Device and method for preparing piperidine triazine derivative and amine condensation compound

By improving the preparation apparatus and method, uniform feeding and efficient stirring of piperidine triazine derivatives and amine condensates were achieved, solving the problems of uneven feeding and insufficient stirring in traditional methods, and improving reaction efficiency and product purity.

CN120860916AActive Publication Date: 2025-10-31FUJIAN DISHENG TECH CO LTD
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Patent Information

Application Number
CN202511409695.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-29
Publication Date
2025-10-31
Estimated Expiration
2045-09-29

AI Technical Summary

Technical Problem

Existing technologies for preparing piperidine triazine derivatives and amine condensates suffer from problems such as uneven feeding, insufficient stirring, and independent operation of feeding and stirring, leading to frequent side reactions, low reaction efficiency, and low product purity.

Method used

A preparation device including a moving stirring component and a follow-up feeding component is adopted. The dynamic addition and three-dimensional stirring of materials are realized through cross struts and hoisting mechanism. Combined with the use of metering pump and heating wire, the feeding uniformity and stirring effect are ensured. The nano-catalyst is used to carry out continuous reaction under high temperature and high pressure.

Benefits of technology

It achieves uniform mixing and efficient reaction of materials, improves reaction efficiency and product purity, and achieves a yield of over 95%.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a preparation device and method of piperidine triazine derivatives and amine condensation compounds, and relates to the technical field of chemical reaction equipment, the preparation device comprises a base, two pairs of supporting brackets are fixed on the base, a main tank is rotatably mounted on the two pairs of supporting brackets respectively, an auxiliary tank is fixedly mounted on the two pairs of supporting brackets, and the preparation device further comprises a movable stirring assembly and a follow-up feeding assembly, the movable stirring assembly comprises a pair of guide transverse shafts; side arm rods are mounted on the guide transverse shafts in a sliding manner; when the cross supporting rod shrinks, the piston rod can move upwards, and materials in the end barrel are discharged through the one-way liquid outlet valve and the three-way pipe; when the cross supporting rod extends, under the action of the extension shaft, the piston rod can move downwards, and materials in an external feeding system are sucked into the end cylinder, so that the materials are added more uniformly and gently, and the adding position is displaced along with the folding and unfolding of the cross supporting rod and is more dynamic, and the mixing effect of the materials is improved.
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Description

Technical Field

[0001] This invention relates to the field of chemical reaction equipment technology, and in particular to an apparatus and method for preparing a piperidine triazine derivative and an amine condensate. Background Technology

[0002] Traditional UV absorbers contain NH groups on their rings, exhibiting a certain degree of alkalinity. This limits their application in acidic resins, acidic compounding agents, and acidic environments. To broaden their application areas, research on low alkalinity has become a hot topic in HALS light stabilizers, especially N-alkoxy hindered amines. Products such as NOR116, Tinuvin123, TINUVIN152, NOR371, and LA-81 are already on the market. Among them, stabilizers with photostability and a certain degree of low alkalinity can be widely used in acidic systems of agricultural film coatings.

[0003] Currently, in the preparation of piperidine triazine derivatives and amine condensates, existing technologies typically employ batch reactors for material mixing and reaction. However, the feeding method and stirring mechanism have the following shortcomings: Traditional methods typically involve adding reactants to the main reaction vessel all at once or rapidly, lacking a smooth and controllable feeding process. This rapid feeding can easily lead to excessively high local concentrations, triggering side reactions or uneven mixing, thus affecting reaction efficiency and product purity. For example, in the preparation process, if TBHP (tert-butyl hydroperoxide) and piperidine triazine derivatives are not mixed sufficiently, localized peroxidation may trigger side reactions, reducing the yield. In addition, conventional stirring devices usually use fixed stirring paddles, which have a limited stirring range. Especially for high viscosity or heterogeneous systems (such as reaction liquids containing nano-catalysts), insufficient mixing will significantly prolong the reaction time. Finally, feeding and stirring are often operated independently, lacking a linkage mechanism. For example, the feeding position is fixed and cannot be dynamically adjusted during the stirring process, making it difficult for newly added materials (such as cyclohexane or TBHP) to disperse in a timely manner, thus slowing down the reaction process. In addition, the preheating function is separated from the stirring stage in traditional equipment, which can easily cause uneven heating of the materials, requiring additional time to balance the temperature. Summary of the Invention

[0004] The purpose of this invention is to provide an apparatus and method for preparing piperidine triazine derivatives and amine condensates, so as to solve the problems mentioned in the background art.

