Method and device for manufacturing octocrylene

Abstract

The invention relates to the technical field of chemical synthesis, in particular to a preparation method and device of octocrylene, and belongs to the technical field of chemical synthesis. The preparation method comprises the following steps: burdening and dissolving, transesterification, decoloration and impurity removal, filtration and slag removal, vacuum distillation and rectification purification. Nitrogen is introduced into the reaction kettle for bubbling to isolate oxygen, so that oxidative deterioration of a product is avoided, and the yield and the purity are improved; medicinal-grade active carbon is adopted for decoloration and impurity removal, and vacuum distillation is combined for efficient recovery of the solvent. The manufacturing device comprises decoloring and impurity removing equipment and filtering equipment, the decoloring and impurity removing equipment adjusts the activated carbon distribution space through lifting of a mesh disc, a feeding mechanism uniformly feeds activated carbon to form a tight filling layer, and the adsorption efficiency is improved; the filtering equipment adopts a spherical filtering mechanism to realize three-stage graded filtering, impurities are discharged in a classified manner in combination with a plugging mechanism, the follow-up treatment difficulty is reduced, and the problems of easy product oxidation, low solvent recovery efficiency and incomplete impurity separation in the traditional process are solved.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical synthesis, and in particular to a method and device for producing octocrylene. Background Art

[0002] Octocrylene, chemically known as ethyl 2-cyano-3,3-diphenylacrylate, is a commonly used organic sunscreen and UV absorber that primarily protects against sunburn by absorbing UVB rays and some UVA rays. Octocrylene is oil-soluble and is often combined with other sunscreen ingredients to enhance the spectral coverage and protective effectiveness of sunscreen products. It is widely used in skin care products such as sunscreen creams and lotions. Within appropriate usage limits, it is highly safe and a common ingredient in sunscreen formulations.

[0003] In the prior art for preparing octocrylene, on the one hand, there is the problem that the reaction process is easily affected by oxygen, resulting in oxidation and deterioration of the product. Due to the lack of effective anti-oxidation measures in the reaction system, the generated intermediate product is prone to side reactions with oxygen in the air during the high-temperature reaction stage, which not only reduces the yield of the target product but also introduces difficult-to-separate oxidative impurities, affecting the purity of the final product. On the other hand, the solvent recovery efficiency is low. In traditional processes, solvents such as isooctyl alcohol used in the reaction are mostly treated by simple distillation. This not only has high energy consumption, but also, due to improper control of distillation conditions, the recovered solvent is of insufficient purity and cannot be directly recycled for production, which not only increases production costs, but also causes resource waste and environmental pollution. Summary of the Invention

[0004] The object of the present invention is to provide a method and apparatus for producing octocrylene to solve the technical problems raised in the above-mentioned background technology.

[0005] To achieve the above objectives, the present invention provides the following technical solutions.

[0006] The present invention provides a method for preparing octocrylene, which specifically comprises the following steps: S1 ingredients and dissolution: according to the mass ratio of 1:2:0.05 take etocrilin, isooctyl alcohol and sodium carbonate, into the reactor and stir to dissolve; S2. Transesterification reaction: nitrogen was bubbled into the reactor, the temperature was raised to reflux, ethanol was recovered by distillation, and the reaction was carried out for 4-6 hours to obtain a reaction solution; S3 decolorization and impurity removal: The reaction solution was decolorized and impurities were removed using pharmaceutical grade activated carbon to obtain a concentrate; S4. Filtration and slag removal: The reaction solution was cooled to 70-80 ° C, and solid impurities and residues were separated by filtration; S5. Vacuum distillation: The filtrate was transferred to a desolventizing vessel and distilled under a vacuum of -0.09 MPa to remove isooctyl alcohol and the front fraction; S6. Distillation and purification: The remaining material is transferred to a distillation kettle, and the target fraction is collected by high vacuum distillation to obtain the finished octocrylene product.

[0007] Preferably, the present invention also provides an octocrylene production device, comprising a decolorization and impurity removal device and a filtering device, the decolorization and impurity removal device is connected and arranged on the downstream side of the reactor, the filtering device is connected and arranged on the downstream side of the decolorization and impurity removal device, and the filtering device is connected to the desolventizing reactor, the decolorization and impurity removal device comprises a tank body A, a mesh disk and a stirring spindle, the stirring spindle is vertically rotatably installed in the tank body A, the mesh disk is movably mounted on the stirring spindle through a sliding hole at its center, and the outer edge wall is slidably fitted with the inner wall of the tank body A, a driving mechanism is provided in the tank body A for driving the mesh disk to rise and fall in the tank body A to adjust the distribution space of the activated carbon, and a feeding mechanism is also provided on the tank body A for evenly feeding the activated carbon into the distribution space in the tank body A, the filtering device comprises a tank body B and a spherical filtering mechanism, the spherical filtering mechanism is provided in the tank body B for filtering and separating solid impurities and residues.

[0008] Preferably, the top opening of the tank body A is provided with a top cover, and the feed port A on the top cover is connected to the discharge port of the reactor through the delivery pipe A. The tank body A is provided with a lifting mechanism for driving the top cover to lift and close. The side of the tank body A is provided with a discharge port A near the bottom end, the top of the tank body B is provided with a feed port B and a water inlet, and the bottom is provided with a discharge port B. The feed port B is connected to the discharge port A through the delivery pipe B, and a pressure pump is installed on the delivery pipe B. The water inlet is connected to the water supply equipment through the water supply pipe, and the discharge port B is connected to the feed port of the desolventizing kettle through a pipeline.

