CN114671773A - High-yield cyclic acid synthesis method - Google Patents
High-yield cyclic acid synthesis method Download PDFInfo
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- CN114671773A CN114671773A CN202210488611.XA CN202210488611A CN114671773A CN 114671773 A CN114671773 A CN 114671773A CN 202210488611 A CN202210488611 A CN 202210488611A CN 114671773 A CN114671773 A CN 114671773A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/16—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions not involving the amino or carboxyl groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
- C07C227/42—Crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of cyclic acid synthesis, in particular to a high-yield cyclic acid synthesis method, aiming at the defects that the existing reaction kettle is lack of a special catalytic hydrogenation structure, the reaction time is long after hydrogen is added, and the hydrogenation effect is poor, the following scheme is provided, namely, a sulfuric acid solution with the mass fraction of 5-7%, a platinum catalyst and pretreated aminomethylbenzoic acid are added into the reaction kettle body from a feed inlet of a synthesis mechanism according to the weight ratio of 2:1:6, the feed inlet of the reaction kettle body is closed, and a device is started; the electric bar heats this internal solution of reation kettle after the hot plate circular telegram, treats that the reaction liquid temperature reaches the preset temperature after, and the motor drives the axostylus axostyle and rotates, and the stirring subassembly mixes the stirring to the reaction liquid.
Description
Technical Field
The invention relates to the technical field of cyclic acid synthesis, in particular to a high-yield cyclic acid synthesis method.
Background
Tranexamic acid, also known as tranexamic acid, has a molecular formula of C8H15NO2, has a chemical name of trans-4-aminomethyl cyclohexanecarboxylic acid, is white crystalline powder, odorless, slightly odorous, easily soluble in water, and hardly soluble in ethanol, acetone, trichloromethane or diethyl ether.
Tranexamic acid has extremely wide effects in the aspect of medical pharmacy, and can safely and reliably reduce the death rate of patients with traumatic hemorrhage; the possibility of progressive bleeding of a craniocerebral patient can be reduced; can significantly reduce the blood loss of women with excessive menstrual blood; the postpartum hemorrhage amount can be obviously reduced; can reduce the risk of postoperative blood transfusion and reduce the amount of bleeding during and after operation, can be used for the adjuvant treatment before and after operation of hemophilia patients with deficiency of factor VIII, and also has the effects of blackening and removing spots.
Tranexamic acid needs to be subjected to catalytic hydrogenation on a semi-finished product in a production and processing process to obtain a required hydrogenation product, the process is usually carried out in a reaction kettle, but the reaction time is long after hydrogen is added due to the fact that the existing reaction kettle is lack of a special catalytic hydrogenation structure, and the hydrogenation effect is poor.
Disclosure of Invention
The invention provides a high-yield cyclic acid synthesis method, which comprises the following steps:
a high-yield cyclic acid synthesis method comprises the following steps:
the method comprises the following steps: mixing aminomethylbenzoic acid and pure water according to a weight ratio of 1:5, slowly adding concentrated sulfuric acid under stirring, heating to a preset temperature, dissolving the aminomethylbenzoic acid, cooling for crystallization, filtering to obtain pretreated aminomethylbenzoic acid, adding a sulfuric acid solution with a mass fraction of 5-7%, a platinum catalyst and the pretreated aminomethylbenzoic acid into a reaction kettle body according to a weight ratio of 2:1:6, closing a feed inlet of the reaction kettle body, and starting a device;
step two: after the heating plate is electrified, the electric heating rod heats the solution in the reaction kettle body, after the temperature of the reaction solution reaches a preset temperature, the motor drives the shaft lever to rotate, and the stirring assembly mixes and stirs the reaction solution;
in the concrete stirring process, along with the rotation of the hexagonal shaft seat, the stirring rod is subjected to the reverse acting force of the internal reaction liquid and the driving force of the rotation of the shaft lever, the spring base (can shake to drive the stirring rod to vibrate, the contact effect of the stirring rod and the reaction liquid can be increased in the vibrating process, and the overall stirring and mixing effect of the stirring assembly is improved;