[0005] The technical solution of the present invention is: an apparatus for preparing a piperidine triazine derivative and an amine condensate, comprising a base, two pairs of support brackets fixed on the base, a main tank rotatably mounted on the two pairs of support brackets and a secondary tank fixedly mounted on the two pairs of support brackets, and further comprising: A mobile mixing assembly includes a pair of guide shafts, each with a side arm slidably mounted on it. The two side arms are fixed to a connecting seat on opposite sides. A main shaft cylinder is rotatably mounted on the connecting seat. A square groove is provided inside the main shaft cylinder. A prism is slidably mounted in the vertical direction inside the square groove. A hoisting mechanism is provided at the top of the prism. The follow-up feeding assembly includes an H-shaped support rod disposed on one side of the main tank, a pair of guide horizontal shafts fixed between the top of the H-shaped support rod and the base, and cross support rods hinged between the two side arm rods and the H-shaped support rod. Two guide connecting rods are slidably installed on the two guide horizontal shafts, and a pair of end cylinders are fixed on each guide connecting rod. A piston rod is slidably installed inside each end cylinder, and an extension rod is fixed to the bottom end of each piston rod. The extension rod and the cross support rod are provided with a transmission unit.

[0006] Preferably, each of the cross struts is rotatably connected via a movable shaft, and an extension shaft is fixedly connected to one side of the movable shaft corresponding to the end cylinder on each cross strut. Each extension rod is rotatably connected to the extension shaft, and multiple paddles are fixed on each extension rod. A heating wire is installed inside the lower half of the extension rod.

[0007] Preferably, each of the end cylinders is fixedly connected to a feed pipe at its top end, and a one-way liquid inlet valve is fixedly installed on the feed pipe. A three-way pipe is fixedly connected to the side of the end cylinder near the top end, and a one-way liquid outlet valve is fixedly installed at one end of the three-way pipe. The feed pipe is connected to an external feed system through a flexible hose.

[0008] Preferably, the hoisting mechanism includes a pair of guide rail brackets fixed to the base, and the two guide rail brackets are fixedly connected to a U-shaped rail groove on opposite sides. The top of the prism is rotatably connected to a lifting rod through a bearing, and two rollers are rotatably installed on the lifting rod, with the rollers rollingly connected to the inner wall of the U-shaped rail groove.

[0009] Preferably, a drive motor is fixedly installed on the side of the base near the main tank, and the output shaft of the drive motor is fixedly connected to an output spindle. A drive wheel is fixedly installed at the top of the output spindle, and a transmission rod is rotatably installed on the surface of the drive wheel. The other end of the transmission rod is rotatably connected to the connecting seat through a movable shaft. A drive gear is fixedly installed on the output spindle, and a driven gear ring that meshes with the drive gear is fixedly installed on the outer peripheral wall of the main tank.

[0010] Preferably, a side support is fixedly installed on the base, a rack is fixedly installed at the end of the side support, and a driven gear that meshes with the rack is fixed at one end of the main shaft near the top.

[0011] Preferably, a pair of side arm columns are fixedly connected to the bottom end of the prism, and multiple symmetrically arranged stirring blocks are fixedly connected to each side arm column. Multiple mesh ring plates are fixedly connected to both side arm columns.

[0012] Preferably, a pair of metering pumps are fixedly installed on the base, the input ends of the two metering pumps are fixedly connected to the discharge pipes, the output ends of the two metering pumps are fixedly connected to the output pipes, and the ends of the two output pipes are fixedly connected to an external reactor.

[0013] Preferably, an electrically controlled valve is fixedly installed at one end of each of the two discharge pipes, the bottom end of the auxiliary tank is fixedly connected to the discharge pipe located at the bottom end, the bottom end of the main tank is rotatably connected to the discharge pipe located at the bottom end, and a reinforcing frame is fixed between each of the two discharge pipes and the base.