[0009] Preferably, a number of mounting grooves are evenly distributed on the stirring main shaft, and a rotating shaft A is rotatably installed at the top of each mounting groove. A stirring rod is fixedly mounted on each rotating shaft A. When the stirring main shaft does not rotate, the stirring rod is embedded in the mounting groove under the action of gravity. A driving motor A is also fixed to the bottom of the tank body A, and the output shaft of the driving motor A is fixedly connected to the bottom end of the stirring main shaft.

[0010] Preferably, the driving mechanism includes a threaded rod and a driving motor A, the threaded rod is vertically rotatably installed on the inner and outer peripheries of the tank body A, the driving motor A is fixed to the bottom of the tank body A, and the output shaft is fixedly connected to the bottom end of the threaded rod, and the mesh plate is threadedly mounted on the threaded rod through the threaded holes thereon. The lifting mechanism includes a C-shaped frame and a cylinder, the C-shaped frame is fixed to the side of the tank body A, the cylinder is vertically fixed at the top of the C-shaped frame, and the telescopic section of the cylinder is fixedly connected to the upper surface of the top cover.

[0011] Preferably, the feeding mechanism includes a storage tank, an annular seat, a power guide rail and a drive assembly. The annular seat is rotatably mounted on the outer wall of the tank body A, and the power guide rail is horizontally mounted on the outer peripheral wall of the annular seat. A vertical frame is fixed to the top of the movable seat on the power guide rail. The storage tank is mounted on the top of the vertical frame. A feeding pipe is provided at the bottom of the storage tank for feeding activated carbon. The drive assembly is arranged on the side of the tank body A for driving the annular seat to rotate around the axis of the tank body A.

[0012] Preferably, the drive assembly includes a drive motor B and a gear, a gear ring is fixed under the annular seat, the drive motor B is fixed to the side of the tank body A through a side frame, and the gear is fixed on the output shaft of the drive motor B and meshes with the gear ring accordingly.

[0013] Preferably, the spherical filtering mechanism includes a spherical shell and a middle filter screen. The spherical shell is adapted to the size of the tank body B. The spherical shell is fixedly composed of a coarse filter screen above and a fine filter screen below. The middle filter screen is fixed on the inner wall of the coarse filter screen and extends downward into the fine filter screen. The bottom end of the fine filter screen has a debris discharge port A. The middle filter screen is in the shape of a trumpet, the diameter of which becomes smaller as it approaches the debris discharge port A, and the bottom end of the middle filter screen is located inside the debris discharge port A and is contracted to form the debris discharge port A. Rotating shafts B are fixed on both sides of the spherical shell, and the two rotating shafts B are respectively connected to the tank body B for rotation. A driving motor C is fixed to the side of the tank body B, and the output shaft of the driving motor C is fixedly connected to the rotating shaft B on one side. Several annular filter screens are coaxially fixed on the coarse filter screen at intervals. The diameter of the outer annular filter screen is larger than the diameter of the adjacent inner annular filter screen. A sealing mechanism is provided at the bottom of the fine filter screen for sealing the debris discharge port A and the debris discharge port B.

[0014] Preferably, the blocking mechanism includes a blocking cover A and a blocking cover B. A blocking cover A for separately blocking the debris discharge port A is installed at the bottom of the fine filter screen through an opening and closing drive structure A. The opening and closing drive structure A is used to control the rotation and opening and closing of the blocking cover A. The blocking cover A has a through opening at the center. A blocking cover B for separately blocking the debris discharge port B is installed below the blocking cover A through an opening and closing drive structure B. The opening and closing drive structure B is used to control the rotation and opening and closing of the blocking cover B.

[0015] Preferably, a feed port B is installed on the outer wall of the tank body B, and a water inlet is installed on the inner wall of the tank body B, and the feed port B is cooperatively connected to the water inlet.

[0016] Compared with the prior art, the present invention has the following beneficial effects.

[0017] In the transesterification reaction, nitrogen is introduced into the reactor for bubbling, thereby effectively isolating oxygen from contacting the reaction system, preventing deterioration of the intermediate product due to oxidation under high-temperature reflux conditions, reducing the generation of by-products, and significantly improving the yield and purity of the target product, octocrylene. This solves the problem of easy oxidation of the product in the traditional process. The isooctyl alcohol and the front fraction are removed by distillation in a desolvation kettle at a vacuum degree of -0.09 MPa, utilizing a high vacuum environment to lower the boiling point of the solvent and reduce solvent loss. The recovered isooctyl alcohol has a high purity and can be directly recycled for the ingredient dissolution step in step one, thereby reducing production costs, resource waste, and environmental pollution.

[0018] The driving assembly drives the annular seat and the storage tank to rotate, so as to achieve uniform feeding of activated carbon. The driving mechanism drives the mesh plate to rise and fall to adjust the distribution space of activated carbon. The feeding mechanism feeds the activated carbon evenly to form a densely packed layer of activated carbon, which can fully adsorb colored impurities when the reaction liquid passes through. When the stirring spindle rotates, the stirring rod stirs to make the activated carbon more fully dispersed, reduce local accumulation, increase the adsorption capacity of activated carbon per unit mass, and reduce the cost of consumables.

