DMAP finished product anti-caking treatment device

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By designing a finished DMAP anti-caking treatment device, using the cooling water area and steam area to control temperature and gas flow, the problem of DMAP being easily condensed into blocks in industrial preparation is solved, and the stable powder storage of DMAP is achieved.

CN222969226UActive Publication Date: 2025-06-13YUMEN KEHAO CATALYTIC MATERIALS CO LTD

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Patent Information

Application Number: CN202422179150.5
Authority / Receiving Office: CN · China
Patent Type: Utility models(China)
Current Assignee / Owner
Filing Date: 2024-09-05
Publication Date: 2025-06-13
Estimated Expiration: 2034-09-05

AI Technical Summary

Technical Problem

Existing laboratory equipment is not suitable for industrial preparation of DMAP, which makes DMAP easy to condense into blocks and difficult to maintain powder form.

Method used

A DMAP finished product anti-caking treatment device is designed, including a crystallization tank and a drying tank. By setting a cooling water area outside the crystallization tank and a steam area outside the drying tank, temperature and gas flow are controlled to prevent DMAP from condensing.

Benefits of technology

Effectively prevent DMAP from condensing into blocks, keeping it in powder form, making it easy to disassemble and store, and is suitable for industrial preparation.

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Abstract

The utility model relates to the technical field of chemical product drying and storage, in particular to a DMAP finished product anti-caking treatment device which comprises a crystallizing tank and a drying tank, the upper portion of one side of the crystallizing tank is fixedly connected with a first oxygen outlet pipe, and the lower portion of one side of the crystallizing tank is fixedly connected with a first carbon dioxide outlet pipe. The middle of the other side of the crystallizing tank is fixedly connected with a nitrogen inlet pipe, the upper portion of the crystallizing tank is fixedly connected with a filtrate inlet pipe, the lower end of the crystallizing tank is fixedly connected with a three-way pipe, and one end of the crystallizing tank is communicated with the drying tank. A second oxygen outlet pipe is fixedly connected to the upper portion of one side of the drying tank, a second carbon dioxide outlet pipe is fixedly connected to the lower portion of one side of the drying tank, a steam inlet pipe and a steam outlet pipe are fixedly connected to the two sides of the second heat preservation tank respectively, and a fixed disc is fixedly connected into the material collecting groove and rotationally connected with the rotating disc through a grinding navel. The device disclosed by the utility model can be suitable for industrial preparation, and the DMAP can be kept in a powdery state after being treated and is not condensed into blocks any more.

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Description

Technical Field

[0001] The utility model relates to the technical field of drying and storage of chemical products, in particular to an anti-caking treatment device for DMAP finished products. Background Art

[0002] Acylation reaction is one of the most common chemical reactions. The initial acylation catalyst was pyridine, but for substrates with high steric hindrance and low activity, the results were often unsatisfactory. In 1967, Litvinenko and Kirichenko found that when using 4-dimethylaminopyridine (hereinafter referred to as DMAP) instead of pyridine in the study of benzoylation of m-chloroaniline, the reaction rate increased by 104-105 times. Subsequently, it was found that the conjugation of the electron-donating dimethylamino group in DMAP with the pyridine ring can strongly activate the nitrogen atom on the ring for nucleophilic substitution reactions, thereby increasing the reaction rate and yield. Due to its remarkable catalytic effect, it is known as the "super catalyst" of acylation reactions and has been widely used in many fields of fine chemistry. DMAP is an excellent acylation catalyst, with a light yellow powder or crystal appearance, relatively stable, and can be stored at room temperature. However, the prepared DMAP at this time is very easy to agglomerate into lumps. To maintain its morphological stability, the laboratory often uses the method of introducing a protective gas such as nitrogen to keep the prepared DMAP in powder form. However, the equipment used in the laboratory is not suitable for industrial preparation. Therefore, an anti-caking treatment device for DMAP finished products that can adapt to industrial preparation and keep DMAP in powder form and no longer agglomerate after treatment is needed. Summary of the Utility Model

[0003] Aiming at the above technical problems, the utility model provides an anti-caking treatment device for DMAP finished products that can adapt to industrial preparation and keep DMAP in powder form and no longer agglomerate after treatment, so as to solve problems such as the inapplicability of existing laboratory equipment to industrial preparation.

[0004] To solve the above technical problems, a DMAP finished product anti-caking treatment device described in the present utility model includes a crystallization tank and a drying tank. One upper part of one side of the crystallization tank is fixedly connected to a first oxygen outlet pipe, and one lower part is fixedly connected to a first carbon dioxide outlet pipe. One middle part of the other side of the crystallization tank is fixedly connected to a nitrogen inlet pipe, and one upper part is fixedly connected to a filtrate inlet pipe. The lower end of the crystallization tank is fixedly connected to the main pipe of a three-way pipe. One branch pipe of the three-way pipe is communicated with a liquid collecting bottle, and the other branch pipe is communicated with the drying tank. Inside the drying tank, an aggregate hopper, a material guiding hopper, and an aggregate trough are fixedly connected in sequence from top to bottom. One upper part of one side of the drying tank is fixedly connected to a second oxygen outlet pipe, and one lower part is fixedly connected to a second carbon dioxide outlet pipe. The outer sides of the crystallization tank and the drying tank are respectively fixedly connected to a first heat preservation tank and a second heat preservation tank. The upper and lower ends of the first heat preservation tank are respectively fixedly connected to a cooling water inlet pipe and a cooling water outlet pipe. The two sides of the second heat preservation tank are respectively fixedly connected to a steam inlet pipe and a steam outlet pipe. An immovable disk is fixedly connected inside the aggregate trough. The immovable disk is rotationally connected to a rotating disk through a grinding navel. The upper part of the grinding navel is fixedly connected to a connecting rod. The upper end of the grinding navel passes through a support frame and is connected to the output end of a grinding disk motor. One side of the rotating disk is fixedly connected to a fixed rod, and the fixed rod is fixedly connected to the connecting rod.