[0014] A method for preparing a piperidine triazine derivative and amine condensate, applied to the apparatus for preparing the piperidine triazine derivative and amine condensate, characterized by comprising the following steps: Step 1: Add industrial-grade molybdenum trioxide (25wt%), deionized water (50wt%), and glass beads (25wt%) to a high-efficiency grinder mixing sampler and grind for more than 10 hours. Take samples to test the particle size until the laser particle size analyzer shows that D90 meets the requirements, where D90≤100nm. After grinding, filter the glass beads with sand cloth first, and then filter the filtrate through a 0.1-micron microporous membrane to obtain nano-sized wet catalyst. After drying the wet catalyst, the nano-catalyst is obtained. Step 2: Add the condensate of 2,4-bis[N-butyl-[1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl]amino]-1,3,5-triazine and N,N-bis(3-aminopropyl)ethyl ethylamine (24.9 wt%) to the external feeding system. Add cyclohexane (41.6 wt%) and nano-catalyst (0.2 wt%) to the main tank. Use the moving stirring component and the follow-up feeding component to mix the three evenly and preheat to 90°C. Step 3: Store 80% TBHP (33.3wt%) separately in an auxiliary tank. Use a metering pump to feed the materials from the main tank and auxiliary tank into the reactor, controlling the reaction temperature at 90℃ and the back pressure at 0.5 MPa, and continuously feed the reaction. Step 4: Take samples for testing. If the samples do not meet the standards, continue the reaction until they are qualified. Step 5: After the reaction is complete, cool to 60℃, filter to recover the catalyst, distill the filtrate under normal pressure to recover cyclohexane, then desolvate in a high vacuum in a demelting kettle, and granulate or pulverize to obtain the condensate of 2,4-bis[N-butyl-(1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl)amino]-1,3,5-triazine and N,N-bis(3-aminopropyl)ethylethylamine, with a yield ≥95%.

[0015] The present invention provides an improved apparatus and method for preparing a piperidine triazine derivative and an amine condensate, which has the following improvements and advantages compared with the prior art: Firstly, when the cross strut retracts, the piston rod moves upward, discharging the material in the end cylinder through the one-way discharge valve and the three-way pipe. When the cross strut extends, the piston rod moves downward under the action of the extension shaft, drawing the material from the external feeding system into the end cylinder. This makes the material addition more uniform and gradual, and the addition position shifts with the extension and retraction of the cross strut, making it more dynamic and improving the mixing effect of the material. Secondly, when the main shaft cylinder of this invention moves horizontally, it promotes the vertical movement of the prism. Specifically, the main shaft cylinder is provided with a square groove, in which the prism can slide up and down. When the connecting seat moves, the prism adjusts its position in the vertical direction through the hoisting mechanism, realizing the three-dimensional movement of the prism, so that the stirring component can cover different height areas of the main tank and enhance the stirring effect. Thirdly, when the main shaft of the present invention moves, the driven gear meshes with the rack and pinion, causing the main shaft to rotate, which drives the stirring component to alternately rotate forward and backward, so as to further enhance the mixing effect. Attached Figure Description

[0016] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0017] Figure 1 This is a first-view perspective three-dimensional structural diagram of the present invention; Figure 2 This is a schematic diagram of the main structure of the present invention; Figure 3 This is a schematic diagram of the overall second-view structure of the present invention; Figure 4 This is a three-dimensional structural diagram of the main tank of the present invention; Figure 5 For the present invention Figure 4 Enlarged structural diagram at point A in the middle; Figure 6 This is a three-dimensional structural diagram of the drive wheel, guide shaft, and H-shaped support rod of the present invention. Figure 7 This is a three-dimensional structural diagram of the main shaft and side arm of the present invention; Figure 8 This is a three-dimensional structural diagram of the output spindle and connecting seat of the present invention; Figure 9 For the present invention Figure 8 Enlarged structural diagram at point B; Figure 10This is a schematic diagram of the planar structure of the end cylinder and piston rod of the present invention; Figure 11 This is a schematic diagram of the cross-sectional structure of the main tank of the present invention.