[0019] The coarse filter, medium filter and fine filter constitute a three-stage filtration structure. The stepped design of the annular filter realizes partitioned filtration to relieve filtration pressure. The trumpet-shaped structure of the medium filter guides the flow of impurities. Combined with the precise control of the blocking mechanism, it realizes graded filtration and collection of sodium carbonate, medium-sized impurities and small-sized activated carbon impurities.

[0020] The impurity discharge port B and the impurity discharge port A are controlled to open in sequence, and the driving motor C drives the spherical shell to rotate. The water supply pipe is combined with the use of ultrasonic equipment to achieve graded cleaning to avoid impurities clogging the filter material and maintain the stability of the filtration performance. At the same time, impurities are discharged in a classified manner, reducing the difficulty of subsequent recycling and processing caused by the mixed discharge of impurities. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 Detailed steps of the method for producing octocrylene according to the present invention; Figure 2 This is the process system diagram of this preparation method; Figure 3 Schematic diagram of the structure of the decolorization and impurity removal equipment in the present invention; Figure 4 for Figure 1 Schematic diagram of the cross section of the structure shown; Figure 5 This is one of the structural diagrams of the feeding mechanism in the present invention; Figure 6 This is the second structural diagram of the feeding mechanism in the present invention; Figure 7 This is a schematic diagram of the installation of the mesh plate structure in the present invention; Figure 8 for Figure 7 The schematic diagram of the local structure shown; Figure 9 Schematic diagram of the formation of a densely packed layer of activated carbon; Figure 10 It is a schematic structural diagram of the filtering device in the present invention; Figure 11 for Figure 10 The schematic cross-sectional view of the local structure is shown; Figure 12 It is a schematic structural diagram of the spherical filtering mechanism in the present invention; Figure 13 for Figure 12 A schematic diagram of another perspective of the structure shown; Figure 14 for Figure 12 Schematic cross-section of the structure shown.

[0022] In the figure: 01, densely packed layer of activated carbon; 02, decolorization and impurity removal equipment; 03, filtration equipment; 1, tank body A; 11, top cover; 12, feed port A; 121, delivery pipe A; 13, discharge port A; 2, mesh plate; 21, slide hole; 22, threaded hole; 3, stirring spindle; 31, drive motor A; 32, stirring rod; 33, mounting groove; 34, rotating shaft A; 4, driving mechanism; 41, threaded rod; 42, driving motor A; 5, feeding mechanism; 51, storage tank; 511, feed pipe; 52, annular seat; 53, power guide rail; 531, moving seat; 54, stand; 55, drive assembly; 551, side frame; 552, drive motor B; 553. Gear; 554. Gear ring; 6. Lifting mechanism; 61. C-shaped frame; 62. Cylinder; 7. Spherical filtering mechanism; 701. Impurity discharge port A; 702. Impurity discharge port B; 71. Ball shell; 711. Coarse filter screen; 712. Fine filter screen; 713. Ring filter screen; 72. Medium filter screen; 73. Rotating shaft B; 74. Drive motor C; 8. Sealing mechanism; 81. Sealing cover A; 811. Through port; 82. Opening and closing drive structure A; 83. Sealing cover B; 84. Opening and closing drive structure B; 9. Tank body B; 91. Feed port B; 911. Delivery pipe B; 912. Pressure pump; 92. Water inlet; 921. Water supply pipe; 93. Discharge port B. DETAILED DESCRIPTION

[0023] The embodiments of the present invention are described below with reference to the accompanying drawings.

[0024] In the description of the embodiments of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms, "connection", and "installation" should be understood in a broad sense. For example, "connection" can be a detachable connection or a non-detachable connection; it can be a direct connection or an indirect connection through an intermediate medium. In addition, "communication" can be a direct connection or an indirect connection through an intermediate medium. Here, "fixed" means that the two are connected to each other and the relative position relationship after connection remains unchanged. The directional terms mentioned in the embodiments of the present invention, such as "inside", "outside", "top", "bottom", etc., are only reference to the directions of the accompanying drawings. Therefore, the directional terms used are for better and clearer explanation and understanding of the embodiments of the present invention, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the embodiments of the present invention.

[0025] In the embodiments of the present invention, the terms "first" and "second" are used for descriptive purposes only and should not be understood to indicate or imply relative importance or implicitly specify the number of technical features indicated. Therefore, features defined as "first" or "second" may explicitly or implicitly include one or more of the features.

[0026] In the embodiments of the present invention, "and / or" is simply a description of the association relationship between associated objects, indicating that three possible relationships exist. For example, "A and / or B" can represent three situations: A exists alone, A and B exist simultaneously, and B exists alone. Furthermore, the character " / " in this document generally indicates that the associated objects are in an "or" relationship.

