sliding block away from the plug rod.

[0013] Further, the side close to the connecting pipe of the feeding pipe is provided with a vibration structure, the vibration structure comprises a connecting plate, an electric telescopic rod, a moving structure, a movable plate, a limiting rod, a fixed rod and a knocking block, the connecting plate is rotatably connected at the top end of the rotating rod, the bottom of the connecting plate is fixedly connected with the electric telescopic rod, the electric telescopic rod is provided with the movable plate at one end, the movable plate is screwedly connected on the rotating rod, the movable plate is movably connected with the limiting rod at both ends, the side close to the feeding pipe of the movable plate is provided with the fixed rod, one end of the fixed rod is fixedly connected with the knocking block, and the movable plate is provided with the moving slot inside, and the moving structure is arranged in the moving slot.

[0014] Further, the electric telescopic rod extends through the bottom of the tank cover into the reaction kettle, the one end of the rod is fixedly connected with the bottom of the tank cover, the other end is rotatably connected with the top of the stirring rod, the moving structure comprises a moving rod, a round convex, a pushing block and a fixed spring, the moving rod is fixedly connected at the bottom of the electric telescopic rod, the bottom of the moving rod is fixedly connected with the round convex, the fixed block is provided with the pushing block at the bottom of the round convex, the side of the pushing block is fixedly connected with the fixed rod, the other side is fixedly connected with the fixed spring, and the side, away from the pushing block, of the fixed spring is fixedly connected with the inner wall of the moving groove.

[0015] A lactulose oral solution purification processing technology, comprising the following steps: Step one: mix food-grade lactose (purity ≥ 99%) with purified water at a ratio of 1:3, heat and stir at 50-60°C until completely dissolved, filter after adding activated carbon to adsorb impurities, and obtain a clear lactose solution; Step two: the clear lactose solution is introduced into the feed pipe through the guide pipe, and is stirred in the reaction kettle through the feed pipe. When the feed pipe is transported, it is supported and fixed by the support limiting structure, and the energy is dispersed by the dispersion plate, then flows down along the dispersion plate, and then is knocked by the vibration structure to remove the material adhered to the wall of the feed pipe. Then, the lactose solution is heated to 55-65°C, sodium hydroxide is added dropwise to adjust the pH to 8.5-9.5, and the reaction is kept for 1.5-2.5 hours (monitored by HPLC). When the lactulose conversion rate reaches about 40%, the reaction is stopped. Hydrochloric acid is added dropwise into the reaction kettle to adjust the pH of the reaction solution to neutral (6.8-7.2), and activated carbon is added at 60-65°C. Stir for 30 minutes by the stirring assembly, remove the pigment and impurities by filtration, and obtain a crude lactulose solution; Step three: pass the crude solution through a "cation resin + anion resin" column to remove salts and small molecular impurities (monitor the conductivity of the effluent ≤5 μS / cm), then use simulated moving bed chromatography to separate and obtain a lactulose solution with a purity of ≥90%. The pure lactulose solution is transferred into a double-effect vacuum concentrator, concentrated to a concentration of 60%-65% at a low temperature (50-55°C) under vacuum, the pH is adjusted to 4.0-5.0 by adding citric acid / sodium citrate, and the purified water is added to the specified size of the oral solution (e.g. 10 ml containing 5 g of lactulose). Step four: filter the prepared solution with a 0.22 μm filter membrane, sterilize it in an oral solution bottle, sterilize it at 121°C for 15 minutes, cool it, label it, package it, and obtain the finished product.

[0016] The technical effects and advantages of the present application are: 1、The present application limits the feed pipe by supporting limiting structure, so that the bottom end of the feed pipe is always inserted below the liquid level of the reaction kettle, preventing the solution from carrying a large amount of air into the kettle to form dense bubbles, and the stability of the feed pipe connected with the guide pipe is improved, preventing the feed pipe from being affected by vibration, so that the feed pipe is not convenient to feed, and the bottom of the feed pipe is shielded by the dispersing plate to prevent the material from being sprayed from the pipe opening to directly impact the liquid surface to form splashing bubbles, thereby improving the material conveying effect.