[0018] Figure label: 1. Base; 101. Support bracket; 102. Guide rail bracket; 103. U-shaped rail groove; 104. Hanging rod; 105. H-shaped strut; 106. Roller; 107. Side support; 108. Rack and pinion; 2. Auxiliary tank; 3. Main tank; 301. Driven gear ring; 4. Metering pump; 401. Output pipe; 402. Discharge pipe; 5. Drive motor; 501. Output spindle; 502. Drive gear; 503. Drive wheel; 504. Transmission rod; 6. 601. Connecting seat; 602. Side arm; 603. Guide horizontal shaft; 604. Guide connecting rod; 7. Main shaft cylinder; 705. Prism; 706. Driven gear; 8. Cross strut; 807. End cylinder; 808. T-shaped pipe; 809. Extension rod; 8001. Piston rod; 8002. Extension shaft; 801. Paddle; 802. One-way liquid outlet valve; 803. Feed pipe; 804. One-way liquid inlet valve; 905. Side arm column; 901. Stirring block; 902. Mesh ring plate. Detailed Implementation

[0019] The present invention will now be described in detail, and the technical solutions in the embodiments of the present invention will be clearly and completely described. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0020] This invention provides an improved apparatus and method for preparing piperidine triazine derivatives and amine condensates. The technical solution of this invention is as follows: like Figures 1 to 11 As shown, this embodiment of the invention provides an apparatus for preparing a piperidine triazine derivative and an amine condensate, including a base 1, on which two pairs of support brackets 101 are fixed. A main tank 3 is rotatably mounted on each of the two pairs of support brackets 101, and a secondary tank 2 is fixedly mounted on each pair of support brackets 101. The support brackets 101 are used to support the main tank 3 and the secondary tank 2. The apparatus also includes: The mobile mixing assembly includes a pair of guide shafts 602, on which side arms 601 are slidably mounted. A connecting seat 6 is fixed to the opposite side of each side arm 601. A main shaft cylinder 7 is rotatably mounted on the connecting seat 6. A square groove is provided inside the main shaft cylinder 7, and a prism 701 is slidably mounted vertically within the square groove. A hoisting mechanism is provided at the top of the prism 701. The hoisting mechanism facilitates the vertical movement of the prism 701 when the main shaft cylinder 7 moves horizontally. Specifically, the main shaft cylinder 7 has a square groove within which the prism 701 can slide up and down. When the connecting seat 6 moves, the prism 701 adjusts its position vertically via the hoisting mechanism, achieving three-dimensional movement of the prism 701.

[0021] The follow-up feeding component enables dynamic material addition, ensuring that feeding and mixing are synchronized, thus improving mixing efficiency. The follow-up feeding component includes an H-shaped support rod 105 located on one side of the main tank 3, a pair of guide horizontal shafts 602 fixed between the top of the H-shaped support rod 105 and the base 1, and cross support rods 8 hinged between the two side arm rods 601 and the H-shaped support rod 105. Two guide connecting rods 603 are slidably installed on the two guide horizontal shafts 602, and a pair of end cylinders 801 are fixed on each guide connecting rod 603. A piston rod 804 is slidably installed inside each end cylinder 801, and an extension rod 803 is fixed to the bottom end of each piston rod 804. The extension rod 803 and the cross support rod 8 are connected by a transmission unit. Through the above structure, when the connecting seat 6 moves along the guide horizontal shaft 602, it can pull the cross support rod 8 to retract or expand, thereby moving the piston rod 804 and the end cylinder 801 while also moving the piston rod 804 in the vertical direction.

[0022] Furthermore, each cross strut 8 is rotatably connected via a movable shaft, and an extension shaft 805 is fixedly connected to one side of the movable shaft corresponding to the end cylinder 801 on each cross strut 8. Each extension rod 803 is rotatably connected to the extension shaft 805, and multiple paddles 806 are fixed on each extension rod 803. A heating wire is installed inside the lower half of the extension rod 803. The heating wire enables the extension rod 803 to have a heating function, thereby facilitating the heating and temperature rise of the material inside the main tank 3, ensuring that the reaction temperature reaches the preset value (such as 90℃), and creating conditions for subsequent reactions.