step three: conveying hydrogen from an air inlet pipe to the inside of the reaction kettle body, closing a valve of the air inlet pipe after conveying quantitative hydrogen to prepare a hydrogenation product, then adding calcium hydroxide in a weight ratio of the hydrogenation product, and continuing reaction treatment;
during the hydrogen conveying process, hydrogen enters the gas return seat and is sprayed out of the gas holes to directly act on reaction solution, the hydrogen forms bubbles in the reaction solution, the contact effect between the gas and the reaction solution is increased, the catalytic hydrogenation effect is improved, the miniature gas pump works by utilizing the gas suction pipe and the gas inlet groove to suck gas inside the reaction kettle body, the gas enters the gas return seat through the gas pipe and is sprayed out of the gas holes, the contact effect between the hydrogen and the reaction solution is improved in a circulating mode, after the reaction is finished, the gas in the reaction kettle is discharged by opening the gas exhaust pipe valve, and then the reacted solution is discharged to perform subsequent transposition reaction;
step four: during the catalytic hydrogenation reaction, hydrogen is introduced into the reaction kettle, the internal pressure is increased, the catalytic hydrogenation reaction effect is reduced, the pressure regulating assembly can change the internal pressure of the reaction kettle body, after the hydrogen is introduced, the air flow control valve can perform exhaust operation to discharge air in the air bag outwards, the air bag contracts in the air cylinder, the bottom plate is pushed to move upwards, the return spring is assisted to push the bottom plate to reset under the action of the reverse force after elastic deformation, and then the high-yield cyclic acid synthesis is completed;
the synthesis mechanism comprises a reaction kettle body, wherein an air return component is arranged inside the reaction kettle body and comprises an air return seat and an air ring, the outer wall of one side of the air return seat is fixedly connected with the inner wall of the reaction kettle body, an exhaust plate is arranged on the air return seat, a plurality of air holes are formed in the exhaust plate in a circumferential equidistant mode, the air ring is located above the air return seat, a plurality of circular holes in the circumferential equidistant mode are formed in the air ring, an air suction pipe is fixedly connected to the inner wall of each circular hole, an air inlet groove is fixedly connected to the other end of each air suction pipe, two air conveying pipes are fixedly connected between the air ring and the air return seat, and a miniature air pump is arranged on each air conveying pipe.
Preferably, fixedly connected with intake pipe on the gas return seat, the other end of intake pipe passes reation kettle body and external trachea fixed connection, and has seted up the round hole on the reation kettle body, and the round hole is located the top of gas ring, the inner wall fixedly connected with blast pipe of round hole.
Preferably, the three equidistant support of circumference of outer wall fixedly connected with of reation kettle body, equal fixedly connected with supporting leg on the support, and the top of reation kettle body is provided with the top cap, and the below of reation kettle body is provided with end box, has seted up the small opening on the end box, and the inner wall fixedly connected with of small opening arranges the material pipe.
Preferably, the inside of reation kettle body is provided with accuse temperature subassembly, and accuse temperature subassembly is located the below of return air seat, and accuse temperature subassembly includes hot plate and spiral pipe that adjusts the temperature, fixed connection between the inner wall of hot plate and reation kettle body is provided with the electric bar of a plurality of circumference equidistance on the hot plate, and has seted up two round holes on the reation kettle body, and the inner wall of two round holes is fixedly connected with inlet tube and outlet pipe respectively, inlet tube and outlet pipe respectively with spiral pipe's both ends fixed connection that adjusts the temperature.
Preferably, the upside outer wall fixedly connected with frame of top cap, the inner wall fixedly connected with motor of frame, the output of motor has the axostylus axostyle through the coupling joint, and the other end of axostylus axostyle passes the top cap, and the outside of axostylus axostyle is provided with the stirring subassembly, has seted up the feed inlet on the top cap.
