Method for synthesizing amyl nonanal based on n-heptanal condensation

Abstract

The invention relates to the technical field of organic synthesis, and particularly discloses a pentylnonanal synthesis method based on n-heptanal condensation, which comprises the following steps: S1, early-stage preparation: raw material preparation, catalyst selection, reaction equipment preparation and safety preparation; s2, reaction operation: inert gas protection, raw material addition, reaction condition control, stirring and monitoring; s3, product separation and purification: reaction completion, product separation, purification treatment and quality detection; s4, performing subsequent treatment; by introducing nitrogen into the reaction kettle, oxygen in a reaction system is eliminated, an oxygen-free environment in the reaction process is maintained, the gas inlet pipe and the exhaust pipe are arranged on the surface of the reaction kettle, and corresponding control equipment is arranged, so that gas in and out in the reaction process are more automatic and accurate, the complexity and the error rate of manual operation are reduced, and the production efficiency is improved. And the possible danger of flammable and explosive substances in the n-heptanal condensation reaction due to the existence of oxygen is avoided.

Description

Technical Field

[0001] The invention belongs to the technical field of organic synthesis, and particularly relates to a method for synthesizing pentylnonanal based on the condensation of n-heptanal. Background Art

[0002] As an important organic compound, n-heptanal has a wide range of industrial applications. It is an important raw material for synthetic fragrances, and is also a key raw material in the fields of pharmaceuticals, organic synthesis, and rubber products. These characteristics of n-heptanal provide a solid foundation for its application in the synthesis of amylnonanal. Condensation reaction is an important type of reaction in organic synthesis. New carbon-carbon bonds can be constructed through condensation reactions to generate compounds with specific structures and properties. In the synthesis process of n-heptanal condensation amylnonanal, condensation reaction plays a vital role.

[0003] However, the existing equipment needs to input a certain amount of inert gas when synthesizing pentylenonenal, but the input of inert gas requires additional equipment and operations, such as gas flow meters, gas pipelines and valves, which will increase the complexity and maintenance difficulty of the system. If the input amount of inert gas is not properly controlled, it may affect the stability and reaction efficiency of the reaction system, resulting in poor synthesis of pentylenonenal, so staff need to improve it. Summary of the invention

[0004] The object of the present invention is to provide a method for synthesizing pentylnonanal based on the condensation of n-heptanal to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A method for synthesizing pentylnonanal based on n-heptanal condensation comprises the following steps:

[0007] S1. Preliminary preparation: including raw material preparation, catalyst selection, reaction equipment preparation and safety preparation;

[0008] S2, reaction operation: including inert gas protection, raw material addition, reaction condition control, stirring and monitoring;

[0009] S3, product separation and purification: including reaction completion, product separation, purification and quality testing;

[0010] S4. Subsequent processing: including catalyst recovery, waste disposal and equipment cleaning and maintenance.

[0011] Preferably, in step S1, raw material preparation: ensure the purity and quality of the n-heptanal raw material, perform drying and impurity removal pretreatment to remove moisture and impurities therein; catalyst selection: select calcium oxide; reaction equipment preparation: prepare the reaction kettle, agitator, thermometer, pressure gauge and reaction equipment of the inert gas supply system, and clean and inspect them to ensure that the equipment is in good condition; safety preparation: formulate detailed safety operating procedures to ensure that operators wear personal protective equipment during operation and operate in a well-ventilated environment.

[0012] Preferably, in step S2, inert gas protection: before the reaction starts, nitrogen is introduced into the reactor to exclude oxygen in the reaction system and maintain an anaerobic environment during the reaction; raw material addition: under nitrogen protection, the pretreated n-heptanal and calcium oxide are added to the reactor in sequence (pay attention to controlling the addition speed and amount to avoid violent reaction); reaction condition control: the reaction temperature is controlled between 60°C and 120°C, the pressure is controlled between normal pressure and 2MPa, and the reaction time is ten hours; stirring and monitoring: during the reaction, the agitator is kept running continuously to ensure that the reactants are fully mixed and the reaction is uniform. At the same time, the temperature and pressure changes of the reaction system are monitored, and the reaction conditions are adjusted as needed.