[0017] 2、The present application moves the fixed rod and the knocking block driven by the movable plate, the rotating rod and the limiting rod, so that the movable plate can move to different positions of the feed pipe, and the outer side is knocked, preventing the material in the feed pipe from being retained or deposited, thereby improving the efficiency of the feed pipe feeding, and facilitating use. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 is the overall structure schematic diagram of the embodiment of the present application; Figure 2 is the cross-sectional view of the reaction kettle of the embodiment of the present application; Figure 3 is the internal structure diagram of the reaction kettle of the embodiment of the present application; Figure 4 is the structure diagram of the vibration structure of the embodiment of the present application; Figure 5 is the structure diagram of the Figure 4 of the embodiment of the present application; Figure 6 is the structure diagram of the supporting limiting structure and the feed pipe of the embodiment of the present application; Figure 7 is the structure diagram of the feed pipe, the guide block and the fixed block of the embodiment of the present application; Figure 8 is the cross-sectional view of the guide block and the fixed block of the embodiment of the present application; Figure 9 is the actual object diagram of the embodiment of the present application.

[0019] In the figure: 1, reaction kettle; 2, kettle cover; 3, feed pipe; 4, guide pipe; 5, motor; 6, rotating rod; 7, stirring rod; 8, connecting pipe; 9, sliding block; 10, insertion rod; 11, guide block; 12, fixed block; 13, dispersing plate; 14, first telescopic rod; 15, clamping plate; 16, moving block; 17, compression spring; 18, fixed plate; 19, support plate; 20, second telescopic rod; 21, electric telescopic rod; 22, movable plate; 23, limiting rod; 24, fixed rod; 25, knocking block; 26, moving rod; 27, round convex; 28, pushing block. DETAILED DESCRIPTION

[0020] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments.

[0021] This invention provides a purification and processing technology for lactulose oral solution, such as... Figures 1 to 9 As shown, it includes a reactor 1, a tank cover 2 is provided on the top of the reactor 1, and a feeding assembly is provided inside the tank cover 2 and the reactor 1; The feeding assembly includes a feeding port, a protective cover, a feeding pipe 3, a guide pipe 4, and a support and limiting component. The feeding port is located at the top of the can lid 2, and a protective cover is installed at the top of the feeding port. The protective cover is hinged to the top of the can lid 2. A guide pipe 4 is installed at the bottom of the feeding port. One end of the guide pipe 4 is fixedly connected to the bottom of the can lid 2, and the feeding pipe 3 is fixedly connected to the bottom of the guide pipe 4. Support and limiting components are installed at both ends of the feeding pipe 3.

[0022] A stirring assembly is provided on the tank cover 2 and the reactor 1. The stirring assembly includes a motor 5, a mounting base, a rotating rod 6 and a stirring rod 7. The mounting base is fixedly connected to the top of the tank cover 2, and the motor 5 is fixedly connected to the top of the mounting base. The rotating rod 6 is fixedly connected to the output end of the motor 5. One end of the rotating rod 6 passes through the mounting base and extends into the reactor 1. Multiple sets of stirring rods 7 are fixedly connected to the outer side 1 of the rotating rod 6.

[0023] Open the protective cover to expose the inlet. The clarified lactose solution enters the inlet through the guide tube 4 into the inlet pipe 3. The guide tube 4 guides the solution, causing it to transfer from the inlet pipe 3 into the reaction vessel 1 for stirring. During the flow of the inlet pipe 3, a supporting and limiting structure supports and fixes it, ensuring that the bottom of the inlet pipe 3 is always below the liquid surface in the reaction vessel 1. This prevents the solution from carrying a large amount of air into the vessel, forming dense bubbles. The stability of the connection between the inlet pipe 3 and the guide tube 4 improves the stability of the inlet pipe 3 within the reaction vessel 1. Then, the lactose solution... The liquid is heated to 55-65℃, and sodium hydroxide is added dropwise to adjust the pH to 8.5-9.5. The reaction is maintained at this temperature for 1.5-2.5 hours (monitored by HPLC). The reaction is stopped when the lactulose conversion rate reaches about 40%. Hydrochloric acid is added dropwise to reactor 1 to adjust the pH of the reaction solution to neutral (6.8-7.2). Activated carbon is added at 60-65℃. The motor 5 is started to drive the rotating rod 6 and the stirring rod 7 to rotate. Multiple sets of stirring rods 7 are used to stir the solution in reactor 1 for 30 minutes to ensure a complete reaction. The solution is filtered to remove pigments and impurities, and a crude lactulose solution is obtained for further processing.