[0023] Furthermore, to prevent backflow and ensure a stable supply of materials to the external feeding system, a feeding pipe 808 is fixedly connected to the top of each end cylinder 801, and a one-way inlet valve 809 is fixedly installed on the feeding pipe 808. A three-way pipe 802 is fixedly connected to the side of the end cylinder 801 near the top, and a one-way outlet valve 807 is fixedly installed at one end of the three-way pipe 802. The feeding pipe 808 is connected to an external feeding system via a flexible hose. The external feeding system is used to supply 2,4-bis[N-butyl-[1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl]amino]-1,3,5-trimethylolpropionic acid. The condensate of aziridine and N,N-di(3-aminopropyl)ethylethylamine; with the above structure, when the cross strut 8 contracts, the piston rod 804 can move upward and discharge the material in the end cylinder 801 through the one-way discharge valve 807 and the three-way pipe 802; when the cross strut 8 extends, under the action of the extension shaft 805, the piston rod 804 can move downward and suck the material in the external feeding system into the end cylinder 801, so that the material addition is more uniform and gentle, and the addition position will be displaced with the extension and retraction of the cross strut 8, thus becoming more dynamic and improving the mixing effect of the material.

[0024] Furthermore, the hoisting mechanism includes a pair of guide rail brackets 102 fixed to the base 1, and the two guide rail brackets 102 are fixedly connected to a U-shaped rail groove 103 on opposite sides. The top of the prism 701 is rotatably connected to a lifting rod 104 via a bearing. Two rollers 106 are rotatably mounted on the lifting rod 104. The rollers 106 are in rolling contact with the inner wall of the U-shaped rail groove 103. It should be noted that the curvature of the U-shaped rail groove 103 is the same as the curvature of the bottom of the main tank 3. With the above structure, when the prism 701 moves with the connecting seat 6, the rollers 106 will move on the U-shaped rail groove 103, thereby adjusting the height of the prism 701 according to the U-shaped rail groove 103. This allows the stirring component to cover different height areas of the main tank 3, enhancing the stirring effect.

[0025] Furthermore, a drive motor 5 is fixedly installed on the side of the base 1 near the main tank 3, and the output shaft of the drive motor 5 is fixedly connected to an output main shaft 501. A drive wheel 503 is fixedly installed at the top of the output main shaft 501, and a transmission rod 504 is rotatably installed on the surface of the drive wheel 503. The other end of the transmission rod 504 is rotatably connected to the connecting seat 6 through a movable shaft. When the drive motor 5 is running, it can drive the drive wheel 503 to rotate through the output main shaft 501. In conjunction with the transmission rod 504, it can drive the connecting seat 6 to reciprocate along the guide horizontal axis 602. A drive gear 502 is fixedly installed on the output main shaft 501, and a driven gear ring 301 that meshes with the drive gear 502 is fixedly installed on the outer peripheral wall of the main tank 3. At the same time, when the output main shaft 501 drives the drive gear 502 to rotate, the main tank 3 can be driven to rotate through the transmission action of the driven gear ring 301, so as to improve the mixing effect of the material in the main tank 3.

[0026] Furthermore, a side support 107 is fixedly installed on the base 1, and a rack 108 is fixedly installed at the end of the side support 107. A driven gear 702 that meshes with the rack 108 is fixed at one end of the main shaft cylinder 7 near the top. When the main shaft cylinder 7 moves along the rack 108, the meshing action of the driven gear 702 and the rack 108 can drive the main shaft cylinder 7 to rotate. Moreover, when moving back and forth, the rotation direction of the main shaft cylinder 7 is opposite, which can further improve the mixing effect of the material in the main tank 3.