[0013] Preferably, in step S3, the reaction ends: when the reaction reaches the predetermined time and the reactants are observed to be significantly reduced and the products are obviously generated, the reaction is basically completed, and the heating and stirring should be stopped at this time, and the inert gas supply system should be turned off; product separation: after the reaction mixture is cooled to room temperature, the nonanal is separated from the unreacted raw materials, catalysts and by-products by distillation, extraction and other suitable separation means, and attention is paid to controlling the distillation temperature and time to avoid product decomposition or loss; purification treatment: the separated nonanal is further purified to remove impurities and improve the purity. The purification method selects one of recrystallization and distillation according to the specific situation; quality inspection: the purified nonanal is quality inspected and analyzed to verify whether its purity and specifications meet the requirements. The detection method adopts one of gas chromatography and liquid chromatography.

[0014] Preferably, in step S4, catalyst recovery: the catalyst is recovered and processed for next use, and attention is paid to maintaining the activity and stability of the catalyst during the recovery process; waste treatment: the waste generated during the reaction process is classified, collected and processed to meet environmental protection requirements; equipment cleaning and maintenance: the reaction equipment is thoroughly cleaned and maintained to ensure its performance and safety when it is used next time.

[0015] Preferably, an air inlet pipe is fixedly connected to one side of the top of the reactor surface, a mounting pipe is fixedly connected to the front end of the air inlet pipe, a protective box is fixedly connected to one side of the surface of the air inlet pipe, a servo motor is fixedly connected to one side of the inner wall of the protective box, a driving rod is installed at the output end of the servo motor, a first driving gear is fixedly connected to the bottom end of the driving rod, a first transmission gear is meshedly connected to one side of the surface of the first driving gear, a connecting rod is fixedly connected to one side of the back of the first transmission gear, a bearing sleeve is rotatably connected to one side of the surface of the connecting rod, and one side of the top of the bearing sleeve is fixedly connected to the inner top wall of the air inlet pipe, a second driving gear is fixedly connected to the front end of the connecting rod, a second transmission gear is meshedly connected to one side of the surface of the second driving gear, a driving wheel is fixedly connected to one side of the bottom of the second transmission gear, a transmission belt is rotatably connected to one side of the inner wall of the transmission belt, a plurality of transmission wheels are rotatably connected to the bottom of the driving wheel and the transmission wheel, a fixed frame is fixedly connected to one side of the inner wall of the mounting tube, and the upper and lower sides of the baffle are rotatably connected to the inner wall of the fixed frame.

[0016] Preferably, the tail end of the air inlet pipe is fixedly connected to a ventilation pipe, the tail end of the ventilation pipe is fixedly connected to a connecting pipe, one side of the inner wall of the connecting pipe is fixedly connected to a driving motor, a transmission rod is installed at the output end of the driving motor, the top of the transmission rod is fixedly connected to a fan blade, one side of the surface of the transmission rod is rotatably connected to a support frame, and one side of the surface of the support frame is fixedly connected to the inner wall of the connecting pipe.

[0017] Preferably, a connecting ring is fixedly connected to the bottom end of the connecting tube, a plurality of sets of through tubes are fixedly connected to one side of the surface of the connecting ring, a plurality of sets of air diffusion holes are provided on one side of the bottom of the through tube, a fixing ring is fixedly connected to one side of the top of the through tube, and the surface of the fixing ring is fixedly connected to the inner wall of the reactor.

[0018] Preferably, an exhaust pipe is fixedly connected to the other side of the top of the reactor surface, a solenoid valve is provided on one side of the inner wall of the exhaust pipe, a pressure gauge is fixedly connected to one side of the reactor surface, a controller is fixedly connected to the other side of the reactor surface, a discharge pipe is fixedly connected to the middle of the bottom of the reactor, and multiple groups of support rods are fixedly connected to one side of the bottom of the reactor.