[0024] like Figure 3 , Figure 6 , 7As shown, the guide pipe 4 is located in the tank cover 2, the feed pipe 3 is located in the reaction kettle 1, the feed pipe 3 is located at the end of the stirring rod 7 away from the rotating rod 6, the outer side of the end of the feed pipe 3 close to the tank cover 2 is fixedly connected with the connecting pipe 8, the connecting pipe 8 is provided with a slot on the outer side, the connecting pipe 8 is provided with a sliding block 9 on both sides, the sliding block 9 is fixedly connected with a plug rod 10 close to one side of the connecting pipe 8, and the plug rod 10 is inserted with the slot.

[0025] The guide pipe 4 is protected by the tank cover 2, and the clarified lactose solution is conveniently conveyed into the feed pipe 3 through the feed inlet. Since the feed pipe 3 is located at the end of the stirring rod 7 away from the rotating rod 6, the rotating rod 6 will not collide with the feed pipe 3 when it drives the stirring rod 7 to rotate, so that the feed pipe 3 is not damaged and the use is affected. The connecting pipe 8 is convenient for protecting the connecting end of the feed pipe 3 and the guide pipe 4, and the plug rod 10 is convenient for fixing the connecting pipe 8. The stability of the connecting pipe 8 is installed, the sliding block 9 drives the plug rod 10 to separate from the slot, and then the connecting pipe 8 and the feed pipe 3 are conveniently taken down for replacement, thereby improving the service life of the feed pipe 3 and improving the efficiency of conveying.

[0026] As shown in the figure, Figures 6 to 8 The support limiting assembly includes a guide block 11, a fixed block 12, a dispersion plate 13, a first telescopic rod 14, a connecting spring and a clamping structure. The guide block 11 is arranged on the outer side of the bottom end of the feed pipe 3, the guide block 11 is fixedly connected with the fixed block 12 at the bottom, the fixed block 12 is provided with a groove at the bottom, the inner wall of the groove is provided with the dispersion plate 13, the top of the dispersion plate 13 is fixedly connected with two first telescopic rods 14, the two first telescopic rods 14 are provided with connecting springs inside, the guide block 11 and the fixed block 12 are provided with installation grooves, and the installation grooves are provided with clamping structures. The guide block 11 and the fixed block 12 are fixedly connected with the inner wall of the reaction kettle 1 on one side, the bottom end of the feed pipe 3 extends through the guide block 11 to the installation groove on the top of the fixed block 12, one end of the connecting spring is fixedly connected with the inner wall of the top of the groove, and the other end is fixedly connected with the dispersion plate 13. The clamping structure is symmetrically arranged on both sides of the feed pipe 3, the side close to the feed pipe 3 of the guide block 11 is inclined, the radius of the dispersion plate 13 is greater than the radius of the feed pipe 3, and the clamping structure includes a clamping plate 15, a moving block 16 and a compression spring 17. The clamping block is slidably connected with the inner wall of the installation groove on both sides, the moving block 16 is fixedly connected with the clamping block on one side, the other side is in close contact with the outer side of the feed pipe 3, the compression spring 17 is fixedly connected with the inner wall of the installation groove on the side away from the feed pipe 3.