[0027] References to "one embodiment" or "some embodiments" in this specification mean that a particular feature, structure, or characteristic described in connection with that embodiment is included in one or more embodiments of the present invention. Thus, phrases such as "in one embodiment," "in some embodiments," "in other embodiments," and "in yet other embodiments" appearing in various places in this specification do not necessarily refer to the same embodiment, but rather mean "one or more, but not all, embodiments," unless otherwise specifically emphasized. The terms "including," "comprising," "having," and variations thereof mean "including but not limited to," unless otherwise specifically emphasized. Example 1

[0028] See also Figure 1 The present invention provides a method for preparing octocrylene, which specifically comprises the following steps: S1 ingredients and dissolution: according to the mass ratio of 1:2:0.05 take etocrilin, isooctyl alcohol and sodium carbonate, into the reactor and stir to dissolve; S2 transesterification reaction: nitrogen was bubbled into the reactor, the temperature was raised to reflux, ethanol was recovered by distillation, and the reaction was carried out for 5 hours to obtain a reaction solution; S3 decolorization and impurity removal: The reaction solution was decolorized and impurities were removed using pharmaceutical grade activated carbon to obtain a concentrate; S4. Filtration and slag removal: The reaction solution was cooled to 70 ° C and filtered to separate solid impurities and residues; S5. Vacuum distillation: The filtrate was transferred to a desolventizing vessel and distilled under a vacuum of -0.09 MPa to remove isooctyl alcohol and the front fraction; S6. Distillation and purification: The remaining material is transferred to a distillation kettle, and the target fraction is collected by high vacuum distillation to obtain the finished octocrylene product. Example 2

[0029] See also Figure 2-Figure 14 The present invention also provides an octocrylene production device, which is applied to steps 3 and 4 of the production method in Example 1. The device includes a decolorization and impurity removal device 02 and a filtering device 03. The decolorization and impurity removal device 02 is connected to the downstream side of the reactor, and the filtering device 03 is connected to the downstream side of the decolorization and impurity removal device 02. The filtering device 03 is connected to the desolventizing reactor. The decolorization and impurity removal device 02 can be used to perform preliminary decolorization and impurity removal on the reaction liquid to improve the quality of the target product. The reaction liquid after preliminary decolorization and impurity removal by the decolorization and impurity removal device 02 is filtered by the filtering device 03. The reaction liquid after filtration is then purified in the desolventizing reactor and the distillation reactor in sequence to finally obtain the desired octocrylene product.

[0030] The decolorization and impurity removal equipment 02 includes a tank body A1, a mesh plate 2 and a stirring shaft 3, wherein the top of the tank body A1 has an opening for placing activated carbon, and the opening is equipped with a top cover 11. The tank body A1 is provided with a lifting mechanism 6 for driving the top cover 11 to perform lifting, opening and closing adjustment. The top cover 11 has a feed port A12, and the feed port A12 is connected to the discharge port of the reactor through a conveying pipe A121. The tank body A1 has a discharge port A13 on the side near the bottom.

[0031] The stirring shaft 3 is vertically rotatably installed in the tank body A1, and the mesh disk 2 is movably mounted on the stirring shaft 3 through the sliding hole 21 at its center, and the outer edge wall is slidably fitted with the inner wall of the tank body A1. The mesh disk 2 is both rotationally connected to the stirring shaft 3 and can slide up and down along the stirring shaft 3. The hole size on the mesh disk 2 is smaller than the activated carbon particle size, so that a distribution space is formed in the tank body A1 between the mesh disk 2 and the top cover 11 for storing activated carbon. A driving mechanism 4 is provided in the tank body A1 for driving the mesh disk 2 to rise and fall in the tank body A1 to adjust the activated carbon distribution space. A feeding mechanism 5 is also provided on the tank body A1.

[0032] During the initial decolorization and impurity removal of the reaction liquid, first, the lifting mechanism 6 drives the top cover 11 upward to remove the blockage of the top opening of the tank body A1. Then, the feeding mechanism 5 evenly feeds the activated carbon from the top opening of the tank body A1 into the tank body A1 and places it above the mesh plate 2. Subsequently, the lifting mechanism 6 drives the top cover 11 downward to seal the top opening of the tank A1. Then, the driving mechanism 4 drives the mesh plate 2 upward, and the mesh plate 2 cooperates with the top cover 11 to squeeze the activated carbon tightly. Figure 9 As shown, a densely packed layer 01 of activated carbon is formed below the feed port A12 in the tank body A1.

[0033] When the reaction liquid is transported from the reactor to the tank body A1 through the delivery pipe A121 and the feed port A12, the reaction liquid passes through the densely packed activated carbon layer 01, and the activated carbon can adsorb the colored substances in the reaction liquid and some impurities formed by the reaction.

[0034] In order to increase the adsorption area, powdered activated carbon is used. Furthermore, the particle size of the activated carbon is much smaller than that of the sodium carbonate. Therefore, the sodium carbonate used as a reaction catalyst cannot pass through the holes on the mesh disk 2 and then be mixed into the densely packed activated carbon layer 01.

[0035] The activated carbon is tightly compacted into an activated carbon dense filling layer 01, so that the gaps between the activated carbon are small, which effectively improves the absorption capacity of colored substances in the reaction solution and improves the decolorization effect.

[0036] like Figure 4 、 Figure 7 and Figure 8 As shown, a number of mounting grooves 33 are evenly distributed on the stirring main shaft 3, and a rotating shaft A34 is rotatably installed at the upper part of each mounting groove 33. A stirring rod 32 is fixedly mounted on each rotating shaft A34. When the stirring main shaft 3 does not rotate, the stirring rod 32 is embedded in the mounting groove 33 under the action of gravity to avoid obstruction and interference with the lifting of the mesh plate 2. In addition, a driving motor A31 is fixed to the bottom of the tank body A1, and the output shaft of the driving motor A31 is fixedly connected to the bottom end of the stirring main shaft 3.