[0027] As a further embodiment of the present invention, a pair of side arm columns 9 are fixedly connected to the bottom end of the prism 701, and a plurality of symmetrically arranged stirring blocks 901 are fixedly connected to each side arm column 9. A plurality of perforated ring plates 902 are fixedly connected to both side arm columns 9. With the above structure, when the main shaft cylinder 7 rotates, it can synchronously drive the prism 701 to rotate. In conjunction with the side arm columns 9 and stirring blocks 901, and along with the main shaft cylinder 7, the stirring range of the side arm columns 9 can be effectively increased. At the same time, the prism 701 can move vertically under the action of the roller 106 and the U-shaped rail groove 103. In conjunction with the plurality of perforated ring plates 902, the stirring effect on the material can be effectively improved in the vertical direction. Specifically, the stirring blocks 901 are responsible for breaking up material clumps, while the perforated ring plates 902 promote the uniform dispersion and flow of the material through their perforated structure.

[0028] Furthermore, a pair of metering pumps 4 are fixedly installed on the base 1. The input ends of both metering pumps 4 are fixedly connected to the discharge pipes 402, and the output ends of both metering pumps 4 are fixedly connected to the output pipes 401. The ends of the two output pipes 401 are fixedly connected to an external reactor. Through the above structure, the materials in the main tank 3 and the auxiliary tank 2 can be fed into the external reactor by the metering pumps 4 to carry out the reaction. In this application, a self-made nano molybdenum oxide catalyst is synthesized and fully mixed in the external reactor under a back pressure of 0.5 MPa, which greatly improves the mixing efficiency, thereby effectively shortening the reaction time and increasing the yield.

[0029] Furthermore, to facilitate the control of the discharge of the main tank 3 and the auxiliary tank 2, an electric control valve is fixedly installed at one end of each of the two discharge pipes 402. The bottom end of the auxiliary tank 2 is fixedly connected to the discharge pipe 402 located at the bottom end. In order to avoid the main tank 3 rotating and causing motion interference with the discharge pipe 402 at the bottom, the bottom end of the main tank 3 is rotatably connected to the discharge pipe 402 located at the bottom end. At the same time, in order to improve the structural stability of the two discharge pipes 402, a reinforcing frame is fixed between the two discharge pipes 402 and the base 1.

[0030] The specific working method is as follows: Cyclohexane and nano-catalyst are added to the main tank 3. Piperidine triazine derivative and amine condensate are connected to the follow-up feeding component through an external feeding system. TBHP is stored separately in the auxiliary tank 2. The drive motor 5 is started, which drives the output main shaft 501 to rotate. The drive wheel 503 pushes the connecting seat 6 to move back and forth along the guide horizontal axis 602 through the transmission rod 504. When the connecting seat 6 moves, the side arm 601 drives the main shaft cylinder 7 to move horizontally. At the same time, the prism 701 slides up and down in the U-shaped rail groove 103 through the roller 106 to realize the three-dimensional movement of the stirring block 901 and the mesh ring plate 902. The cross support rod 8 extends and retracts with the movement of the connecting seat 6. The piston rod 804 is pulled by the extension shaft 805 to suck the material from the feeding pipe 808 into the end cylinder 801, and then into the main tank 3 through the three-way pipe 802. In addition, the heating wire preheats the material simultaneously. When the main shaft cylinder 7 moves, the driven gear 702 meshes with the rack rod 108, causing the main shaft cylinder 7 to rotate, which drives the stirring component to alternately rotate forward and backward, enhancing the mixing effect. The uniformly mixed material is pumped into the external reactor in proportion by the metering pump 4, and reacts continuously under high temperature and high pressure. After the reaction is completed, the product undergoes cooling, filtration, distillation and other steps to obtain a high-purity target compound. The catalyst and solvent can be recycled.

