A continuous oxidation apparatus for the production of fatty acids from a fatty alcohol

Abstract

The utility model relates to organic synthesis equipment technical field, concretely to a kind of fatty alcohol production fatty acid's continuous oxidation device, including raw material tank, oxygen assembly, gas-liquid mixing component, one-stage oxidation unit, two-stage oxidation unit, extraction unit, washing unit and solvent recovery unit, and the pipe connection control unit between each system, the one-stage oxidation unit and the two-stage oxidation unit are all jacketed pipe reactor, the jacketed pipe reactor includes outer tube, the inside of outer tube is provided with inner tube, the outer portion of inner tube is equipped with helical temperature control pipeline, this fatty alcohol production fatty acid's continuous oxidation device, by two regular oxidation units as core, through diversion dispersion, double catalyst system strengthens three-phase contact, spiral temperature control avoids local overheating, collocation sampling backflow adjustment, improve reaction conversion rate and product purity, continuous operation is combined closed loop solvent recovery, adaptation scale production, with efficient and environmental protection advantage.

Description

Technical Field

[0001] This utility model relates to the field of organic synthesis equipment technology, specifically to a continuous oxidation device for producing fatty acids from fatty alcohols. Background Technology

[0002] A continuous oxidation unit is a device that enables continuous feeding, oxidation reaction, and discharge of materials. It is used to efficiently complete multi-step oxidation processes. A continuous oxidation unit for the production of fatty acids from fatty alcohols is used because the reaction requires continuous oxygen supply and temperature control. The unit can achieve continuous feeding and discharge, avoiding the low efficiency and parameter fluctuation problems of intermittent operation. It can also stabilize the purity of the product and adapt to the needs of large-scale production.

[0003] The oxidation of fatty alcohols to fatty acids is one of the key technologies in the specialty fatty acid industry. Currently, industrial synthesis mainly uses batch oxidation, which is a process with high heat release. Considering safety risks, the reaction rate needs to be slowed down and multiple oxidation processes are required, resulting in low reaction efficiency. In addition, the catalyst needs to be removed by distillation after the traditional batch reaction, which is costly.

[0004] To address this, we propose a continuous oxidation device for fatty alcohols to fatty acids, which features catalyst immobilization and precise temperature control via a spiral temperature-controlled pipeline, effectively preventing localized overheating. Utility Model Content

[0005] One of the technical problems this application aims to solve is that traditional batch oxidation processes generate a large amount of heat, and the catalyst needs to be removed by distillation after the process, resulting in high costs for catalyst separation.

[0006] To address the aforementioned technical problems, this application provides a continuous oxidation apparatus for producing fatty acids from fatty alcohols, comprising a raw material tank, an oxygen assembly, a gas-liquid mixing component, a primary oxidation unit, a secondary oxidation unit, an extraction unit, a washing unit, and a solvent recovery unit, as well as a pipeline connection control unit between the various systems. Both the primary oxidation unit and the secondary oxidation unit are jacketed tubular reactors.

[0007] In some embodiments, the jacketed tubular reactor includes an outer tube, an inner tube is disposed inside the outer tube, a spiral temperature-controlled pipe is sleeved on the outside of the inner tube, a temperature-controlled medium outlet is disposed at the top left side of the outer tube, and a temperature-controlled medium inlet is disposed at the bottom left side of the outer tube.

[0008] In some embodiments, connecting flanges are provided on both the upper and lower sides of the outer tube, and a connecting cone ring is provided on the outside of the connecting flanges, with the outside of the connecting cone ring located on the inside of the inner tube.

[0009] In some embodiments, the inner tube is provided with three support grids, the upper and middle layers of the support grids are filled with honeycomb ceramic catalyst, and the middle and lower layers of the support grids are filled with porous alumina ball catalyst.

[0010] In some embodiments, the outer side of the connecting cone ring abuts against the outer side of the support grid, and the inner side of the connecting cone ring is provided with a placement groove. Four connecting blocks are provided at the bottom of the placement groove, and the outer sides of the four connecting blocks are provided on the inner side of the connecting cone ring.