[0019] Preferably, an assembly frame is fixedly connected to the middle part of the top of the reactor, a driving motor is fixedly connected to the top of the inner wall of the assembly frame, a movable rod is installed at the output end of the driving motor, and one side of the surface of the movable rod is inserted into the inner wall of the connecting ring, and one side of the surface of the movable rod is fixedly connected to multiple groups of stirring rods.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] (1) By introducing nitrogen into the reactor, oxygen in the reaction system is eliminated and an oxygen-free environment is maintained during the reaction. An air inlet pipe and an exhaust pipe are arranged on the surface of the reactor and the reactor is equipped with corresponding control equipment, so that the gas inlet and outlet during the reaction process are more automated and precise, reducing the complexity and error rate of manual operation, avoiding the danger of flammable and explosive substances in the condensation reaction of n-heptanal due to the presence of oxygen, and significantly improving the safety of the reaction.

[0022] (2) The reactor can accurately control the reaction temperature and pressure, and carry out reactions within a temperature range of 60°C to 120°C and a pressure range of normal pressure to 2 MPa, ensuring the stability and controllability of the reaction conditions and reducing the occurrence of unexpected situations.

[0023] (3) Under nitrogen protection, the pretreated n-heptanal and calcium oxide are added to the reactor in sequence, and the addition speed and amount are strictly controlled to avoid the occurrence of violent reactions and facilitate the smooth progress of the reaction. After the reaction is completed, the pentyl nonanal is effectively separated from the unreacted raw materials, catalysts and by-products by distillation. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 is a flow chart of the method of the present invention;

[0025] Figure 2 It is a three-dimensional diagram of the reaction kettle of the present invention;

[0026] Figure 3 is a three-dimensional diagram of the air intake pipe of the present invention;

[0027] Figure 4 is a perspective view of a through-tube of the present invention;

[0028] Figure 5 is a stereogram of the connecting ring of the present invention;

[0029] Figure 6 is a three-dimensional diagram of the stirring rod of the present invention;

[0030] In the figure: 1. reactor; 2. air inlet pipe; 3. mounting pipe; 4. protection box; 5. servo motor; 6. driving rod; 7. first driving gear; 8. first transmission gear; 9. connecting rod; 10. second driving gear; 11. second transmission gear; 12. driving wheel; 13. transmission belt; 14. transmission wheel; 15. baffle; 16. fixing frame; 17. ventilation pipe; 18. connecting pipe; 19. driving motor; 20. driving rod; 21. fan blade; 22. supporting frame; 23. connecting ring; 24. through pipe; 25. air diffusion hole; 26. fixing ring; 27. exhaust pipe; 28. pressure gauge; 29. ​​controller; 30. discharge pipe; 31. supporting rod; 32. assembly frame; 33. driving motor; 34. movable rod; 35. stirring rod. DETAILED DESCRIPTION

[0031] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0032] Embodiment 1:

[0033] See also Figure 1 As shown, a method for synthesizing pentylnonanal based on the condensation of n-heptanal comprises the following steps:

[0034] S1. Preliminary preparation: including raw material preparation, catalyst selection, reaction equipment preparation and safety preparation;

[0035] S2, reaction operation: including inert gas protection, raw material addition, reaction condition control, stirring and monitoring;

[0036] S3, product separation and purification: including reaction completion, product separation, purification and quality testing;

[0037] S4. Subsequent processing: including catalyst recovery, waste disposal and equipment cleaning and maintenance.

[0038] In step S1, raw material preparation: ensure the purity and quality of n-heptanal raw material, perform drying and impurity removal pretreatment to remove moisture and impurities therein; catalyst selection: select calcium oxide; reaction equipment preparation: prepare reaction kettle 1, agitator, thermometer, pressure gauge and reaction equipment of inert gas supply system, and clean and inspect them to ensure that the equipment is in good condition; safety preparation: formulate detailed safety operating procedures to ensure that operators wear personal protective equipment during operation and operate in a well-ventilated environment.

[0039] In step S2, inert gas protection: before the reaction starts, nitrogen is introduced into the reactor to exclude oxygen in the reaction system and maintain an oxygen-free environment during the reaction; raw material addition: under nitrogen protection, the pretreated n-heptanal and calcium oxide are added to the reactor in sequence (pay attention to control the addition speed and addition amount to avoid violent reaction); reaction condition control: the reaction temperature is controlled between 60°C and 120°C, the pressure is controlled between normal pressure and 2MPa, and the reaction time is ten hours; stirring and monitoring: during the reaction process, the agitator is kept running continuously to ensure that the reactants are fully mixed and the reaction is uniform. At the same time, the temperature and pressure changes of the reaction system are monitored, and the reaction conditions are adjusted as needed.