Preferably, the stirring subassembly includes hexagonal axle seat and a plurality of branch, has seted up the hexagonal recess on the hexagonal axle seat, fixed connection between the inner wall of hexagonal recess and the outer wall of axostylus axostyle, and fixed connection between a plurality of branches and the hexagonal axle seat, a plurality of branches are circumference equidistance and distribute.
Preferably, it is a plurality of all seted up the round hole of three equidistance on the branch, the equal fixedly connected with spring base of the inner wall of three round hole, and the equal fixedly connected with puddler in spring base's top.
Preferably, two symmetrical air overflow holes are formed in the top cover, and pressure regulating assemblies are arranged inside the two air overflow holes.
Preferably, the pressure regulating subassembly includes inflator and gasbag, fixed connection between the outer wall of inflator and the inner wall of gas discharge hole, and the gasbag is located the inside of inflator, and the top fixedly connected with air current control valve of inflator is connected through the nozzle stub between air current control valve and the gasbag.
Preferably, the inside of gasbag is provided with and bulldozes the bottom plate, and the top inner wall fixedly connected with of gasbag attaches the seat in, and the downside outer wall fixedly connected with reset spring of interior attached seat, reset spring's the other end with bulldoze between the bottom plate fixed connection.
The beneficial effects of the invention are as follows:
1. according to the reaction kettle, the reaction kettle body, the air return seat, the air ring, the exhaust plate, the air hole, the air suction groove, the air inlet groove, the air delivery pipe and the micro air pump are arranged, the device can directly convey input hydrogen into reaction liquid by utilizing the air return assembly, so that bubbles are generated to increase the contact effect between the hydrogen and the reaction liquid, meanwhile, in the reaction process, the micro air pump is used for repeatedly conveying the gas in the reaction kettle body into the reaction liquid, and the reaction effect between the hydrogen and the internal reaction liquid after the hydrogen is conveyed into the reaction kettle body is further improved; during the hydrogen conveying process, hydrogen enters the gas return seat and is sprayed out of the gas holes to directly act on the reaction solution, and the hydrogen forms bubbles in the reaction solution, so that the contact effect between the gas and the reaction solution is further increased, and the catalytic hydrogenation effect is improved.
2. According to the invention, through the arranged temperature control assembly, the electric heating rod heats the solution in the reaction kettle body after the heating plate is electrified, so that the temperature of the reaction solution reaches the preset temperature to meet the conditions required by the reaction, the temperature regulating liquid (water) is introduced into the spiral temperature regulating pipe, the temperature of the reaction solution exceeds the preset value along with the lengthening of the reaction time or the overheating of the heating plate, the water is input from the water inlet pipe, the water outlet pipe is sent out, the temperature of the reaction solution is reduced, and the integral process of the reaction is prevented from being influenced by the overhigh temperature.
3. According to the invention, the stirring component is arranged, the motor drives the shaft lever to rotate, and the stirring component is used for mixing and stirring reaction liquid; in the stirring process, along with the rotation of hexagonal axle bed, the puddler receives the counter action power and the axostylus axostyle pivoted drive power of inside reaction liquid, and spring base can take place to rock and drive the puddler vibration, and the puddler can increase the contact effect with the reaction liquid among the vibration process to improve the whole stirring mixed effect of stirring subassembly.
4. According to the invention, through the arranged pressure regulating assembly, during the catalytic hydrogenation reaction, as hydrogen is introduced into the reaction kettle, the internal pressure of the reaction kettle is increased, so that the catalytic hydrogenation reaction effect is reduced (the solubility of the hydrogen is reduced after the air pressure is increased), the pressure regulating assembly can change the internal pressure of the reaction kettle body, after the hydrogen is introduced, the air flow control valve can perform exhaust operation to discharge the gas in the air bag outwards (the air bag is filled with the external air to expand the air bag initially), the air bag contracts in the air cylinder, the bottom plate is pushed to move upwards, and the reset spring is assisted to push the bottom plate to reset under the reverse acting force after elastic deformation.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a high-yield cyclic acid synthesis method according to the present invention;
FIG. 2 is a schematic structural diagram of a gas return module of a high-yield cyclic acid synthesis method according to the present invention;
FIG. 3 is a schematic diagram of a gas ring structure of a high-yield cyclic acid synthesis method according to the present invention;
FIG. 4 is a schematic diagram of a temperature control module of the high-yield cyclic acid synthesis method according to the present invention;
FIG. 5 is a schematic view of a cross-sectional structure of a reaction vessel body of a high-yield cyclic acid synthesis method according to the present invention;
FIG. 6 is a schematic structural diagram of a stirring assembly of the high-yield cyclic acid synthesis method of the present invention;
FIG. 7 is a schematic diagram of a top cover structure of a high yield cyclic acid synthesis method according to the present invention;
FIG. 8 is a schematic structural diagram of a pressure regulating assembly of the high-yield cyclic acid synthesis method provided by the present invention.