[0031] Example 2 A method for preparing a piperidine triazine derivative-amine condensate, applied in an apparatus for preparing the piperidine triazine derivative-amine condensate, includes the following steps: Step 1: Add industrial-grade molybdenum trioxide (25wt%), deionized water (50wt%), and glass beads (25wt%) to a high-efficiency grinder mixing sampler and grind for more than 10 hours. Take samples to test the particle size until the laser particle size analyzer shows that D90 meets the requirements, where D90≤100nm. After grinding, filter the glass beads with sand cloth first, and then filter the filtrate through a 0.1-micron microporous membrane to obtain nano-sized wet catalyst. After drying the wet catalyst, the nano-catalyst is obtained. Step 2: Add the condensate of 2,4-bis[N-butyl-[1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl]amino]-1,3,5-triazine and N,N-bis(3-aminopropyl)ethyl ethylamine (24.9 wt%) to the external feeding system. Add cyclohexane (41.6 wt%) and nano-catalyst (0.2 wt%) to the main tank 3. Use the moving stirring component and the follow-up feeding component to mix the three evenly and preheat to 90°C. Step 3: Store 80% TBHP (33.3wt%) separately in auxiliary tank 2. Use metering pump 4 to feed the materials from main tank 3 and auxiliary tank 2 into the reactor, control the reaction temperature at 90℃ and the back pressure at 0.5 MPa, and continuously feed the reaction. Step 4: Take samples for testing. If the samples do not meet the standards, continue the reaction until they are qualified. Step 5: After the reaction is complete, cool to 60℃, filter to recover the catalyst, distill the filtrate under normal pressure to recover cyclohexane, and then desolvate in a high vacuum in a demelting kettle. The condensate of 2,4-bis[N-butyl-(1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl)amino]-1,3,5-triazine with N,N-bis(3-aminopropyl)ethylethylamine is obtained by granulation or pulverization, with a yield ≥95%.

[0032] The foregoing description enables those skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. An apparatus for preparing a piperidine triazine derivative and an amine condensate, comprising a base (1), two pairs of support brackets (101) fixed on the base (1), a main tank (3) rotatably mounted on the two pairs of support brackets (101) and a secondary tank (2) fixedly mounted thereon, characterized in that, Also includes: A mobile mixing assembly includes a pair of guide shafts (602), on which side arms (601) are slidably mounted. A connecting seat (6) is fixed on the opposite side of the two side arms (601). A main shaft cylinder (7) is rotatably mounted on the connecting seat (6). A square groove is opened in the main shaft cylinder (7). A prism (701) is slidably mounted in the square groove in the vertical direction. A hoisting mechanism is provided at the top of the prism (701). The follow-up feeding assembly includes an H-shaped support rod (105) set on one side of the main tank (3), a pair of guide horizontal shafts (602) fixed between the top of the H-shaped support rod (105) and the base (1), and two side arm rods (601) and the H-shaped support rod (105) are hinged with cross support rods (8). Two guide connecting rods (603) are slidably installed on the two guide horizontal shafts (602), and a pair of end cylinders (801) are fixed on each guide connecting rod (603). A piston rod (804) is slidably installed inside the end cylinder (801), and an extension rod (803) is fixed at the bottom of the piston rod (804). The extension rod (803) and the cross support rod (8) are provided with a transmission unit.

2. The apparatus for preparing a piperidine triazine derivative and amine condensate according to claim 1, characterized in that: Each of the cross struts (8) is rotatably connected via a movable shaft, and an extension shaft (805) is fixedly connected to one side of the movable shaft corresponding to the end cylinder (801) on each cross strut (8). Each of the extension rods (803) is rotatably connected to the extension shaft (805). Multiple paddles (806) are fixed on each extension rod (803). A heating wire is installed inside the lower half of the extension rod (803).

3. The apparatus for preparing a piperidine triazine derivative and amine condensate according to claim 2, characterized in that: Each of the end cylinders (801) is fixedly connected to a feed pipe (808) at its top end, and a one-way inlet valve (809) is fixedly installed on the feed pipe (808). A three-way pipe (802) is fixedly connected to one side of the end cylinder (801) near the top end, and a one-way outlet valve (807) is fixedly installed at one end of the three-way pipe (802). The feed pipe (808) is connected to an external feed system through a hose.

4. The apparatus for preparing a piperidine triazine derivative and amine condensate according to claim 1, characterized in that: The hoisting mechanism includes a pair of guide rail brackets (102) fixed on the base (1), and the two guide rail brackets (102) are fixedly connected to the opposite sides of a U-shaped rail groove (103). The top of the prism (701) is rotatably connected to a lifting rod (104) via a bearing. Two rollers (106) are rotatably mounted on the lifting rod (104), and the rollers (106) are rolled in connection with the inner wall of the U-shaped rail groove (103).