[0040] In step S3, the reaction ends: when the reaction reaches the predetermined time and the reactants are observed to be significantly reduced and the products are significantly generated, the reaction is basically completed. At this time, the heating and stirring should be stopped, and the inert gas supply system should be turned off; product separation: after the reaction mixture is cooled to room temperature, the nonanal is separated from the unreacted raw materials, catalysts and by-products by distillation, extraction and other suitable separation means, and the distillation temperature and time are controlled to avoid product decomposition or loss; purification treatment: the separated nonanal is further purified to remove impurities and improve the purity. The purification method selects one of recrystallization and distillation according to the specific situation; quality inspection: the purified nonanal is quality inspected and analyzed to verify whether its purity and specifications meet the requirements. The detection method adopts one of gas chromatography and liquid chromatography.

[0041] In step S4, catalyst recovery: the catalyst is recovered and processed for next use, and attention is paid to maintaining the activity and stability of the catalyst during the recovery process; waste treatment: the waste generated during the reaction process is classified, collected and processed to meet environmental protection requirements; equipment cleaning and maintenance: the reaction equipment is thoroughly cleaned and maintained to ensure its performance and safety when it is used next time.

[0042] Before the reaction begins, nitrogen is introduced into the reactor to exclude oxygen from the reaction system and maintain an anaerobic environment during the reaction. Under nitrogen protection, the pretreated n-heptanal and calcium oxide are added to the reactor in sequence. Attention is paid to controlling the addition speed and amount to avoid violent reactions, which helps to control the reaction temperature and pressure and improve the safety of the reaction. The reaction temperature is controlled between 60°C and 120°C, and the pressure is controlled between normal pressure and 2MPa. The reaction time is ten hours. When the reaction reaches the predetermined time and the reactants are significantly reduced and the products are significantly generated, the reaction is basically completed. At this time, heating and stirring should be stopped, and the inert gas supply system should be turned off. After the reaction mixture is cooled to room temperature, the pentyl nonanal is separated from the unreacted raw materials, catalysts and by-products by distillation, extraction or other suitable separation means. Attention is paid to controlling the distillation temperature and time to avoid product decomposition or loss. The separated pentyl nonanal is further purified to remove impurities and improve the purity. The purified pentyl nonanal is quality tested and analyzed to verify whether its purity and specifications meet the requirements.

[0043] Embodiment 2:

[0044] See also Figures 2 to 6As shown, an air inlet pipe 2 is fixedly connected to one side of the top of the surface of the reactor 1, a mounting pipe 3 is fixedly connected to the front end of the air inlet pipe 2, a protective box 4 is fixedly connected to one side of the surface of the air inlet pipe 2, a servo motor 5 is fixedly connected to one side of the inner wall of the protective box 4, a driving rod 6 is installed at the output end of the servo motor 5, a first driving gear 7 is fixedly connected to the bottom end of the driving rod 6, a first driving gear 7 is meshedly connected to one side of the surface of the first driving gear 7, a connecting rod 9 is fixedly connected to one side of the back of the first driving gear 8, a bearing sleeve is rotatably connected to one side of the surface of the connecting rod 9, and a side of the top of the bearing sleeve is fixedly connected On the inner top wall of the intake pipe 2, the front end of the connecting rod 9 is fixedly connected to the second driving gear 10, one side of the surface of the second driving gear 10 is meshedly connected to the second transmission gear 11, one side of the bottom of the second transmission gear 11 is fixedly connected to the driving wheel 12, one side of the surface of the driving wheel 12 is rotatably connected to the transmission belt 13, one side of the inner wall of the transmission belt 13 is rotatably connected to multiple groups of transmission wheels 14, the bottoms of the driving wheels 12 and the transmission wheels 14 are fixedly connected to the baffle 15, one side of the inner wall of the mounting tube 3 is fixedly connected to the fixing frame 16, and the upper and lower sides of the baffle 15 are rotatably connected to the inner wall of the fixing frame 16.