In the figure: 1. a reaction kettle body; 2. a gas return seat; 3. a gas ring; 4. an exhaust plate; 5. air holes; 6. an air intake duct; 7. an air inlet groove; 8. a gas delivery pipe; 9. a micro air pump; 10. an air inlet pipe; 11. an exhaust pipe; 12. a support; 13. supporting legs; 14. a top cover; 15. a bottom case; 16. a discharge pipe; 17. heating plates; 18. a spiral temperature regulating tube; 19. an electric heating rod; 20. a water inlet pipe; 21. a water outlet pipe; 22. a frame; 23. an electric motor; 24. a shaft lever; 25. a feed inlet; 26. a hexagonal shaft seat; 27. a strut; 28. a spring mount; 29. a stirring rod; 30. an air overflow hole; 31. an air cylinder; 32. an air bag; 33. an airflow control valve; 34. pushing and pressing the bottom plate; 35. an internal attachment seat; 36. a return spring.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
A high-yield cyclic acid synthesis method comprises the following steps:
the method comprises the following steps: mixing aminomethylbenzoic acid and pure water according to a weight ratio of 1:5, slowly adding concentrated sulfuric acid under stirring, heating to a preset temperature, dissolving the aminomethylbenzoic acid, cooling for crystallization, filtering to obtain pretreated aminomethylbenzoic acid, then adding a sulfuric acid solution with a mass fraction of 5-7%, a platinum catalyst and the pretreated aminomethylbenzoic acid into a reaction kettle body 1 from a feed port 25 of a synthesis mechanism according to a weight ratio of 2:1:6, closing the feed port 25 of the reaction kettle body 1, and starting a device;
step two: after the heating plate 17 is electrified, the electric heating rod 19 heats the solution in the reaction kettle body 1, after the temperature of the reaction solution reaches the preset temperature, the motor 23 drives the shaft lever 24 to rotate, and the stirring assembly mixes and stirs the reaction solution;
in the concrete stirring process, along with the rotation of the hexagonal shaft seat 26, the stirring rod 29 is subjected to the reverse acting force of the internal reaction liquid and the driving force of the rotation of the shaft lever 24, the spring base (28 can shake to drive the stirring rod 29 to vibrate, the contact effect of the stirring rod 29 and the reaction liquid can be increased in the vibrating process, and the overall stirring and mixing effect of the stirring assembly is improved;
step three: conveying hydrogen from an air inlet pipe 10 to the interior of the reaction kettle body 1, closing a valve of the air inlet pipe 10 after conveying quantitative hydrogen to prepare a hydrogenation product, then adding calcium hydroxide with the weight ratio of the hydrogenation product being 1:6, and continuing reaction treatment;
during the hydrogen conveying process, hydrogen enters the gas return seat 2 and is sprayed out of the gas holes 5 to directly act on reaction solution, the hydrogen forms bubbles in the reaction solution, the contact effect between the gas and the reaction solution is increased, the catalytic hydrogenation effect is improved, the miniature air pump 9 works to utilize the air suction pipe 6 and the air inlet groove 7 to perform air suction operation on the interior of the reaction kettle body 1, the hydrogen enters the gas return seat 2 through the air conveying pipe 8 and is sprayed out of the gas holes 5, the contact effect of the hydrogen and the reaction solution is circularly improved, after the reaction is finished, the valve of the exhaust pipe 11 is opened to exhaust the gas in the reaction kettle, and then the solution after the reaction is exhausted to perform subsequent transposition reaction;