[0027] The bottom end of the feed pipe 3 is protected by the guide block 11 and the fixed block 12. Since one side of the guide block 11 is inclined, the material accumulation is prevented, the material stirring effect is improved, and the clamping structure is facilitated to install. The clamping plate 15 is attached to the outside of the bottom end of the feed pipe 3, and the bottom end of the feed pipe 3 is fixed. When the clarified lactose solution is transported or the solution is stirred by the stirring assembly in the reaction kettle 1, the clamping plate 15 and the moving block 16 are moved to absorb the vibration of the bottom end of the feed pipe 3, so that the compression spring 17 is compressed, the feed pipe 3 is affected, and the stability of the installation of the feed pipe 3 is improved. When the clarified lactose solution is transported by the feed pipe 3, the solution is transported to the dispersion plate 13, the first telescopic rod 14 is elongated, the connecting spring is stretched, the dispersion plate 13 is moved to the bottom of the fixed block 12, the bottom of the feed pipe 3 is shielded by the dispersion plate 13, the material is prevented from being sprayed from the pipe opening to directly impact the liquid surface to form splashing bubbles, and the material transportation effect is improved. Since the radius of the dispersion plate 13 is greater than the radius of the feed pipe 3, the impact force of the solution falling through the dispersion plate 13 is dispersed, and the solution flows into the bottom of the reaction kettle 1 along the dispersion plate 13, and the reaction is facilitated.

[0028] As shown in Figure 3 、 Figure 6 、 Figure 7 The support limiting assembly further includes a fixed plate 18, a support plate 19 and a second telescopic rod 20. The fixed plate 18 is arranged at the bottom of the connecting pipe 8, the middle part of the fixed plate 18 is fixedly connected with the feed pipe 3, the top of the fixed plate 18 is fixedly connected with the support plate 19 on both sides, the top end of the support plate 19 is fixedly connected with the bottom of the tank cover 2, the side close to the sliding block 9 of the support plate 19 is fixedly connected with the second telescopic rod 20, and one end of the second telescopic rod 20 is fixedly connected with the sliding block 9 away from the side of the insertion rod 10.

[0029] The fixed plate 18 is used to install the connecting pipe 8 and the support plate 19. The support plate 19 is arranged in an inclined manner, which improves the stability of the installation of the connecting pipe 8 and the guide pipe 4, prevents the connection end from shaking, and affects the use of the feed pipe 3. At the same time, the second telescopic rod 20 and the sliding block 9 are installed through the support plate 19, so that the sliding block 9 drives the second telescopic rod 20 to extend or retract when the sliding block 9 moves, and the sliding block 9 drives the insertion rod 10 to move, which facilitates the replacement of the connecting pipe 8 and the feed pipe 3.

[0030] As shown in Figures 3 to 5As shown, the feeding pipe 3 is provided with a vibration structure near the side of the connecting pipe 8, the vibration structure comprises a connecting plate, an electric telescopic rod 21, a moving structure, a movable plate 22, a limiting rod 23, a fixed rod 24 and a knocking block 25, the connecting plate is rotationally connected at the top end of the rotating rod 6, the bottom of the connecting plate is fixedly connected with the electric telescopic rod 21, one end of the electric telescopic rod 21 is provided with the movable plate 22, the movable plate 22 is screwedly connected on the rotating rod 6, the movable plate 22 is movably connected with the limiting rod 23 at both ends, the movable plate 22 is provided with the fixed rod 24 near the side of the feeding pipe 3, one end of the fixed rod 24 is fixedly connected with the knocking block 25, the inside of the movable plate 22 is provided with a moving groove, the moving groove is provided with the moving structure, one end of the electric telescopic rod 21 extends into the reaction kettle 1 through the bottom of the cover 2, one end of the limiting rod 23 is fixedly connected with the bottom of the cover 2, and the other end is rotationally connected with the top of the stirring rod 7, the moving structure comprises a moving rod 26, a round convex 27, a pushing block 28 and a fixed spring, the moving rod 26 is fixedly connected at the bottom of the electric telescopic rod 21, the bottom of the moving rod 26 is fixedly connected with the round convex 27, the side of the fixed block 12 near the round convex 27 is a slope, the bottom of the round convex 27 is provided with the pushing block 28, one side of the pushing block 28 is fixedly connected with the fixed rod 24, and the other side is fixedly connected with the fixed spring, and the side, away from the pushing block 28, of the fixed spring is fixedly connected with the inner wall of the moving groove.