[0045] When in use, an air inlet pipe 2 is arranged on one side of the top of the surface of the reactor 1, a mounting pipe 3 is arranged at the front end of the air inlet pipe 2, and a servo motor 5 is arranged on the surface of the air inlet pipe 2 through a protective box 4. The staff connects the servo motor 5 to the power supply, and the output end of the servo motor 5 drives the driving rod 6 to rotate, and the driving rod 6 drives the first driving gear 7 at the bottom to rotate, and the first driving gear 7 drives the first transmission gear 8 meshingly connected on the surface to rotate, and the first transmission gear 8 drives the connecting rod 9 on the back to rotate, and the surface of the connecting rod 9 is arranged on the inner top wall of the air inlet pipe 2 through a bearing sleeve to prevent the inert gas from entering, and the connecting rod 9 drives the second driving gear 10 at the front end to rotate, and the second driving gear 10 drives the second transmission gear 11 meshingly connected on the surface The second transmission gear 11 drives the driving wheel 12 at the bottom to rotate, the driving wheel 12 drives the transmission belt 13 on the surface to rotate, and the transmission belt 13 drives multiple driving wheels 14 on the inner wall to rotate, thereby utilizing the driving wheel 12 and the transmission wheel 14 to drive multiple baffles 15 at the bottom to rotate at an angle, and a fixing frame 16 is provided on the inner wall of the mounting tube 3, and the baffle 15 is transversely arranged on the inner wall of the fixing frame 16 when the mounting tube 3 is closed, and the baffle 15 can present different angles in the fixing frame 16 when the mounting tube 3 is opened to control the opening size of the mounting tube 3, and the surface of the mounting tube 3 is convenient for installing a connecting pipe for inert gas, and a fixing frame 16 is provided near the connecting pipe to facilitate controlling the efficiency and flow rate of the inert gas entering the reactor 1.

[0046] Embodiment three:

[0047] See also Figures 2 to 6As shown, the tail end of the air inlet pipe 2 is fixedly connected with a vent pipe 17, the tail end of the vent pipe 17 is fixedly connected with a connecting pipe 18, one side of the inner wall of the connecting pipe 18 is fixedly connected with a driving motor 19, the output end of the driving motor 19 is installed with a transmission rod 20, the top of the transmission rod 20 is fixedly connected with a fan blade 21, one side of the surface of the transmission rod 20 is rotatably connected with a support frame 22, and one side of the surface of the support frame 22 is fixedly connected to the inner wall of the connecting pipe 18, the bottom end of the connecting pipe 18 is fixedly connected with a connecting ring 23, one side of the surface of the connecting ring 23 is fixedly connected with multiple groups of through pipes 24, one side of the bottom of the through pipe 24 is provided with multiple groups of air diffusion holes 25, one side of the top of the through pipe 24 is fixedly connected with a fixing ring 26, and the surface of the fixing ring 26 is fixedly connected with a fixing ring 26. It is connected to the inner wall of the reactor 1, an exhaust pipe 27 is fixedly connected to the other side of the top of the surface of the reactor 1, a solenoid valve is provided on one side of the inner wall of the exhaust pipe 27, a pressure gauge 28 is fixedly connected to one side of the surface of the reactor 1, a controller 29 is fixedly connected to the other side of the surface of the reactor 1, a discharge pipe 30 is fixedly connected to the middle of the bottom of the reactor 1, a plurality of support rods 31 are fixedly connected to one side of the bottom of the reactor 1, an assembly frame 32 is fixedly connected to the middle of the top of the reactor 1, a drive motor 33 is fixedly connected to the top of the inner wall of the assembly frame 32, a movable rod 34 is installed at the output end of the drive motor 33, and one side of the surface of the movable rod 34 is plugged into the inner wall of the connecting ring 23, and one side of the surface of the movable rod 34 is fixedly connected to a plurality of stirring rods 35.