step four: during the catalytic hydrogenation reaction, hydrogen is introduced into the reaction kettle, the internal pressure is increased, the catalytic hydrogenation reaction effect is reduced, the pressure regulating assembly can change the internal pressure of the reaction kettle body 1, after the hydrogen is introduced, the air flow control valve 33 can perform exhaust operation to discharge the air in the air bag 32 outwards, the air bag 32 contracts the volume in the air cylinder 31 to push the bottom plate 34 to move upwards, the return spring 36 is assisted by the reverse acting force after elastic deformation to push the bottom plate 36 to return, and then the high-yield cyclic acid synthesis is completed; as shown in fig. 1, fig. 2 and fig. 3, the reactor comprises a reactor body 1, a gas return assembly is arranged in the reactor body 1, and the gas return assembly comprises a gas return seat 2 and a gas ring 3, one side outer wall of the gas return seat 2 is connected with the inner wall of the reactor body 1 through a bolt, the gas return seat 2 is provided with an exhaust plate 4, the exhaust plate 4 is provided with a plurality of gas holes 5 at equal intervals on the circumference, the gas ring 3 is positioned above the gas return seat 2, the gas ring 3 is connected with the inner wall of the reactor body 1 through a bolt, the gas ring 3 is provided with a plurality of round holes at equal intervals on the circumference, the inner wall of the round hole is connected with a gas suction pipe 6 through a bolt, the other end of the gas suction pipe 6 is connected with a gas inlet slot 7 through a bolt, two gas conveying pipes 8 are connected between the gas ring 3 and the gas return seat 2 through a bolt, and the two gas conveying pipes 8 are provided with a micro gas pump 9, during the hydrogen conveying process, hydrogen enters the gas return seat 2 and is ejected from the gas holes 5, the hydrogen directly acts on the reaction solution to form bubbles in the reaction solution, so that the contact effect between the gas and the reaction solution is further increased, and the catalytic hydrogenation effect is improved.
Further, as shown in fig. 2, an air inlet pipe 10 is connected to the air return seat 2 through a bolt, the other end of the air inlet pipe 10 penetrates through the reaction kettle body 1 and is connected with an external air pipe through a bolt, a circular hole is formed in the reaction kettle body 1 and is located above the air ring 3, and the inner wall of the circular hole is connected with an exhaust pipe 11 through a bolt; the outer wall of reation kettle body 1 has three support 12 that are circumference equidistance through bolted connection, all has supporting leg 13 through bolted connection on the support 12, and reation kettle body 1's top is provided with top cap 14, and reation kettle body 1's below is provided with end box 15, has seted up the small opening on the end box 15, and there is row material pipe 16 inner wall of small opening through bolted connection.
Further, as shown in fig. 1 and 4, a temperature control assembly is disposed inside the reaction kettle body 1, the temperature control assembly is located below the gas return seat 2, the temperature control assembly includes a heating plate 17 and a spiral temperature adjusting pipe 18, the heating plate 17 is connected to the inner wall of the reaction kettle body 1 by a bolt, a plurality of electric heating rods 19 with equal circumferential distances are disposed on the heating plate 17, two circular holes are disposed on the reaction kettle body 1, the inner walls of the two circular holes are respectively connected to a water inlet pipe 20 and a water outlet pipe 21 by bolts, the water inlet pipe 20 and the water outlet pipe 21 are respectively connected to two ends of the spiral temperature adjusting pipe 18 by bolts, the electric heating rods 19 heat the solution in the reaction kettle body 1 after the heating plate 17 is energized, so that the temperature of the reaction solution reaches a preset temperature, the condition required by the reaction is satisfied, the temperature adjusting liquid (water) is introduced into the spiral temperature adjusting pipe 18, and the heating plate 17 is excessively heated along with the lengthening of the reaction time or the heating plate 17, when the temperature of the reaction liquid exceeds the preset value, water is input from the water inlet pipe 20, the water outlet pipe 21 is sent out, the reaction liquid is cooled, and the whole process of the reaction is prevented from being influenced by overhigh temperature.