[0031] The electric telescopic rod 21 is installed through the connecting plate, when the motor 5 rotates, the rotating rod 6, the stirring rod 7 and the movable plate 22 are driven to rotate, and the rotating rod 6 drives the one end of the limiting rod 23 to rotate along the top of the stirring rod 7, through the action of the limiting rod 23, the movable plate 22 can move along the rotating rod 6, when the movable plate 22 moves, the fixed rod 24 and the knocking block 25 are driven to move, when it is needed to knock the feeding pipe 3, the electric telescopic rod 21 is started to drive the moving rod 26 and the round convex 27 to move downwards, so that the round convex 27 moves into the moving groove, moves along the slope of the pushing block 28 to extrude the pushing block 28, the pushing block 28 drives the fixed rod 24 and the knocking block 25 to move to the outer wall of the feeding pipe 3, so that the fixed spring is stretched, through the movement of the electric telescopic rod 21, the moving rod 26 and the round convex 27, the pushing block 28 drives the fixed rod 24 and the knocking block 25 to knock the feeding pipe 3, so that the fixed rod 24 and the knocking block 25 driven by the movable plate 22 can move to different positions of the feeding pipe 3 to knock the outer side, so as to prevent the material in the feeding pipe 3 from being retained or deposited, and further improve the feeding efficiency of the feeding pipe 3, and facilitate use.

[0032] The present application provides a lactulose oral solution purification processing technology, comprising the following steps: Step one: food-grade lactose (purity ≥ 99%) is mixed with purified water at a ratio of 1:3, heated and stirred at 50-60°C until completely dissolved, filtered after adding activated carbon to adsorb impurities, and a clear lactose solution is obtained; Step two: the clear lactose solution is guided by the guide pipe 4 into the feeding pipe 3 through the feeding port, and is transferred into the reaction kettle 1 from the feeding pipe 3, is supported and fixed by the support limiting structure when the feeding pipe 3 is conveyed, is dispersed by the dispersion plate 13, flows down along the dispersion plate 13 after energy dispersion, is knocked by the vibration structure to remove the material adhered to the wall of the feeding pipe 3, is heated to 55-65 DEG C, and is added dropwise with sodium hydroxide to adjust the pH to 8.5-9.5, and is reacted for 1.5-2.5 hours (monitored by HPLC), and the reaction is stopped when the lactulose conversion rate reaches about 40%; the pH of the reaction solution in the reaction kettle 1 is adjusted to neutral (6.8-7.2) by adding hydrochloric acid, activated carbon is added at 60-65 DEG C, and the solution is stirred by the stirring assembly for 30 minutes, and then is filtered to remove impurities and pigments, so that a crude lactulose solution is obtained; Step three: the crude solution is guided through the "cation resin + anion resin" column to remove salt and small molecular impurities (monitoring the conductivity of the effluent liquid ≤5 μS / cm), and then is separated by a simulated moving bed chromatography to obtain a lactulose solution with a purity ≥90%; the pure lactulose solution is transferred into a double-effect vacuum concentrator, is concentrated at a low temperature (50-55 DEG C) under vacuum to a concentration of 60%-65%, is added with citric acid / sodium citrate to adjust the pH to 4.0-5.0, and is diluted with purified water to the specification of an oral solution (for example, 10 ml containing 5 g of lactulose); Step four: the prepared liquid medicine is filtered by a 0.22 μm filter membrane, is aseptically filled into an oral solution bottle, is subjected to 121 DEG C moist heat sterilization for 15 minutes, is cooled, is labeled and packaged after cooling, and is obtained as a finished product.