[0011] In some embodiments, an annular mounting base is placed inside the mounting groove, and four connecting rods are provided on the inner side of the annular mounting base. A flow guide cone is provided on the horizontally similar side of the four connecting rods.

[0012] In some embodiments, the bottom of the flow guide cone is rotatably connected to a rotating shaft, four flow guide plates are provided on the outside of the rotating shaft, four through holes are opened on the outside of the annular mounting base, and the bottom of the annular mounting base is in contact with the top of the four connecting blocks.

[0013] In some embodiments, a sampling tube is provided outside the connecting cone ring, a shut-off valve is provided at the front side of the outer tube, and the end of the sampling tube is provided at the output end of the shut-off valve.

[0014] This utility model has at least the following beneficial effects: 1. Through the regular structural design of the two-stage oxidation unit, combined with the effects of flow guidance and rotating guide plates, the gas-liquid mixture is uniformly dispersed. With the dual catalyst system of honeycomb ceramics and porous alumina balls, the material residence time is extended and the contact between the gas, liquid and solid phases is enhanced. The catalyst is immobilized, reducing the cost of catalyst separation. At the same time, the spiral temperature control pipeline accurately controls the temperature, effectively avoiding local overheating, greatly improving the oxidation conversion rate of fatty alcohols and the purity of fatty acid products, and ensuring the stability of the reaction.

[0015] 2. The entire set of equipment adopts a continuous operation mode, coupled with sampling and detection and reflux adjustment mechanism, which can control the reaction process in real time and ensure that the product meets the standards. The extraction, washing and solvent recovery units form a closed loop to realize solvent recycling, which not only reduces raw material consumption and waste liquid discharge, but also adapts to the needs of large-scale production, significantly improving production efficiency and environmental benefits. Attached Figure Description

[0016] Figure 1 This is a flowchart of the present utility model; Figure 2 This is a schematic diagram of the overall structure of the jacketed tube reactor of this utility model; Figure 3 This is a schematic diagram of the sampling tube structure of this utility model; Figure 4This is a schematic diagram of the connecting cone ring structure of this utility model; Figure 5 This is a schematic diagram of the supporting grid structure of this utility model; Figure 6 This is a schematic diagram of the guide plate structure of this utility model.

[0017] In the diagram: 1. Raw material tank; 2. Oxygen assembly; 3. Gas-liquid mixing component; 4. First-stage oxidation unit; 5. Second-stage oxidation unit; 6. Extraction unit; 7. Washing unit; 8. Solvent recovery unit; 9. Outer pipe; 10. Inner pipe; 11. Spiral temperature-controlled pipe; 12. Temperature-controlled medium outlet; 13. Temperature-controlled medium inlet; 14. Connecting flange; 15. Connecting cone ring; 16. Support grid; 17. Honeycomb ceramic catalyst; 18. Porous alumina ball catalyst; 19. Placement tank; 20. Connecting block; 21. Annular mounting seat; 22. Through hole; 23. Connecting rod; 24. Guide cone; 25. Rotating shaft; 26. Guide plate; 27. Sampling tube; 28. Shut-off valve. Detailed Implementation