Furthermore, as shown in fig. 5 and 6, the outer wall of the upper side of the top cover 14 is connected with a frame 22 through a bolt, the inner wall of the frame 22 is connected with a motor 23 through a bolt, the output end of the motor 23 is connected with a shaft rod 24 through a coupler, the other end of the shaft rod 24 penetrates through the top cover 14, a stirring assembly is arranged outside the shaft rod 24, and the top cover 14 is provided with a feeding hole 25; the stirring assembly comprises a hexagonal shaft seat 26 and a plurality of struts 27, a hexagonal groove is formed in the hexagonal shaft seat 26, the inner wall of the hexagonal groove is connected with the outer wall of the shaft rod 24 through a bolt, the struts 27 are connected with the hexagonal shaft seat 26 through bolts, and the struts 27 are distributed circumferentially at equal intervals; all seted up the round hole of three equidistance on a plurality of branches 27, the inner wall of three round hole all has spring base 28 through bolted connection, and spring base 28's top all has puddler 29 through bolted connection, the stirring in-process, along with hexagonal axle bed 26's rotation, puddler 29 receives the counter action power and the 24 pivoted drive powers of axostylus axostyle of inside reaction liquid, spring base 28 can take place to rock and drive puddler 29 vibration, the contact effect with reaction liquid can be increased to stirring rod 29 among the vibration process, thereby improve the whole stirring mixed effect of stirring subassembly.
Furthermore, as shown in fig. 7 and 8, two symmetrical air holes 30 are formed in the top cover 14, and pressure regulating assemblies are disposed inside the two air holes 30; the pressure regulating assembly comprises an air cylinder 31 and an air bag 32, the outer wall of the air cylinder 31 is connected with the inner wall of the air overflow hole 30 through a bolt, the air bag 32 is positioned in the air cylinder 31, the top of the air cylinder 31 is connected with an airflow control valve 33 through a bolt, and the airflow control valve 33 is connected with the air bag 32 through a short pipe; the inner part of the air bag 32 is provided with a pushing and pressing bottom plate 34, the inner wall of the top part of the air bag 32 is connected with an internal attached seat 35 through a bolt, the outer wall of the lower side of the internal attached seat 35 is connected with a return spring 36 through a bolt, the other end of the return spring 36 is connected with the pushing and pressing bottom plate 34 through a bolt, during the catalytic hydrogenation reaction, because hydrogen is introduced into the reaction kettle, the pressure inside the reaction kettle body 1 can be increased, so that the effect of catalytic hydrogenation reaction can be reduced (the solubility of hydrogen is reduced after the air pressure is increased), the pressure regulating assembly can change the pressure inside the reaction kettle body 1, when the hydrogen gas is introduced, the gas flow control valve 33 performs a gas exhaust operation to exhaust the gas in the air bag 32 (initially, the air bag 32 is inflated by the external air), the air bag 32 contracts in volume in the gas cylinder 31 to push the bottom plate 34 to move upward, and the return spring 36 receives a reverse acting force after elastic deformation to assist in pushing the bottom plate 34 to return.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (10)
1. A high-yield cyclic acid synthesis method is characterized by comprising the following steps:
the method comprises the following steps: mixing aminomethylbenzoic acid and pure water according to a weight ratio of 1:5, slowly adding concentrated sulfuric acid under stirring, heating to a preset temperature, dissolving the aminomethylbenzoic acid, cooling for crystallization, filtering to obtain pretreated aminomethylbenzoic acid, then adding a sulfuric acid solution with a mass fraction of 5-7%, a platinum catalyst and the pretreated aminomethylbenzoic acid into a reaction kettle body (1) from a feed inlet (25) of a synthesis mechanism according to a weight ratio of 2:1:6, closing the feed inlet (25) of the reaction kettle body (1), and starting a device;