[0048] When in use, a ventilation pipe 17 is provided at the tail end of the air inlet pipe 2, a connecting pipe 18 is provided at the bottom end of the ventilation pipe 17, and a driving motor 19 is provided on the inner wall of the connecting pipe 18. The staff connects the driving motor 19 to a power source, and the output end of the driving motor 19 drives the transmission rod 20 to rotate, and the transmission rod 20 drives the fan blades 21 at the bottom to rotate. The rotation of the fan blades 21 generates wind energy, and the inert gas in the ventilation pipe 17 is transported to the connecting ring 23 at the bottom through the wind energy and suction, and a plurality of through pipes 24 are provided on the surface of the connecting ring 23, and the inert gas is evenly dispersed into the reactor 1 through a plurality of diffusion holes 25 at the bottom of the through pipes 24.

[0049] Embodiment 4:

[0050] See also Figures 1 to 6 As shown, experimental materials: pretreated n-heptanal (purity ≥ 98%), calcium oxide (analytical grade), nitrogen (purity ≥ 99.99%) and other necessary separation and purification reagents (such as solvents, solvents for recrystallization, etc.).

[0051] Experimental equipment: customized reactor (equipped with nitrogen inlet pipe, exhaust pipe, stirring device, temperature and pressure control system, etc.), gas chromatograph, liquid chromatograph, distillation device, extraction device and other necessary laboratory equipment

[0052] Experimental steps:

[0053] Inert gas protection: Before the reaction starts, nitrogen is introduced into the reactor to remove oxygen from the reaction system and maintain an oxygen-free environment during the reaction.

[0054] Raw material addition: under nitrogen protection, add the pretreated n-heptanal and calcium oxide into the reactor in sequence, paying attention to controlling the adding speed and amount to avoid violent reaction.

[0055] Reaction condition control: The reaction temperature is controlled between 60℃ and 120℃, the pressure is controlled between normal pressure and 2MPa, and the reaction time is ten hours. At the same time, the agitator is kept running to ensure that the reactants are fully mixed and the reaction proceeds evenly. Monitor the temperature and pressure changes of the reaction system and adjust the reaction conditions as needed.

[0056] End of reaction and separation of products: When the reaction reaches the predetermined time and the reactants are observed to be significantly reduced and the products are significantly generated, stop heating and stirring, and turn off the inert gas supply system. After the reaction mixture is cooled to room temperature, separate the nonanal from the unreacted raw materials, catalysts and by-products by suitable separation means such as distillation and extraction. Pay attention to controlling the distillation temperature and time to avoid product decomposition or loss.

[0057] Purification: The separated pentylenonanal is further purified to remove impurities and improve purity. The purification method is selected from recrystallization and distillation according to the specific situation.

[0058] Quality testing: The purified pentylnonanal is subjected to quality testing and analysis to verify whether its purity and specifications meet the requirements. The testing method adopts one of the methods of gas chromatography and liquid chromatography.

[0059] Experimental results:

[0060] After the above experimental steps, pentylnonanal was successfully synthesized, and its purity and specifications were verified by gas chromatography and liquid chromatography. The experimental results show that the synthesis method has high yield and purity, and is simple to operate and easy to control, and is suitable for industrial production.

[0061] in conclusion:

[0062] The synthesis method of pentylenonanal based on the condensation of n-heptanal has performed well in practical applications, which not only improves the safety and efficiency of the synthesis, but also reduces production costs and environmental pollution.

[0063] Working principle: when in use, the staff connects the servo motor 5 to the power supply, and the output end of the servo motor 5 drives the driving rod 6 to rotate, and the driving rod 6 drives the first driving gear 7 at the bottom to rotate, and the first driving gear 7 drives the first transmission gear 8 meshingly connected on the surface to rotate, and the first transmission gear 8 drives the connecting rod 9 on the back to rotate, and the surface of the connecting rod 9 is arranged on the inner top wall of the intake pipe 2 through a bearing sleeve to prevent the inert gas from entering, and the connecting rod 9 drives the second driving gear 10 at the front end to rotate, and the second driving gear 10 drives the second transmission gear 11 meshingly connected on the surface to rotate, and the second transmission gear 11 drives the driving wheel 12 at the bottom to rotate, and the driving wheel 12 drives the transmission belt 13 on the surface to rotate, and the transmission belt 13 drives multiple transmission wheels 14 on the inner wall to rotate, thereby utilizing the driving wheel 12 and the transmission wheel 14 to drive multiple gears at the bottom. The plate 15 rotates at an angle. The baffle 15 is laterally arranged on the inner wall of the fixed frame 16 when the mounting tube 3 is closed. When the mounting tube 3 is opened, the baffle 15 can present different angles in the fixed frame 16 to control the opening size of the mounting tube 3. The surface of the mounting tube 3 is convenient for installing the connecting pipe of the inert gas, and a fixed frame 16 is arranged near the connecting pipe to facilitate controlling the efficiency and flow rate of the inert gas entering the reactor 1. The staff connects the drive motor 19 to the power supply, and the output end of the drive motor 19 drives the transmission rod 20 to rotate, and the transmission rod 20 drives the fan blades 21 at the bottom to rotate. The rotation of the fan blades 21 generates wind energy, and the inert gas in the ventilation pipe 17 is transported to the connecting ring 23 at the bottom through the wind energy and suction, and the inert gas is evenly dispersed into the reactor 1 through the multiple diffuser holes 25 at the bottom of the through-tube 24.

