A crude product crystallization device for preparing phosphorus-containing triazine ring flame retardant

Abstract

The utility model discloses a crude product crystallization device for preparation of phosphorus-containing triazine ring flame retardant, including frame and from top to bottom arrange in the frame in dissolving cylinder, filter hopper and crystallizing bottle, be equipped with heat -preserving jacket no.

Description

Technical Field

[0001] This utility model relates to the technical field of crystallization processing equipment, and in particular to a crude crystallization device for preparing phosphorus triazine ring flame retardants. Background Technology

[0002] Triazine ring flame retardants, especially phosphorus-containing triazine ring compounds, have become a research hotspot in the field of halogen-free flame retardants due to their highly efficient phosphorus-nitrogen synergistic flame retardant effect. According to prior art information from patent application number 200710026361.3, 1,3,5-triazine cycloneopentyl glycol phosphate is a representative flame retardant. Its synthesis typically involves the condensation reaction of cyanuric chloride and neopentyl glycol phosphite. After the reaction, the crude product needs to be recrystallized and purified to obtain high-purity white crystals. This recrystallization purification is usually carried out in multiple independent glassware, including heating and dissolving in a flask, hot filtration through a preheated Buchner funnel, and then transferring the filtrate to another container for cooling and crystallization.

[0003] However, this process has many drawbacks: First, transferring hot solutions between multiple unit operations is not only cumbersome, but also prone to premature crystallization of the target product during transfer or on the filter medium due to heat loss, resulting in yield loss and equipment blockage.

[0004] To address these issues, we propose a crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants. Utility Model Content

[0005] The purpose of this invention is to provide a crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants, so as to solve the problems mentioned in the background art.

[0006] To achieve the above objectives, this utility model provides the following technical solution:

[0007] A crude crystallization apparatus for preparing a phosphorus-containing triazine ring flame retardant includes a frame and a dissolving cylinder, a filter bucket, and a crystallization bottle arranged sequentially from top to bottom within the frame. The outer wall of the dissolving cylinder is provided with a first heat-insulating jacket, and the outer wall of the filter bucket is provided with a second heat-insulating jacket. A hot water circulation tank is provided on the side of the frame, and a water pump and a return pipe are installed on the hot water circulation tank. The water pump, the second heat-insulating jacket, the first heat-insulating jacket, and the return pipe are connected sequentially by rubber tubes.

[0008] In a further embodiment, a cylinder cover is installed on the dissolving cylinder by a number of sets of bolts and nuts evenly distributed around the circumference. A stirring motor is installed on the cylinder cover, and the output shaft of the stirring motor passes through the bottom of the cylinder cover and is connected to a stirring rod.

[0009] In a further embodiment, a condenser tube is also installed on the cap, and the condenser tube is connected to the inside of the dissolving cylinder.

[0010] In a further embodiment, a flow regulating valve is installed between the liquid outlet of the dissolving cylinder and the liquid inlet of the filter bucket.

[0011] In a further embodiment, the filter bucket includes a funnel cover and a funnel body that are threaded together, and filter paper that is tightly attached to the inner wall of the funnel body. The inner edge of the funnel body is provided with a stepped platform, and the upper edge of the filter paper is folded onto the stepped platform. A sealing ring is embedded in the lower end face of the funnel cover.

[0012] In a further embodiment, the outlet of the filter bucket is provided with a liquid guide tube, which is inserted into the mouth of the crystallization bottle, and a pad is placed at the bottom of the crystallization bottle.

[0013] In a further embodiment, the hot water circulation tank is also equipped with a heating rod and a temperature sensor, and the heating section of the heating rod and the detection probe of the temperature sensor both extend into the water body. The heating rod and the temperature sensor are electrically connected to an external controller.

[0014] Compared with the prior art, the beneficial effects of this utility model are:

[0015] This invention integrates the three core steps of dissolution, hot filtration, and crystallization into one device, achieving a seamless connection from crude product solution to crystallization filtrate. It avoids the heat loss and product precipitation risks caused by the transfer of hot solution between multiple containers in traditional methods, greatly reduces product loss caused by mid-process crystallization, and effectively improves the yield of the final product.