5. The apparatus for preparing a piperidine triazine derivative and amine condensate according to claim 1, characterized in that: A drive motor (5) is fixedly installed on the side of the base (1) near the main tank (3), and the output shaft of the drive motor (5) is fixedly connected to an output spindle (501). A drive wheel (503) is fixedly installed at the top of the output spindle (501), and a transmission rod (504) is rotatably installed on the surface of the drive wheel (503). The other end of the transmission rod (504) is rotatably connected to the connecting seat (6) through a movable shaft. A drive gear (502) is fixedly installed on the output spindle (501), and a driven gear ring (301) that meshes with the drive gear (502) is fixedly installed on the outer peripheral wall of the main tank (3).

6. The apparatus for preparing a piperidine triazine derivative and amine condensate according to claim 1, characterized in that: A side support (107) is fixedly installed on the base (1), and a rack rod (108) is fixedly installed at the end of the side support (107). A driven gear (702) that meshes with the rack rod (108) is fixed at one end of the main shaft cylinder (7) near the top.

7. The apparatus for preparing a piperidine triazine derivative and amine condensate according to claim 1, characterized in that: The bottom end of the prism (701) is fixedly connected to a pair of side arm columns (9), and each side arm column (9) is fixedly connected to a plurality of symmetrically arranged stirring blocks (901), and the two side arm columns (9) are fixedly connected to a plurality of mesh ring plates (902).

8. The apparatus for preparing a piperidine triazine derivative and amine condensate according to claim 1, characterized in that: A pair of metering pumps (4) are fixedly installed on the base (1). The input ends of the two metering pumps (4) are fixedly connected to the discharge pipes (402), and the output ends of the two metering pumps (4) are fixedly connected to the output pipes (401). The ends of the two output pipes (401) are fixedly connected to an external reactor.

9. The apparatus for preparing a piperidine triazine derivative and amine condensate according to claim 8, characterized in that: An electric control valve is fixedly installed at one end of each of the two discharge pipes (402). The bottom end of the auxiliary tank (2) is fixedly connected to the discharge pipe (402) located at the bottom end. The bottom end of the main tank (3) is rotatably connected to the discharge pipe (402) located at the bottom end. A reinforcing frame is fixed between each of the two discharge pipes (402) and the base (1).

10. A method for preparing a piperidine triazine derivative and amine condensate, wherein the method is applied to the apparatus for preparing the piperidine triazine derivative and amine condensate according to any one of claims 1-9, characterized in that: Includes the following steps: Step 1: Add industrial-grade molybdenum trioxide (25wt%), deionized water (50wt%), and glass beads (25wt%) to a high-efficiency grinder mixing sampler and grind for more than 10 hours. Take samples to test the particle size until the laser particle size analyzer shows that D90 meets the requirements, where D90≤100nm. After grinding, filter the glass beads with sand cloth first, and then filter the filtrate through a 0.1-micron microporous membrane to obtain nano-sized wet catalyst. After drying the wet catalyst, the nano-catalyst is obtained. Step 2: Add the condensate of 2,4-bis[N-butyl-[1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl]amino]-1,3,5-triazine and N,N-bis(3-aminopropyl)ethyl ethylamine (24.9 wt%) to the external feeding system, and add cyclohexane (41.6 wt%) and nano-catalyst (0.2 wt%) to the main tank (3). Use the moving stirring component and the follow-up feeding component to mix the three evenly, and preheat to 90°C; Step 3: Store 80% TBHP (33.3wt%) separately in auxiliary tank (2), and use metering pump (4) to feed the materials from main tank (3) and auxiliary tank (2) into the reactor, control the reaction temperature at 90℃ and the back pressure at 0.5 MPa, and continuously feed the reaction. Step 4: Take samples for testing. If the samples do not meet the standards, continue the reaction until they are qualified. Step 5: After the reaction is complete, cool to 60℃, filter to recover the catalyst, distill the filtrate under normal pressure to recover cyclohexane, then desolvate in a high vacuum in a demelting kettle, and granulate or pulverize to obtain the condensate of 2,4-bis[N-butyl-(1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl)amino]-1,3,5-triazine and N,N-bis(3-aminopropyl)ethylethylamine, with a yield ≥95%.

Citation Information

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