[0018] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0019] Example 1: Please refer to Figure 1 , Figure 4 , Figure 5 and Figure 6 This utility model provides a technical solution: a continuous oxidation device for producing fatty acids from fatty alcohols. The first-stage oxidation unit 4 and the second-stage oxidation unit 5 are both jacketed tube reactors. The jacketed tube reactor includes an outer tube 9, which is the outer shell of the reactor. It is cylindrical in shape and has certain strength and corrosion resistance. An inner tube 10 is provided inside the outer tube 9. The inner tube 10 is a flow channel for the reactants. Its inner wall is smooth to reduce the flow resistance of the materials. A spiral temperature control pipe 11 is sleeved on the outside of the inner tube 10. The spiral temperature control pipe 11 is used to control the reaction temperature. Its spiral shape design increases the contact area with the inner tube 10 to improve the temperature control effect. A temperature control medium outlet 12 is provided on the top left side of the outer tube 9. The temperature control medium outlet 12 is used to discharge the temperature control medium. Its position design facilitates the smooth flow of the medium. A temperature control medium inlet 13 is provided on the bottom left side of the outer tube 9. The temperature control medium inlet 13 is used to introduce the temperature control medium. Its position design facilitates the uniform distribution of the medium. Connecting flanges 14 are provided on both the upper and lower sides of the outer tube 9. These connecting flanges 14 are used to connect various parts of the reactor. They are circular in shape and have bolt holes for easy fixing. A connecting conical ring 15 is provided on the outside of the connecting flange 14. The connecting conical ring 15 is used to enhance the sealing of the connection. It is conical in shape and fits tightly against the inside of the inner tube 10. The outside of the connecting conical ring 15 is located on the inside of the inner tube 10. Three support grids 16 are provided inside the inner tube 10. These support grids 16 are used to support the catalyst and keep its position stable. They are circular in shape and have bolt holes for easy fixing. Multiple small holes facilitate the passage of materials. The upper and middle layers of the support grid 16 are filled with honeycomb ceramic catalyst 17, which has a large specific surface area and good catalytic activity. Its honeycomb shape increases the contact area with the reactants. The middle and lower layers of the support grid 16 are filled with porous alumina ball catalyst 18, which has high mechanical strength and chemical stability. Its spherical shape and surface covered with micropores enhance the catalytic effect. The outer part of the connecting cone ring 15 abuts against the outer part of the support grid 16. An installation groove 19 is provided on the inner side of the connecting cone ring 15. The installation groove 19 is used to install the flow guiding device. It is annular in shape and has a moderate depth to ensure stable installation of the device. Four connecting blocks 20 are provided at the bottom of the installation groove 19. The connecting blocks 20 are used to fix the annular mounting base 21. They are rectangular in shape and evenly distributed to provide stable support. The outer side of the four connecting blocks 20 is provided on the inner side of the connecting cone ring 15. The annular mounting base 21 is placed inside the installation groove 19. The annular mounting base 21 is used to install the flow guiding cone 24 and the flow guiding plate 26. It is annular in shape and matches the installation groove 19 to ensure a tight fit. Four connecting rods 23 are provided on the inner side of the annular mounting base 21. The connecting rods 23 are used to connect the flow guiding cone 24 and the annular mounting base 21. They are slender in shape and have a certain strength to support the flow guiding cone 24. A flow guide cone 24 is provided on one side of the four connecting rods 23 at similar horizontal positions. The flow guide cone 24 is used to guide the flow direction of the material. It is cone-shaped with the tip facing the flow direction of the material to reduce flow resistance. A rotating shaft 25 is rotatably connected to the bottom of the flow guide cone 24. The rotating shaft 25 is used to drive the flow guide plate 26 to rotate. It is cylindrical in shape and has a smooth surface to reduce friction. Four flow guide plates 26 are provided on the outside of the rotating shaft 25. The flow guide plates 26 are used to further disperse the material and enhance the mixing effect. They are fan-shaped and evenly distributed around the rotating shaft 25 to achieve uniform flow guidance. Four through holes 22 are provided on the outside of the annular mounting base 21. The through holes 22 are used for detachable connection with the connecting cone ring 15.