[0033] The working principle of the present application is as follows: Referring to Figures 1 to 9 When in use, the protective cover is opened to expose the feeding port, the clear lactose solution is guided by the guide pipe 4 through the feeding port, the clear lactose solution is transferred to the dispersion plate 13 from the feeding pipe 3, the first telescopic rod 14 is elongated, the connecting spring is stretched, the dispersion plate 13 is moved to the bottom of the fixed block 12, the impact force of the solution falling through the dispersion plate 13 is reduced due to the fact that the radius of the dispersion plate 13 is greater than the radius of the feeding pipe 3, the clear lactose solution flows into the reaction kettle 1 along the dispersion plate 13, the connecting pipe 8 and the guide pipe 4 are protected by the support plate 19 which is arranged in an inclined manner, the vibration of the bottom end of the feeding pipe 3 is absorbed by the movement of the clamping plate 15 and the moving block 16 when the clear lactose solution is conveyed, the compression spring 17 is compressed, the bottom end of the feeding pipe 3 is always stably inserted below the liquid level of the reaction kettle 1, so that the solution cannot carry a large amount of air into the kettle to form dense bubbles, the motor 5 is started to rotate the rotating rod 6 and the stirring rod 7, and the solution in the reaction kettle 1 is stirred.

[0034] When the motor 5 rotates, the rotating rod 6, the stirring rod 7 and the movable plate 22 are rotated, and the one end of the limiting rod 23 is rotated along the top of the stirring rod 7. Through the action of the limiting rod 23, the movable plate 22 can move along the rotating rod 6. When the movable plate 22 moves, the fixed rod 24 and the knocking block 25 are moved. Then the electric telescopic rod 21 is started to drive the moving rod 26 and the round convex 27 to move downward, so that the round convex 27 moves into the moving groove, moves the extrusion block 28 along the inclined surface of the pushing block 28, drives the fixed rod 24 and the knocking block 25 to move outward from the outer wall of the feeding pipe 3, so that the fixed spring is stretched. Through the movement of the electric telescopic rod 21, the moving rod 26 and the round convex 27, the pushing block 28 drives the fixed rod 24 and the knocking pipe to knock the feeding pipe 3, so that the movable plate 22 drives the fixed rod 24 and the knocking block 25 to move to different positions of the feeding pipe 3, and knocks the outer side, so that there is no material retention or deposition in the feeding pipe 3.

[0035] When the delivery of the clarified lactose solution is completed, the lactose solution is heated to 55-65℃, sodium hydroxide is added dropwise to adjust the pH to 8.5-9.5, and the reaction is kept for 1.5-2.5 hours (monitored by HPLC). When the lactulose conversion rate reaches about 40%, the reaction is stopped. Hydrochloric acid is added dropwise to the reaction kettle 1 to adjust the pH of the reaction solution to neutral (6.8-7.2), and activated carbon is added at 60-65℃. The rotating rod 6 and the stirring rod 7 are rotated by starting the motor 5, and the solution in the reaction kettle 1 is stirred for 30 minutes by the multiple stirring rods 7 to fully react. After filtration to remove pigments and impurities, a crude lactulose solution is obtained, and subsequent processing is continued.

[0036] The above examples are only used to illustrate the technical solutions of the present application, and not to limit it.

Claims

1. A galactose oral solution purification process using a reaction vessel (1), characterized by: The top of the reactor (1) is provided with a tank cover (2), the tank cover (2) is provided with a feeding assembly in the reactor (1); the feeding assembly includes a feeding port, a protective cover, a feeding pipe (3), a guide pipe (4) and a support limiting assembly, the top of the tank cover (2) is provided with a feeding port, the top of the feeding port is provided with a protective cover, the protective cover is hinged to the top of the tank cover (2), the bottom of the feeding port is provided with a guide pipe (4), one end of the guide pipe (4) is fixedly connected with the bottom of the tank cover (2), the bottom of the guide pipe (4) is fixedly connected with a feeding pipe (3), and both ends of the feeding pipe (3) are provided with a support limiting assembly.