[0037] The mesh plate 2 is driven downward to the bottom limit position of the tank body A1 by the driving mechanism 4. At this time, the mesh plate 2 is lower than the discharge port A13, so that the activated carbon and sodium carbonate solid materials are filled and evenly distributed in the tank body A1. Then, the driving motor A31 is driven to drive the stirring shaft 3 to rotate in the tank body A1. Under the action of the centrifugal force of the rotation, the installation groove 33 hingedly installed by the rotating shaft A34 will be inclined at a certain angle and rotate synchronously with the stirring shaft 3, thereby stirring the reaction liquid mixed with activated carbon and sodium carbonate. The purpose of stirring is to make the activated carbon evenly dispersed in the reaction liquid, increase the adsorption and impurity removal area of ​​the activated carbon, and further adsorb the tiny impurities in the reaction liquid, thereby improving the initial impurity removal effect of the reaction liquid.

[0038] During the above stirring process, the mesh plate 2 is driven by the driving mechanism 4 to perform a small distance reciprocating lifting and lowering adjustment. The upward height of the driving mechanism 4 is lower than the stirring rod 32 of the lowest layer on the stirring main shaft 3. The driving mechanism 4 reciprocates up and down at the bottom of the tank body A1, thereby intensifying the surge of the reaction liquid at the bottom of the tank body A1, thereby reducing the precipitation of activated carbon and further improving the initial adsorption and impurity removal effect.

[0039] The filtering equipment 03 includes a tank body B9 and a spherical filtering mechanism 7. The tank body B9 has a feed port B91 and a water inlet 92 on the top, and a discharge port B93 on the bottom. The feed port B91 is connected to the discharge port A13 through a conveying pipe B911. The reaction liquid in the tank body A1 that has been preliminarily decolorized and impurity-removed can enter the tank body B9 through the discharge port A13, the conveying pipe B911 and the feed port B91 in sequence. The conveying pipe B911 is equipped with a pressure pump 912 for conveying the reaction liquid under positive pressure. The water inlet 92 is connected to the water supply equipment through a water supply pipe 921, which is used to supply water to the tank body B9 during cleaning. The discharge port B93 is connected to the feed port of the desolventizing kettle through a pipeline, which is used to convey the filtered reaction liquid to the desolventizing kettle. The spherical filtering mechanism 7 is arranged in the tank body B9, which is used to filter and separate solid impurities and residues, wherein the solid impurities and residues are specifically activated carbon, sodium carbonate, original impurities and impurities produced by other reactions. Example 3

[0040] See also Figure 4 The difference between this embodiment and embodiment 2 is that: The driving mechanism 4 includes a threaded rod 41 and a driving motor A42. The threaded rod 41 is vertically installed on the inner and outer peripheries of the tank body A1. The driving motor A42 is fixed at the bottom of the tank body A1, and the output shaft is fixedly connected to the bottom end of the threaded rod 41. The mesh plate 2 is threadedly mounted on the threaded rod 41 through the threaded hole 22 thereon. The driving motor A42 drives the threaded rod 41 to rotate forward and reverse. The rotating threaded rod 41 can threadably drive the mesh plate 2 to slide up and down, providing stable drive for the lifting and lowering of the mesh plate 2.

[0041] The lifting mechanism 6 includes a C-shaped frame 61 and a cylinder 62. The C-shaped frame 61 is fixed to the side of the tank body A1, and the cylinder 62 is vertically fixed to the top of the C-shaped frame 61. The telescopic section of the cylinder 62 is fixedly connected to the upper surface of the top cover 11. When the cylinder 62 extends, it can push the top cover 11 downward so that the top cover 11 can cover the top of the tank body A1 to block the top opening of the tank body A1. When the cylinder 62 retracts, it can drive the top cover 11 upward to cancel the blockage of the top opening of the tank body A1 and at the same time make room above the tank body A1 so that the feeding mechanism 5 can feed the activated carbon into the tank body A1. Example 4

[0042] See also Figure 5 and Figure 6 The difference between this embodiment and embodiment 3 is that: Specifically, the feeding mechanism 5 includes a storage tank 51, an annular seat 52, a power guide rail 53 and a driving assembly 55. The annular seat 52 is rotatably mounted on the outer wall of the tank body A1, and the power guide rail 53 is horizontally installed on the outer peripheral wall of the annular seat 52. A vertical frame 54 is fixed to the top of the movable seat 531 on the power guide rail 53. The storage tank 51 is installed on the top of the vertical frame 54. A feeding pipe 511 is provided at the bottom of the storage tank 51 for feeding activated carbon, and a feeding valve is provided on the feeding pipe 511. The driving assembly 55 is provided on the side of the tank body A1 for driving the annular seat 52 to rotate around the axis of the tank body A1.

[0043] Among them, the driving assembly 55 includes a driving motor B552 and a gear 553. A gear ring 554 is fixed under the annular seat 52. The driving motor B552 is fixed to the side of the tank body A1 through the side frame 551. The gear 553 is fixed on the output shaft of the driving motor B552 and engages with the gear ring 554 accordingly.