[0020] Example 2: Please refer to Figure 2 and Figure 3The system comprises: a raw material tank 1 for storing fatty alcohol raw materials to be oxidized and premixing solvents; an oxygen assembly 2 for providing oxygen for the oxidation reaction, including an oxygen storage tank, pressure regulating valve, and flow meter to ensure the stability and accuracy of oxygen supply; a gas-liquid mixing assembly 3 for mixing fatty alcohol raw materials with oxygen to achieve initial dispersion and mixing of the gas-liquid medium; a first-stage oxidation unit 4 for the initial oxidation reaction, where fatty alcohol undergoes initial catalytic oxidation under the action of a catalyst; a second-stage oxidation unit 5 for the deep oxidation reaction, where the product after the first-stage oxidation is further oxidized to produce fatty acids; an extraction unit 6 for extracting fatty acids from the oxidation product and separating the fatty acid product from the unreacted medium; a washing unit 7 for washing the extracted product to remove impurities; and a solvent recovery unit 8 for recovering the solvent used in the washing process to achieve resource recycling; and a pipeline connection control unit for controlling the material flow and reaction conditions between the systems. The bottom of the annular mounting base 21 contacts the top of the four connecting blocks 20. A sampling tube 27 is provided on the outside of the connecting conical ring 15. The sampling tube 27 is used to take samples from the reactor to monitor the reaction process. It is long and thin and has a valve at the end to control the sampling amount. A shut-off valve 28 is provided on the front side of the outer tube 9. The shut-off valve 28 is used to control the opening and closing of the sampling tube 27. It is spherical and easy to operate to achieve quick opening and closing. The end of the sampling tube 27 is located at the output end of the shut-off valve 28.

[0021] Based on the above embodiments, the following is the complete working principle of the above embodiments: The fatty alcohol raw material and solvent in the raw material tank 1 are mixed in a preset ratio to form a raw material liquid. The conveying rate is adjusted by the control unit connected by the pipeline. At the same time, the oxygen component 2 provides the molecular oxygen required for the reaction. The raw material liquid and oxygen are introduced into the gas-liquid mixing component 3. The gas-liquid mixing component 3 performs preliminary dispersion and mixing of the two media, providing a uniform gas-liquid contact basis for the subsequent oxidation reaction. The mixed gas-liquid mixture is transported to the first oxidation unit 4 through the pipeline. The mixed gas-liquid mixture enters the inner tube 10 through the connecting flange 14 at the upper end of the first oxidation unit 4. It first contacts the guide structure inside the annular mounting seat 21. The guide cone 24 guides the material to diffuse in all directions. At the same time, the impact force of the material flow drives the rotating shaft. The rotation of the four guide plates 26 on the outside of the tube 25 further breaks the agglomeration of the material, so that the gas-liquid mixture is evenly dispersed on the cross-section of the inner tube 10. The dispersed material flows through the honeycomb ceramic catalyst 17 between the upper support grid 16. The regular channel structure of the honeycomb ceramic catalyst 17 provides sufficient contact area for the gas-liquid-solid three phases, realizing the initial catalytic oxidation reaction of fatty alcohol. During the reaction, the temperature control medium enters the spiral temperature control pipe 11 through the temperature control medium inlet 13 at the bottom left of the outer tube 9, flows along the spiral path and exchanges heat with the reaction material in the inner tube 10 in the opposite direction, and removes the heat released by the reaction in time. The temperature-controlled medium is discharged from the temperature control medium outlet 12. The spiral flow channel design ensures that the temperature in the inner tube 10 is uniform and avoids local overheating. The material initially oxidized in the first-stage oxidation unit 4 is transported to the second-stage oxidation unit 5 via a pipeline connected to the control unit. This unit has the same structure as the first-stage oxidation unit 4. After being dispersed again by the guide cone 24 and the rotating guide plate 26, the material enters the porous alumina ball catalyst 18 region between the lower two layers of the supporting grid 16. The high porosity of the porous alumina ball catalyst 18 extends the material residence time, allowing for deep catalytic oxidation of incompletely reacted fatty alcohols and ensuring the desired reaction conversion rate. In both oxidation units, the connecting cone ring 15, through the cooperation of the inner connecting block 20 and the annular mounting seat 21, secures the supporting grid 16, ensuring the structural stability of the catalyst filling area and preventing catalyst layer displacement due to material flow impact. During the reaction... Samples of the reactants inside the inner tube 10 can be collected through sampling tubes 27 in the first-stage oxidation unit 4 and the second-stage oxidation unit 5. The shut-off valve 28 at the front of the outer tube 9 is opened, allowing the material inside the inner tube 10 to flow out through the sampling tubes 27 under reaction pressure. Operators perform conversion rate testing on the samples and adjust the material flow direction via a pipeline-connected control unit based on the test results. If the conversion rate does not reach the preset value, the material is returned to the corresponding oxidation unit for re-reaction. If the conversion rate meets the target, the material enters the next process. The reactants that meet the target enter the extraction unit 6, where the fatty acid products are initially separated from the unreacted medium through contact with the extractant. The separated crude product enters the washing unit 7, where it is purified by washing solvent to remove residual impurities, yielding a high-purity fatty acid product. The solvents separated in the extraction unit 6 and washing unit 7 are transported through pipelines to the solvent recovery unit 8 for purification. The purified solvent is then recycled back to the raw material tank 1, reducing solvent consumption and waste discharge.