step two: after the heating plate (17) is electrified, the electric heating rod (19) heats the solution in the reaction kettle body (1), after the temperature of the reaction liquid reaches a preset temperature, the motor (23) drives the shaft lever (24) to rotate, and the stirring assembly mixes and stirs the reaction liquid;
in the concrete stirring process, along with the rotation of the hexagonal shaft seat (26), the stirring rod (29) receives the reverse acting force of the internal reaction liquid and the driving force of the rotation of the shaft lever (24), the spring base (28) can shake to drive the stirring rod (29) to vibrate, the stirring rod (29) can increase the contact effect with the reaction liquid in the vibration process, and the overall stirring and mixing effect of the stirring assembly is improved;
step three: conveying hydrogen from an air inlet pipe (10) to the interior of the reaction kettle body (1), closing a valve of the air inlet pipe (10) after conveying quantitative hydrogen to prepare a hydrogenation product, then adding calcium hydroxide with the weight ratio of the hydrogenation product being 1:6, and continuing reaction treatment;
during the hydrogen conveying process, hydrogen enters the gas return seat (2) and is sprayed out of the gas holes (5) to directly act on reaction solution, the hydrogen forms bubbles in the reaction solution, the contact effect between the gas and the reaction solution is increased, the catalytic hydrogenation effect is improved, the miniature gas pump (9) works by utilizing the gas suction pipe (6) and the gas inlet groove (7) to suck gas into the reaction kettle body (1), the gas enters the gas return seat (2) through the gas conveying pipe (8), the hydrogen is sprayed out of the gas holes (5), the contact effect between the hydrogen and the reaction solution is circularly improved, after the reaction is finished, the valve of the exhaust pipe (11) is opened to exhaust the gas in the reaction kettle, and then the reacted solution is exhausted to perform subsequent transposition reaction;
step four: during the catalytic hydrogenation reaction, inside the reation kettle lets in hydrogen, inside pressure can increase, catalytic hydrogenation reaction's effect can reduce, and the pressure regulating subassembly can change the inside pressure of reation kettle body (1), after hydrogen lets in, air current control valve (33) can carry out the exhaust operation, outwards discharge the gas in gasbag (32), gasbag (32) shrink volume in inflator (31), bulldoze bottom plate (34) rebound, reset spring (36) receive the reverse effort behind the elastic deformation to assist and bulldoze bottom plate (36) and reset, and then accomplish high yield's cyclic acid synthesis.
2. The method for synthesizing the high-yield naphthenic acid according to claim 1, wherein the synthesis mechanism comprises a reaction kettle body (1), a gas return assembly is arranged inside the reaction kettle body (1), the gas return assembly comprises a gas return seat (2) and a gas ring (3), the outer wall of one side of the gas return seat (2) is fixedly connected with the inner wall of the reaction kettle body (1), an exhaust plate (4) is arranged on the gas return seat (2), a plurality of gas holes (5) are formed in the exhaust plate (4) at equal intervals on the circumference, the gas ring (3) is positioned above the gas return seat (2), the gas ring (3) is fixedly connected with the inner wall of the reaction kettle body (1), a plurality of circular holes at equal intervals on the circumference are formed in the gas ring (3), a gas suction pipe (6) is fixedly connected with the inner wall of the circular hole, and a gas inlet groove (7) is fixedly connected with the other end of the gas suction pipe (6), two air pipes (8) are fixedly connected between the air ring (3) and the air return seat (2), and a micro air pump (9) is arranged on each of the two air pipes (8).
3. The method for synthesizing the cyclic acid with high yield according to claim 2, wherein the gas inlet pipe (10) is fixedly connected to the gas return base (2), the other end of the gas inlet pipe (10) penetrates through the reaction kettle body (1) to be fixedly connected with an external gas pipe, a circular hole is formed in the reaction kettle body (1), the circular hole is located above the gas ring (3), and an exhaust pipe (11) is fixedly connected to the inner wall of the circular hole.