[0044] When adding activated carbon, the required amount of activated carbon is first loaded into the storage tank 51 for temporary storage. Then, the top cover 11 is adjusted upward by the lifting mechanism 6. At the same time, the power guide rail 53 drives the moving seat 531 to move along the radial direction of the tank body A1. Under the support of the stand 54, the storage tank 51 is driven to move closer to the axis of the tank body A1 until the feeding pipe 511 is tilted and aligned with the opening of the tank body A1. Subsequently, by adjusting the feeding valve, the activated carbon in the storage tank 51 is guided into the tank body A1 through the feeding pipe 511. At the same time, the driving motor B552 is used to drive the gear 553 to rotate, and the rotating gear 553 engages the driving gear ring 554 and the annular seat 52 to rotate, thereby driving the storage tank 51 to rotate around the axis of the tank body A1, so that the feeding pipe 511 feeds along a circular path, ensuring that the activated carbon fed above the mesh plate 2 is evenly distributed, avoiding local excessive accumulation that affects the formation of the activated carbon dense filling layer 01. Example 5

[0045] See also Figure 11-14 The difference between this embodiment and embodiment 4 is that: The spherical filtering mechanism 7 includes a spherical shell 71 and a medium filter 72. The spherical shell 71 is adapted to the size of the tank body B9. The spherical shell 71 is fixedly composed of a coarse filter 711 above and a fine filter 712 below. The medium filter 72 is fixed on the inner wall of the coarse filter 711 and extends downward into the fine filter 712. The filter pore size of the coarse filter 711 is larger than the filter pore size of the medium filter 72, and the filter pore size of the medium filter 72 is larger than the filter pore size of the fine filter 712. That is, the coarse filter 711 is used to filter large-particle impurities such as sodium carbonate, the medium filter 72 is used to filter other medium-particle impurities, and the fine filter 712 is used to filter small-particle impurities such as activated carbon, so as to achieve a graded filtration effect and improve filtration efficiency.

[0046] In addition, the medium filter 72 is arranged in the spherical shell 71 formed by the coarse filter 711 and the fine filter 712, so that a cavity A is formed between the medium filter 72 and the coarse filter 711 for collecting medium-sized impurities, and a cavity B is formed between the medium filter 72 and the fine filter 712 for collecting impurities such as activated carbon, and the spherical shell 71 is adaptably installed in the tank body B9, so that impurities such as sodium carbonate are filtered out above the coarse filter 711, thereby realizing the classified collection of impurities.

[0047] In addition, a number of annular filters 713 are coaxially fixed at intervals on the coarse filter 711. The diameter of the outer annular filter 713 is larger than the diameter of the adjacent inner annular filter 713. This design allows the filtering portion on the coarse filter 711 to be arranged in zones, effectively alleviating the filtration pressure of filtering large particles of impurities due to excessive concentration. At the same time, after the impurities enter between the two annular filters 713, due to the slope structure of the coarse filter 711, the reaction liquid flushes the impurities to a lower place, thereby reducing the situation where impurities accumulate excessively in a certain place and cause blockage.

[0048] Among them, the bottom end of the fine filter 712 has a debris discharge port A701, the medium filter 72 is in the shape of a trumpet, the diameter of which becomes smaller as it approaches the debris discharge port A701, and the bottom end of the medium filter 72 is located inside the debris discharge port A701 to form the debris discharge port A701. The coarse filter 711, the medium filter 72 and the fine filter 712 are all three-dimensional surface structures with arcs, which effectively increase the filtration area and further reduce the filtration pressure.

[0049] Rotating shafts B73 are fixed on both sides of the spherical shell 71, and the two rotating shafts B73 are respectively connected to the tank body B9 for rotation. A driving motor C74 is fixed on the side of the tank body B9, and the output shaft of the driving motor C74 is fixedly connected to the rotating shaft B73 on one side. A sealing mechanism 8 is provided at the bottom of the fine filter 712 for sealing the impurity discharge port A701 and the impurity discharge port B702.

[0050] A feed port B91 is installed on the outer wall of the tank body B9, and a water inlet 92 is installed on the inner wall of the tank body B9. The feed port B91 and the water inlet 92 are connected together. The feed port B91 and the water inlet 92 constitute the ultrasonic equipment as a whole. The equipment also includes other accessories, all of which adopt existing technologies. The specific structure and working principle will not be described in detail.

[0051] After the filtration is completed, clean water is supplied to the tank body B9 through the water inlet 92, and then the blockage of the impurity discharge port B702 is cancelled by controlling the sealing mechanism 8, and the signal is transmitted to the water inlet 92 through the operation of the tank body B9, generating ultrasonic vibration in the water body, which can shake off the medium-sized impurities temporarily stored in the clamping cavity A from the middle filter 72 and discharge them from the impurity discharge port B702, and finally discharge them from the discharge port B93 along with the water body, thereby achieving the cleaning of medium-sized impurities.

[0052] Similarly, by controlling the blocking mechanism 8 to cancel the blocking of the impurity discharge port A701, impurities such as activated carbon in the clamping cavity B are discharged from the impurity discharge port A701 and finally discharged through the discharge port B93, thereby achieving the cleaning of the particle size of activated carbon.