[0064] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for synthesizing pentylnonanal based on the condensation of n-heptanal, characterized in that: The following steps are involved: S1. Preliminary preparation: including raw material preparation, catalyst selection, reaction equipment preparation and safety preparation; S2, reaction operation: including inert gas protection, raw material addition, reaction condition control, stirring and monitoring; S3, product separation and purification: including reaction completion, product separation, purification and quality testing; S4. Subsequent processing: including catalyst recovery, waste disposal and equipment cleaning and maintenance.

2. The method for synthesizing pentylnonanal based on the condensation of n-heptanal according to claim 1, characterized in that: In step S1, raw material preparation: ensuring the purity and quality of the n-heptanal raw material, performing drying and impurity removal pretreatment to remove moisture and impurities therein; catalyst selection: selecting calcium oxide; reaction equipment preparation: preparing the reaction kettle (1), agitator, thermometer, pressure gauge and reaction equipment of the inert gas supply system, and cleaning and inspecting them to ensure that the equipment is in good condition; safety preparation: formulating detailed safety operating procedures to ensure that operators wear personal protective equipment during operation and operate in a well-ventilated environment.

3. The method for synthesizing pentylnonanal based on n-heptanal condensation according to claim 1, characterized in that: In step S2, inert gas protection: before the reaction starts, nitrogen is introduced into the reactor to exclude oxygen in the reaction system and maintain an anaerobic environment during the reaction; raw material addition: under nitrogen protection, the pretreated n-heptanal and calcium oxide are added to the reactor in sequence (pay attention to controlling the addition speed and amount to avoid violent reactions); reaction condition control: the reaction temperature is controlled between 60°C and 120°C, the pressure is controlled between normal pressure and 2MPa, and the reaction time is ten hours; stirring and monitoring: during the reaction, the agitator is kept running continuously to ensure that the reactants are fully mixed and the reaction is uniform. At the same time, the temperature and pressure changes of the reaction system are monitored, and the reaction conditions are adjusted as needed.

4. The method for synthesizing pentylnonanal based on the condensation of n-heptanal according to claim 1, characterized in that: In step S3, the reaction ends: when the reaction reaches the predetermined time and the reactants are observed to be significantly reduced and the products are significantly generated, the reaction is basically completed, at which time the heating and stirring should be stopped, and the inert gas supply system should be turned off; product Separation: After the reaction mixture is cooled to room temperature, the pentylenonanal is separated from the unreacted raw materials, catalysts and by-products by distillation, extraction and other suitable separation means, and attention is paid to controlling the distillation temperature and time to avoid product decomposition or loss; Purification: The separated pentylenonanal is further purified to remove impurities and improve the purity. The purification method is selected from recrystallization and distillation according to the specific situation; Quality inspection: The purified pentylenonanal is subjected to quality inspection and analysis to verify whether its purity and specifications meet the requirements. The inspection method adopts one of gas chromatography and liquid chromatography.

5. The method for synthesizing pentylnonanal based on n-heptanal condensation according to claim 1, characterized in that: In step S4, catalyst recovery: the catalyst is recovered and processed for next use, and attention is paid to maintaining the activity and stability of the catalyst during the recovery process; waste treatment: the waste generated during the reaction process is classified, collected and processed to meet environmental protection requirements; equipment cleaning and maintenance: the reaction equipment is thoroughly cleaned and maintained to ensure its performance and safety when it is used next time.