2. The galacto-oligosaccharides oral solution purification process according to claim 1, characterized by the fact that: The tank cover (2) and the reactor (1) are provided with a stirring assembly, the stirring assembly includes a motor (5), a mounting seat, a rotating rod (6) and a stirring rod (7), the top of the tank cover (2) is fixedly connected with a mounting seat, the top of the mounting seat is fixedly connected with a motor (5), the output end of the motor (5) is fixedly connected with a rotating rod (6), one end of the rotating rod (6) extends into the reactor (1) through the mounting seat, and the outer side of the rotating rod (6) is fixedly connected with a plurality of stirring rods (7).

3. The galacto-oligosaccharides oral solution purification process according to claim 2, characterized by the fact that: The guide pipe (4) is located in the tank cover (2), the feeding pipe (3) is located in the reactor (1), the feeding pipe (3) is located at one end of the stirring rod (7) away from the rotating rod (6), the outer side of one end of the feeding pipe (3) close to the tank cover (2) is fixedly connected with a connecting pipe (8), the outer side of the connecting pipe (8) is provided with a slot, both sides of the connecting pipe (8) are provided with a sliding block (9), one side of the sliding block (9) close to the connecting pipe (8) is fixedly connected with a plug rod (10), and the plug rod (10) is inserted into the slot.

4. The galacto-oligosaccharides oral solution purification process according to claim 3, characterized by the fact that it comprises the following steps: The support limiting assembly includes a guide block (11), a fixed block (12), a dispersion plate (13), a first telescopic rod (14), a connecting spring and a clamping structure, the guide block (11) is arranged on the outer side of the bottom end of the feeding pipe (3), the bottom of the guide block (11) is fixedly connected with a fixed block (12), the bottom of the fixed block (12) is provided with a groove, the inner wall of the groove is provided with a dispersion plate (13), the top of the dispersion plate (13) is fixedly connected with two first telescopic rods (14), the inside of the two first telescopic rods (14) is provided with a connecting spring, and the guide block (11) and the fixed block (12) are provided with a mounting groove.

5. The galacto-oligosaccharides oral solution purification process according to claim 4, characterized by the fact that: The guide block (11) and the fixed block (12) are fixedly connected with the inner wall of the reactor (1) on one side, the bottom end of the feeding pipe (3) extends to the mounting groove in the top of the fixed block (12) through the guide block (11), one end of the connecting spring is fixedly connected with the top inner wall of the groove, the other end is fixedly connected with the dispersion plate (13), and the clamping structure is symmetrically arranged on both sides of the feeding pipe (3).

6. The galacto-oligosaccharides oral solution purification process according to claim 5, characterized by the fact that it comprises the following steps: The guide block (11) is inclined near the side of the feeding pipe (3), the radius of the dispersion plate (13) is greater than that of the feeding pipe (3), the clamping structure comprises a clamping plate (15), a moving block (16) and a compression spring (17), the two sides of the clamping block are slidably connected with the inner wall of the mounting groove, the moving block (16) is fixedly connected to one side of the clamping block, and the other side is attached to the outer side of the feeding pipe (3); the compression spring (17) is fixedly connected to the side of the moving block (16) away from the feeding pipe (3), and one end of the compression spring (17) is fixedly connected with the inner wall of the mounting groove.

7. The galacto-oligosaccharides oral solution purification process according to claim 6, characterized by the fact that it comprises the following steps: The support limiting assembly further comprises a fixed plate (18), a support plate (19) and a second telescopic rod (20), the fixed plate (18) is arranged at the bottom of the connecting pipe (8), the middle part of the fixed plate (18) is fixedly connected with the feeding pipe (3), the top of the fixed plate (18) is fixedly connected with the support plate (19) on both sides, the top of the support plate (19) is fixedly connected with the bottom of the tank cover (2), the side of the support plate (19) close to the sliding block (9) is fixedly connected with the second telescopic rod (20), and one end of the second telescopic rod (20) is fixedly connected with the sliding block (9) away from the side of the inserting rod (10).