[0053] By driving the motor C74, the rotating shaft B73 is driven to rotate, driving the ball shell 71 and the middle filter 72 to rotate 180 degrees as a whole, so that the coarse filter 711 faces downward, and impurities such as sodium carbonate accumulated between the two adjacent annular filter screens 713 fall down and are finally discharged through the discharge port B93.

[0054] The above-mentioned impurity classification and discharge mechanism avoids the mixed discharge of impurities such as activated carbon and sodium carbonate in traditional technologies, reducing the difficulty of subsequent activated carbon and sodium carbonate recovery.

[0055] The blocking mechanism 8 includes a blocking cover A81 and a blocking cover B83. A blocking cover A81 for separately blocking the debris discharge port A701 is installed at the bottom of the fine filter 712 through an opening and closing drive structure A82. The opening and closing drive structure A82 is used to control the rotation and opening and closing of the blocking cover A81. A through opening 811 is provided at the center of the blocking cover A81. A blocking cover B83 for separately blocking the debris discharge port B702 is installed below the blocking cover A81 through an opening and closing drive structure B84. The opening and closing drive structure B84 is used to control the rotation and opening and closing of the blocking cover B83. Both the opening and closing drive structure A82 and the opening and closing drive structure B84 adopt existing technologies and will not be described in detail.

[0056] The opening and closing driving structure A82 drives the blocking cover A81 to rotate and close, so as to block the debris discharge port A701. The opening and closing driving structure B84 drives the blocking cover B83 to rotate and close, so as to block the through-port 811. The through-port 811 corresponds to the position of the debris discharge port B702, thereby achieving the blocking of the debris discharge port B702. When discharging impurities, the opening and closing driving structure B84 first drives the blocking cover B83 to rotate and open, and cancels the blocking of the debris discharge port B702, so that medium-sized impurities can be discharged from the debris discharge port B702. Afterwards, the opening and closing driving structure A82 drives the blocking cover A81 to rotate and open, and cancels the blocking of the debris discharge port A701, so that impurities such as activated carbon can be discharged from the debris discharge port A701.

[0057] Among them, when the sealing cover A81 is opened, the blockage of the impurity discharge port A701 is cancelled and the blockage of the impurity discharge port B702 is also cancelled. The cleaning of the clamping cavity A precedes the cleaning of the clamping cavity B. Therefore, even if the impurity discharge port B702 and the impurity discharge port A701 are opened at the same time, it will not affect the discharge of impurities such as activated carbon.

[0058] The control method of the present invention is automatic control through a controller. The control circuit of the controller can be implemented by simple programming by technicians in this field. The provision of power is also common knowledge in this field, so the present invention will no longer explain the control method and circuit connection in detail.

[0059] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention.

Claims

1. A method for producing octocrylene, characterized in that: The specific steps include: S1 ingredients and dissolution: according to the mass ratio of 1:2:0.05 take etocrilin, isooctyl alcohol and sodium carbonate, into the reactor and stir to dissolve; S2. Transesterification reaction: nitrogen was bubbled into the reactor, the temperature was raised to reflux, ethanol was recovered by distillation, and the reaction was carried out for 4-6 hours to obtain a reaction solution; S3 decolorization and impurity removal: The reaction solution was decolorized and impurities were removed using pharmaceutical grade activated carbon to obtain a concentrate; S4. Filtration and slag removal: The reaction solution was cooled to 70-80 ° C, and solid impurities and residues were separated by filtration; S5. Vacuum distillation: The filtrate was transferred to a desolventizing vessel and distilled under a vacuum of -0.09 MPa to remove isooctyl alcohol and the front fraction; S6. Distillation and purification: The remaining material is transferred to a distillation kettle, and the target fraction is collected by high vacuum distillation to obtain the finished octocrylene product.

2. An octocrylene production device, used in the octocrylene production method according to claim 1, characterized in that: It comprises a decolorization and impurity removal device (02) and a filtering device (03), wherein the decolorization and impurity removal device (02) is arranged in a communication manner on the downstream side of the reaction kettle, and the filtering device (03) is arranged in a communication manner on the downstream side of the decolorization and impurity removal device (02), and the filtering device (03) is connected to the desolventizing kettle; The decolorization and impurity removal equipment (02) comprises a tank body A (1), a mesh plate (2) and a stirring main shaft (3); The stirring main shaft (3) is vertically rotatably mounted in the tank body A (1), and the mesh plate (2) is movably mounted on the stirring main shaft (3) through a sliding hole (21) at its center, and the outer edge wall is slidably fitted with the inner wall of the tank body A (1); A driving mechanism (4) is provided in the tank body A (1) for driving the mesh plate (2) to move up and down in the tank body A (1) to adjust the distribution space of the activated carbon; The tank body A (1) is also provided with a feeding mechanism (5) for uniformly feeding the activated carbon into the distribution space within the tank body A (1); The filtering device (03) comprises a tank body B (9) and a spherical filtering mechanism (7). The spherical filtering mechanism (7) is arranged in the tank body B (9) and is used for filtering and separating solid impurities and residues.