[0016] This invention, by setting up a hot water circulation system and equipping the dissolving cylinder and filter funnel with heat-insulating jackets, can continuously and uniformly heat and insulate the dissolved hot solution and the channels through which it flows, ensuring that the solution is always kept above its crystallization point before entering the crystallization bottle. This completely solves the problem of funnel blockage caused by cooling in the hot filtration process and ensures the smooth operation of the process. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the structure of this utility model;

[0018] Figure 2 This is a front view cross-sectional structural diagram of the dissolving cylinder, filter bucket, and crystallization bottle of this utility model;

[0019] Figure 3 This utility model Figure 2 A magnified view of the structure at point A in the middle;

[0020] Figure 4 This is a schematic diagram of the arrangement of the hot water circulation tank and rubber pipe of this utility model.

[0021] In the diagram: 1. Frame; 2. Dissolving cylinder; 21. Cylinder cover; 22. Stirring motor; 23. Stirring rod; 24. Condenser; 3. Filter hopper; 31. Funnel cover; 32. Funnel body; 321. Stepped platform; 33. Filter paper; 34. Sealing ring; 4. Crystallization bottle; 5. Insulation jacket one; 6. Insulation jacket two; 7. Hot water circulation tank; 71. Heating rod; 72. Temperature sensor; 8. Water pump; 9. Return pipe; 10. Rubber hose; 11. Flow regulating valve; 12. Liquid guide pipe; 13. Pad; 14. Controller. Detailed Implementation

[0022] In the description of this utility model, it should be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings and are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model. In the description of this utility model, unless otherwise stated, "a plurality of" means two or more.

[0023] In the description of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0024] 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.

[0025] Please see Figure 1-4 A crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants includes a frame 1 for supporting and fixing all components. On the frame 1, a dissolving cylinder 2, a filter hopper 3, and a crystallization bottle 4 are arranged sequentially from top to bottom.

[0026] The dissolving cylinder 2 is a container with an open top. Its outer wall is provided with a hollow heat-insulating jacket 5. The cylinder cover 21 is fastened to the top of the dissolving cylinder 2 by bolts and nuts evenly distributed around the circumference to ensure airtightness. A stirring motor 22 is installed on the cylinder cover 21, and its output shaft extends downward into the cylinder. The end is connected to a stirring rod 23, which is used to stir the material during the dissolving process to promote heat transfer and dissolution. A spherical condenser tube 24 is also installed on the cylinder cover 21. Its lower end is connected to the inside of the dissolving cylinder 2 to return solvent vapor, reduce solvent loss and prevent external moisture from entering.

[0027] The filter funnel 3 is located directly below the dissolving cylinder 2. The filter funnel 3 is composed of a funnel cover 31 and a funnel body 32 connected by threads. The outer wall of the funnel body 32 is also provided with a hollow heat-insulating jacket 6. The inside of the funnel body 32 is provided with a stepped platform 321 to support the filter paper 33. A sealing ring 34 is embedded in the lower end face of the funnel cover 31. When it is tightened with the funnel body 32, it can press the upper edge of the filter paper 33 and form a seal to prevent the solution from leaking from the edge. A flow regulating valve 11 is installed between the liquid outlet of the dissolving cylinder 2 and the liquid inlet of the filter funnel 3 to control the flow rate of the hot solution.

[0028] A hot water circulation tank 7 is provided on the side of the frame 1. A heating rod 71 and a temperature sensor 72 are installed in the tank. They are electrically connected to an external controller 14, which can be installed on the frame 1. The temperature sensor 72 monitors the water temperature and feeds it back to the controller 14. The controller 14 controls the heating power of the heating rod 71 to facilitate the control of the hot water temperature. The inlet of the water pump 8 is connected to the hot water circulation tank 7, and its outlet is connected to the inlet of the insulation jacket 2 6 through a rubber tube 10. The outlet of the insulation jacket 2 6 is connected to the inlet of the insulation jacket 1 5 through another rubber tube 10. Finally, the outlet of the insulation jacket 1 5 is connected to the return pipe 9 of the hot water circulation tank 7 through another rubber tube 10. This forms a complete closed-loop hot water circulation system, providing a stable heat source for dissolution and filtration.