[0022] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0023] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention.

Claims

1. A continuous oxidation apparatus for producing fatty acids from fatty alcohols, comprising a raw material tank (1), an oxygen assembly (2), a gas-liquid mixing component (3), a primary oxidation unit (4), a secondary oxidation unit (5), an extraction unit (6), a washing unit (7), and a solvent recovery unit (8), as well as a pipeline connection control unit between the systems, characterized in that: Both the first-stage oxidation unit (4) and the second-stage oxidation unit (5) are jacketed tube reactors.

2. The continuous oxidation apparatus for producing fatty acids from fatty alcohols according to claim 1, characterized in that: The jacketed tube reactor includes an outer tube (9), an inner tube (10) is provided inside the outer tube (9), a spiral temperature control pipe (11) is sleeved on the outside of the inner tube (10), a temperature control medium outlet (12) is provided on the top left side of the outer tube (9), and a temperature control medium inlet (13) is provided on the bottom left side of the outer tube (9).

3. The continuous oxidation apparatus for producing fatty acids from fatty alcohols according to claim 2, characterized in that: The outer tube (9) is provided with connecting flanges (14) on both the upper and lower sides. A connecting cone ring (15) is provided on the outside of the connecting flange (14). The outside of the connecting cone ring (15) is located on the inside of the inner tube (10).

4. The continuous oxidation apparatus for producing fatty acids from fatty alcohols according to claim 3, characterized in that: The inner tube (10) is provided with three support grids (16). The upper and middle layers of the support grids (16) are filled with honeycomb ceramic catalysts (17), and the middle and lower layers of the support grids (16) are filled with porous alumina ball catalysts (18).

5. The continuous oxidation apparatus for producing fatty acids from fatty alcohols according to claim 4, characterized in that: The outer side of the connecting cone ring (15) abuts against the outer side of the support grid (16). The inner side of the connecting cone ring (15) is provided with a mounting groove (19). The bottom of the mounting groove (19) is provided with four connecting blocks (20). The outer side of the four connecting blocks (20) is provided on the inner side of the connecting cone ring (15).

6. The continuous oxidation apparatus for producing fatty acids from fatty alcohols according to claim 5, characterized in that: An annular mounting base (21) is placed inside the mounting groove (19). Four connecting rods (23) are provided on the inner side of the annular mounting base (21). A flow guide cone (24) is provided on the horizontally similar side of the four connecting rods (23).

7. The continuous oxidation apparatus for producing fatty acids from fatty alcohols according to claim 6, characterized in that: The bottom of the flow guide cone (24) is rotatably connected to a rotating shaft (25), and four flow guide plates (26) are provided on the outside of the rotating shaft (25). The annular mounting base (21) has four through holes (22) on its outside. The bottom of the annular mounting base (21) is in contact with the top of the four connecting blocks (20).

8. The continuous oxidation apparatus for producing fatty acids from fatty alcohols according to claim 5, characterized in that: A sampling tube (27) is provided on the outside of the connecting cone ring (15), and a shut-off valve (28) is provided on the front side of the outer tube (9). The end of the sampling tube (27) is provided at the output end of the shut-off valve (28).

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