3. The octocrylene production device according to claim 2, characterized in that: The top opening of the tank body A (1) is provided with a top cover (11), and the feed port A (12) on the top cover (11) is connected to the discharge port of the reactor through a delivery pipe A (121); The tank body A (1) is provided with a lifting mechanism (6) for driving the top cover (11) to be raised and lowered, opened and closed; The tank body A (1) has a discharge port A (13) at the side near the bottom end; The tank body B (9) has a feed port B (91) and a water inlet (92) at the top, and a discharge port B (93) at the bottom; The feed port B (91) is connected to the discharge port A (13) via a delivery pipe B (911), and a pressure pump (912) is installed on the delivery pipe B (911). The water inlet (92) is connected to a water supply device via a water supply pipe (921); The discharge port B (93) is connected to the feed port of the desolventizing kettle through a pipeline.

4. The octocrylene production device according to claim 2, characterized in that: The stirring main shaft (3) is evenly distributed with a plurality of mounting grooves (33), and a rotating shaft A (34) is rotatably mounted at the top of each mounting groove (33); Each of the rotating shafts A (34) is fixedly mounted with a stirring rod (32); When the stirring main shaft (3) does not rotate, the stirring rod (32) is embedded and accommodated in the installation groove (33) under the action of gravity; A driving motor A (31) is also fixed to the bottom of the tank body A (1), and the output shaft of the driving motor A (31) is fixedly connected to the bottom end of the stirring main shaft (3).

5. The device for producing octocrylene according to claim 3, wherein: The driving mechanism (4) comprises a threaded rod (41) and a driving motor A (42); The threaded rod (41) is vertically rotatably mounted on the inner and outer peripheries of the tank body A (1), the driving motor A (42) is fixed to the bottom of the tank body A (1), and the output shaft is fixedly connected to the bottom end of the threaded rod (41); The mesh plate (2) is threadably mounted on the threaded rod (41) through the threaded hole (22) thereon; The lifting mechanism (6) includes a C-shaped frame (61) and a cylinder (62); The C-shaped frame (61) is fixed to the side of the tank body A (1), the cylinder (62) is vertically fixed to the top of the C-shaped frame (61), and the telescopic section of the cylinder (62) is fixedly connected to the upper surface of the top cover (11).

6. The device for producing octocrylene according to claim 2, wherein: The feeding mechanism (5) comprises a storage tank (51), an annular seat (52), a power guide rail (53) and a driving assembly (55); The annular seat (52) is rotatably mounted on the outer wall of the tank body A (1), and the power guide rail (53) is horizontally mounted on the outer peripheral wall of the annular seat (52); A stand (54) is fixed on the top of the movable seat (531) on the power guide rail (53), and the storage tank (51) is installed on the top of the stand (54); The bottom of the storage tank (51) is provided with a feeding pipe (511) for feeding activated carbon; The driving assembly (55) is provided on the side of the tank body A (1) and is used to drive the annular seat (52) to rotate around the axis of the tank body A (1).

7. The device for producing octocrylene according to claim 6, wherein: The driving assembly (55) includes a driving motor B (552) and a gear (553); A gear ring (554) is fixed below the annular seat (52); The driving motor B (552) is fixed to the side of the tank body A (1) via a side frame (551), and the gear (553) is fixed to the output shaft of the driving motor B (552) and meshes with the gear ring (554).

8. The device for producing octocrylene according to claim 2, wherein: The spherical filter mechanism (7) comprises a spherical shell (71) and a middle filter screen (72); The spherical shell (71) is adapted to the size of the tank body B (9), and the spherical shell (71) is fixedly composed of an upper coarse filter (711) and a lower fine filter (712); The medium filter (72) is fixed on the inner wall of the coarse filter (711) and extends downward into the fine filter (712); The bottom end of the fine filter (712) is provided with a debris discharge port A (701); The middle filter (72) is in a trumpet shape, the diameter of which decreases as it approaches the impurity discharge opening A (701), and the bottom end of the middle filter (72) is located inside the impurity discharge opening A (701) and is constricted to form the impurity discharge opening A (701); Rotating shafts B (73) are fixed to both sides of the spherical shell (71), and the two rotating shafts B (73) are rotatably connected to the tank body B (9). A driving motor C (74) is fixed to the side of the tank body B (9), and an output shaft of the driving motor C (74) is fixedly connected to the rotating shaft B (73) on one side; A plurality of annular filter screens (713) are coaxially fixed at intervals on the coarse filter screen (711), and the diameter of the outer annular filter screen (713) is larger than the diameter of the adjacent inner annular filter screen (713); A blocking mechanism (8) is provided at the bottom of the fine filter (712) for blocking the impurity discharge port A (701) and the impurity discharge port B (702).

9. The device for producing octocrylene according to claim 8, wherein: The blocking mechanism (8) comprises a blocking cover A (81) and a blocking cover B (83); The bottom of the fine filter (712) is provided with the blocking cover A (81) for blocking the impurity discharge port A (701) separately via an opening and closing drive structure A (82), and the opening and closing drive structure A (82) is used to control the rotation opening and closing of the blocking cover A (81); The blocking cover A (81) has a through opening (811) at its center. The blocking cover B (83) for independently blocking the impurity discharge opening B (702) is installed below the blocking cover A (81) via an opening and closing drive structure B (84). The opening and closing drive structure B (84) is used to control the rotation and opening and closing of the blocking cover B (83).

10. The device for producing octocrylene according to claim 2, wherein: A feed port B (91) is installed on the outer wall of the tank body B (9), and a water inlet (92) is installed on the inner wall of the tank body B (9). The feed port B (91) is cooperatively connected with the water inlet (92).

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