8. The galacto-oligosaccharides oral solution purification process according to claim 7, characterized by the fact that it comprises the following steps: The feeding pipe (3) is provided with a vibration structure near the side of the connecting pipe (8), the vibration structure comprises a connecting plate, an electric telescopic rod (21), a moving structure, a movable plate (22), a limiting rod (23), a fixed rod (24) and a knocking block (25), the connecting plate is rotatably connected to the top of the rotating rod (6), the bottom of the connecting plate is fixedly connected with the electric telescopic rod (21), one end of the electric telescopic rod (21) is provided with the movable plate (22), the movable plate (22) is threadedly connected to the rotating rod (6), the movable plate (22) is movably connected with the limiting rod (23) at both ends, the side of the movable plate (22) close to the feeding pipe (3) is provided with the fixed rod (24), one end of the fixed rod (24) is fixedly connected with the knocking block (25), and the movable plate (22) is internally provided with a moving groove, and the moving structure is arranged in the moving groove.

9. The galacto-oligosaccharides oral solution purification process according to claim 8, characterized by the fact that it comprises the following steps: One end of the electric telescopic rod (21) extends into the reaction kettle (1) through the bottom of the tank cover (2), one end of the limiting rod (23) is fixedly connected with the bottom of the tank cover (2), and the other end is rotatably connected with the top of the stirring rod (7), the moving structure comprises a moving rod (26), a round convex (27), a pushing block (28) and a fixed spring, the moving rod (26) is fixedly connected to the bottom of the electric telescopic rod (21), the bottom of the moving rod (26) is fixedly connected with the round convex (27), the side of the fixed block (12) close to the round convex (27) is inclined, the bottom of the round convex (27) is provided with the pushing block (28), one side of the pushing block (28) is fixedly connected with the fixed rod (24), the other side is fixedly connected with the fixed spring, and the side of the fixed spring away from the pushing block (28) is fixedly connected with the inner wall of the moving groove.

10. The galacto-oligosaccharides oral solution purification process according to claim 9, characterized in that, The method comprises the following steps: Step one: mix food-grade lactose (purity ≥ 99%) with purified water at a ratio of 1:3, heat and stir at 50-60°C until completely dissolved, add activated carbon to adsorb impurities, and filter to obtain a clear lactose solution; Step two: pass the clear lactose solution through the feed inlet into the guide pipe (4) and then into the feed pipe (3), and then into the reaction kettle (1) for stirring. When the feed pipe (3) is conveying, it is supported and fixed by the support limiting structure, and after the energy is dispersed by the dispersion plate (13), it flows down along the dispersion plate (13), and then is knocked by the vibration structure to remove the material adhering to the wall of the feed pipe (3). Then, the lactose solution is heated to 55-65°C, sodium hydroxide is added to adjust the pH to 8.5-9.5, and the reaction is kept for 1.5-2.5 hours (monitored by HPLC). When the lactulose conversion rate reaches about 40%, the reaction is stopped. Add hydrochloric acid to the reaction kettle (1) to adjust the pH of the reaction solution to neutral (6.8-7.2), add activated carbon at 60-65°C, stir for 30 minutes by the stirring assembly, filter to remove pigments and impurities, and obtain a crude lactulose solution; Step three: pass the crude solution through a "cation resin + anion resin" column to remove salts and small molecular impurities (monitor the conductivity of the effluent ≤5 μS / cm), and then use simulated moving bed chromatography to separate and obtain a lactulose solution with a purity of ≥90%. Transfer the pure lactulose solution to a double-effect vacuum concentrator, concentrate it at a low temperature (50-55°C) under vacuum to a concentration of 60%-65%, adjust the pH to 4.0-5.0 with citric acid / sodium citrate, and dilute it to the specifications of an oral solution (e.g., 10 ml containing 5 g of lactulose) with purified water. Step four: filter the prepared drug solution with a 0.22 μm filter membrane, aseptically fill it into an oral solution bottle, sterilize it at 121°C for 15 minutes, cool it, label and package it, and the finished product is obtained.

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