[0029] The outlet of the filter hopper 3 is connected to a liquid guide tube 12, which is directly inserted into the mouth of the bottom crystallization bottle 4, so that the filtrate can flow directly into the bottle. A pad 13 is placed at the bottom of the crystallization bottle 4 to stabilize the bottle body. Afterwards, by removing the pad 13, the height of the crystallization bottle 4 can be lowered and detached from the liquid guide tube 12, making it easy to remove the crystallization bottle 4.

[0030] Workflow: First, unscrew the filter hopper 3, place the filter paper 33 inside, and then tighten it again. Add the crude product and an appropriate amount of anhydrous ethanol to the dissolving cylinder 2, and then tighten the cylinder cap 21. Set the temperature of the hot water circulation tank 7 through the controller 14. The temperature is usually higher than the boiling point of the solvent. Start the water pump 8 and the heating rod 71. The hot water begins to circulate in the insulation jacket 1 5 and the insulation jacket 2 6. At the same time, start the stirring motor 22 to heat and stir the mixture until the crude product is completely dissolved, forming a clear hot solution. Slowly open the flow regulating valve 11. The hot solution flows into the preheated filter hopper 3 under the action of gravity. Under the action of the insulation jacket 2 6, the solution maintains a high temperature during the filtration process. Insoluble impurities are trapped by the filter paper 33. The clear hot filtrate flows directly into the crystallization bottle 4 below through the liquid guide pipe 12. After all the solutions have been filtered, remove the crystallization bottle 4 and let the filtrate in the crystallization bottle 4 cool slowly to room temperature in a static state, thereby precipitating pure target product crystals.

[0031] It will be apparent to those skilled in the art that this invention is not limited to the details of the exemplary embodiments described above, and that it can be implemented in other specific forms without departing from the spirit or essential characteristics of this invention. Therefore, the embodiments should be considered illustrative and non-limiting in all respects, and the scope of this invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within this invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0032] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants, characterized in that: The equipment includes a frame (1) and a dissolving cylinder (2), a filter bucket (3) and a crystallization bottle (4) arranged from top to bottom in the frame (1). The outer wall of the dissolving cylinder (2) is provided with a heat insulation jacket (5), and the outer wall of the filter bucket (3) is provided with a heat insulation jacket (6). A hot water circulation tank (7) is provided on the side of the frame (1). A water pump (8) and a return pipe (9) are installed on the hot water circulation tank (7). The water pump (8), the second heat insulation jacket (6), the first heat insulation jacket (5) and the return pipe (9) are connected in sequence by a rubber tube (10).

2. The crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants according to claim 1, characterized in that: The dissolving cylinder (2) is fitted with a cylinder cover (21) by several sets of bolts and nuts evenly distributed around the circumference. A stirring motor (22) is installed on the cylinder cover (21), and the output shaft of the stirring motor (22) passes through the bottom of the cylinder cover (21) and is connected to a stirring rod (23).

3. The crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants according to claim 2, characterized in that: A condenser tube (24) is also installed on the cap (21), and the condenser tube (24) is connected to the inside of the dissolving cylinder (2).

4. The crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants according to claim 1, characterized in that: A flow regulating valve (11) is installed between the liquid outlet of the dissolving cylinder (2) and the liquid inlet of the filter bucket (3).

5. The crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants according to claim 1, characterized in that: The filter funnel (3) includes a funnel cover (31) and a funnel body (32) that are threaded together, and a filter paper (33) that is tightly attached to the inner wall of the funnel body (32). The inner edge of the funnel body (32) is provided with a stepped platform (321), and the upper edge of the filter paper (33) is pressed onto the stepped platform (321). A sealing ring (34) is embedded in the lower end face of the funnel cover (31).

6. The crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants according to claim 1, characterized in that: The outlet of the filter bucket (3) is provided with a liquid guide tube (12), which is inserted into the mouth of the crystallization bottle (4). A pad (13) is placed at the bottom of the crystallization bottle (4).

7. The crude crystallization apparatus for preparing phosphorus-containing triazine ring flame retardants according to claim 1, characterized in that: The hot water circulation tank (7) is also equipped with a heating rod (71) and a temperature sensor (72), and the heating section of the heating rod (71) and the detection probe of the temperature sensor (72) are both inserted into the water body. The heating rod (71) and the temperature sensor (72) are electrically connected to an external controller (14).

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