4. The method for synthesizing the high-yield cyclic acid according to claim 3, wherein three supports (12) with equal intervals in the circumference are fixedly connected to the outer wall of the reaction kettle body (1), the supports (12) are all fixedly connected with supporting legs (13), a top cover (14) is arranged above the reaction kettle body (1), a bottom box (15) is arranged below the reaction kettle body (1), a leakage hole is formed in the bottom box (15), and a discharge pipe (16) is fixedly connected to the inner wall of the leakage hole.
5. The method for synthesizing the high-yield naphthenic acid according to claim 4, wherein a temperature control assembly is arranged inside the reaction kettle body (1), the temperature control assembly is located below the gas return seat (2), the temperature control assembly comprises a heating plate (17) and a spiral temperature adjusting pipe (18), the heating plate (17) is fixedly connected with the inner wall of the reaction kettle body (1), a plurality of electric heating rods (19) with equal circumferential distances are arranged on the heating plate (17), two round holes are formed in the reaction kettle body (1), the inner walls of the two round holes are respectively and fixedly connected with a water inlet pipe (20) and a water outlet pipe (21), and the water inlet pipe (20) and the water outlet pipe (21) are respectively and fixedly connected with two ends of the spiral temperature adjusting pipe (18).
6. The method for synthesizing the high-yield naphthenic acid according to claim 2, wherein a rack (22) is fixedly connected to the outer wall of the upper side of the top cover (14), a motor (23) is fixedly connected to the inner wall of the rack (22), the output end of the motor (23) is connected with a shaft rod (24) through a coupling, the other end of the shaft rod (24) penetrates through the top cover (14), a stirring assembly is arranged outside the shaft rod (24), and a feeding hole (25) is formed in the top cover (14).
7. The method for synthesizing high-yield naphthenic acid according to claim 6, wherein the stirring assembly comprises a hexagonal shaft seat (26) and a plurality of struts (27), the hexagonal shaft seat (26) is provided with a hexagonal groove, the inner wall of the hexagonal groove is fixedly connected with the outer wall of the shaft rod (24), the plurality of struts (27) are fixedly connected with the hexagonal shaft seat (26), and the plurality of struts (27) are circumferentially distributed at equal intervals.
8. The method for synthesizing the cyclic acid with high yield according to claim 7, wherein three circular holes with equal distance are formed on the plurality of the supporting rods (27), the inner walls of the three circular holes are fixedly connected with spring bases (28), and the top ends of the spring bases (28) are fixedly connected with stirring rods (29).
9. The method for synthesizing the cyclic acid with high yield according to claim 8, wherein the top cover (14) is provided with two symmetrical air overflow holes (30), and pressure regulating components are arranged inside the two air overflow holes (30).
10. The method for synthesizing the cyclic acid with high yield according to claim 9, wherein the pressure regulating assembly comprises a gas cylinder (31) and a gas bag (32), the outer wall of the gas cylinder (31) is fixedly connected with the inner wall of the gas overflow hole (30), the gas bag (32) is positioned inside the gas cylinder (31), the top of the gas cylinder (31) is fixedly connected with a gas flow control valve (33), and the gas flow control valve (33) is connected with the gas bag (32) through a short pipe; the inner part of the air bag (32) is provided with a pushing and pressing bottom plate (34), an inner attached seat (35) is fixedly connected to the inner wall of the top of the air bag (32), a return spring (36) is fixedly connected to the outer wall of the lower side of the inner attached seat (35), and the other end of the return spring (36) is fixedly connected with the pushing and pressing bottom plate (34).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116393019A (en) * | 2023-05-29 | 2023-07-07 | 青州金昊新材料有限公司 | Circulation cooling type liquid chemical raw material mixing equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116393019A (en) * | 2023-05-29 | 2023-07-07 | 青州金昊新材料有限公司 | Circulation cooling type liquid chemical raw material mixing equipment |
| CN116393019B (en) * | 2023-05-29 | 2023-08-15 | 青州金昊新材料有限公司 | Circulation cooling type liquid chemical raw material mixing equipment |
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