6. A method for synthesizing pentylnonanal based on n-heptanal condensation according to claim 2, characterized in that: An air inlet pipe (2) is fixedly connected to one side of the top of the surface of the reactor (1), a mounting pipe (3) is fixedly connected to the front end of the air inlet pipe (2), a protective box (4) is fixedly connected to one side of the surface of the air inlet pipe (2), a servo motor (5) is fixedly connected to one side of the inner wall of the protective box (4), a driving rod (6) is installed at the output end of the servo motor (5), a first driving gear (7) is fixedly connected to the bottom end of the driving rod (6), a first transmission gear (8) is meshedly connected to one side of the surface of the first driving gear (7), a connecting rod (9) is fixedly connected to one side of the back of the first transmission gear (8), a bearing sleeve is rotatably connected to one side of the surface of the connecting rod (9), and a top side of the bearing sleeve is fixedly connected to The inner top wall of the air intake pipe (2), the front end of the connecting rod (9) is fixedly connected to a second driving gear (10), one side of the surface of the second driving gear (10) is meshingly connected to a second transmission gear (11), one side of the bottom of the second transmission gear (11) is fixedly connected to a driving wheel (12), one side of the surface of the driving wheel (12) is rotatably connected to a transmission belt (13), one side of the inner wall of the transmission belt (13) is rotatably connected to multiple groups of transmission wheels (14), the bottoms of the driving wheel (12) and the transmission wheel (14) are both fixedly connected to a baffle (15), one side of the inner wall of the mounting tube (3) is fixedly connected to a fixing frame (16), and the upper and lower sides of the baffle (15) are both rotatably connected to the inner wall of the fixing frame (16).

7. A method for synthesizing pentylnonanal based on n-heptanal condensation according to claim 6, characterized in that: The tail end of the air inlet pipe (2) is fixedly connected to a ventilation pipe (17), the tail end of the ventilation pipe (17) is fixedly connected to a connecting pipe (18), one side of the inner wall of the connecting pipe (18) is fixedly connected to a driving motor (19), a transmission rod (20) is installed at the output end of the driving motor (19), a fan blade (21) is fixedly connected to the top end of the transmission rod (20), one side of the surface of the transmission rod (20) is rotatably connected to a support frame (22), and one side of the surface of the support frame (22) is fixedly connected to the inner wall of the connecting pipe (18).

8. The method for synthesizing pentylnonanal based on the condensation of n-heptanal according to claim 7, characterized in that: The bottom end of the connecting tube (18) is fixedly connected to a connecting ring (23), one side of the surface of the connecting ring (23) is fixedly connected to multiple groups of through tubes (24), one side of the bottom of the through tube (24) is provided with multiple groups of air diffusion holes (25), one side of the top of the through tube (24) is fixedly connected to a fixing ring (26), and the surface of the fixing ring (26) is fixedly connected to the inner wall of the reaction kettle (1).

9. The method for synthesizing pentylnonanal based on n-heptanal condensation according to claim 6, characterized in that: An exhaust pipe (27) is fixedly connected to the other side of the top of the surface of the reactor (1), a solenoid valve is arranged on one side of the inner wall of the exhaust pipe (27), a pressure gauge (28) is fixedly connected to one side of the surface of the reactor (1), a controller (29) is fixedly connected to the other side of the surface of the reactor (1), a discharge pipe (30) is fixedly connected to the middle of the bottom of the reactor (1), and a plurality of support rods (31) are fixedly connected to one side of the bottom of the reactor (1).

10. The method for synthesizing pentylnonanal based on the condensation of n-heptanal according to claim 6, characterized in that: An assembly frame (32) is fixedly connected to the middle of the top of the reaction kettle (1), a driving motor (33) is fixedly connected to the top of the inner wall of the assembly frame (32), a movable rod (34) is installed at the output end of the driving motor (33), and one side of the surface of the movable rod (34) is inserted into the inner wall of the connecting ring (23), and one side of the surface of the movable rod (34) is fixedly connected to multiple groups of stirring rods (35).

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