[0005] Further, a stirring shaft is arranged in the crystallization tank. A stirring blade is fixedly connected to the lower part of the stirring shaft. The upper part of the stirring shaft penetrates through the crystallization tank and the first heat preservation tank, and the upper end of the stirring shaft is connected to the output end of a stirring motor.

[0006] Further, a U-shaped rod is fixedly connected to the inner wall of the drying tank. Rotating shafts are respectively rotationally connected to both sides of the U-shaped rod. One end of each rotating shaft is fixedly connected to an eccentric wheel, and the other end is connected to the output end of an eccentric wheel motor. A connecting rod is fixedly connected to the eccentric wheel, and the connecting rod is fixedly connected to a baffle plate. The baffle plate is located below the aggregate hopper.

[0007] Further, a reinforcing rib is fixedly connected between the grinding navel and the connecting rod.

[0008] Further, a feed inlet is formed in the rotating disk.

[0009] Further, a valve is fixedly connected between the main pipe and the branch pipe of the three-way pipe.

[0010] The present utility model has the following advantages compared with the prior art:

[0011] By arranging a first heat preservation tank outside the crystallization tank to form a cooling water area to maintain a low temperature state inside the crystallization tank, accelerating the crystallization of the filtrate through the stirring shaft and the stirring blade, arranging a second heat preservation tank outside the drying tank to form a steam area to maintain a high temperature environment inside the drying tank, discharging the evaporated solvent and nitrogen together through the second oxygen outlet pipe for unified recovery to avoid environmental pollution, and grinding the dried falling crystals into powder by the rotating disk and the immovable disk, which is convenient for sub-packaging and storage. Brief Description of the Drawings

[0012] Figure 1 This is a schematic structural view of the present utility model.

[0013] Figure 2 This is a sectional view of the aggregate chute and the stationary disk structure of the present utility model.

[0014] Figure 3 This is a schematic view of the connection structure between the U-shaped rod and the baffle of the present utility model.

[0015] In the figure: 1, crystallization tank; 2, drying tank; 3, first heat preservation tank; 4, cooling water area; 5, cooling water inlet pipe; 6, cooling water outlet pipe; 7, nitrogen inlet pipe; 8, first oxygen outlet pipe; 9, first carbon dioxide outlet pipe; 10, filtrate inlet pipe; 11, three-way pipe; 12, second heat preservation tank; 13, steam area; 14, steam inlet pipe; 15, steam outlet pipe; 16, second oxygen outlet pipe; 17, second carbon dioxide outlet pipe; 18, aggregate hopper; 19, baffle; 20, U-shaped rod; 21, material guiding hopper; 22, grinding disc motor; 23, grinding navel; 24, reinforcing rib; 25, connecting rod; 26, fixed rod; 27, rotating disk; 28, aggregate chute; 29, stationary disk; 30, connecting rod; 31, eccentric wheel; 32, eccentric wheel motor; 33, rotating shaft; 34, stirring motor; 35, stirring shaft; 36, stirring blade; 37, support frame. Detailed Description of the Preferred Embodiments

[0016] The following further describes the present utility model with reference to the drawings.

[0017] As Figure 1 , 2, A DMAP finished product anti-caking treatment device shown in Figures 3, including a crystallization tank 1 and a drying tank 2. In order to exhaust the original gas in the tank, a first oxygen outlet pipe 8 is fixedly connected to the upper part of one side of the crystallization tank 1, and a first carbon dioxide outlet pipe 9 is fixedly connected to the lower part. A nitrogen inlet pipe 7 is fixedly connected to the middle part of the other side of the crystallization tank 1, and a filtrate inlet pipe 10 is fixedly connected to the upper part. The lower end of the crystallization tank 1 is fixedly connected to the main pipe of a three-way pipe 11. One branch pipe of the three-way pipe 11 is communicated with a liquid collecting bottle, and the other branch pipe is communicated with the drying tank 2. Inside the drying tank 2, an aggregate hopper 18, a material guiding hopper 21, and an aggregate trough 28 are fixedly connected in sequence from top to bottom. A second oxygen outlet pipe 16 is fixedly connected to the upper part of one side of the drying tank 2, and a second carbon dioxide outlet pipe 17 is fixedly connected to the lower part. In order to provide temperature control and maintenance, a first heat preservation tank 3 and a second heat preservation tank 12 are respectively fixedly connected to the outside of the crystallization tank 1 and the drying tank 2. A cooling water inlet pipe 5 and a cooling water outlet pipe 6 are respectively fixedly connected to the upper and lower ends of the first heat preservation tank 3. A steam inlet pipe 14 and a steam outlet pipe 15 are respectively fixedly connected to both sides of the second heat preservation tank 12. In order to grind the dried crystals into powder, a fixed disk 29 is fixedly connected inside the aggregate trough 28. The fixed disk 29 is rotationally connected to a rotating disk 27 through a grinding navel 23. The upper part of the grinding navel 23 is fixedly connected to a connecting rod 25. The upper end of the grinding navel 23 passes through a support frame 37 and is connected to the output end of a grinding disk motor 22. A fixed rod 26 is fixedly connected to one side of the rotating disk 27. The fixed rod 26 is fixedly connected to the connecting rod 25.

[0018] In order to accelerate the crystallization speed of the filtrate, a stirring shaft 35 is arranged in the crystallization tank 1. A stirring blade 36 is fixedly connected to the lower part of the stirring shaft 35. The upper part of the stirring shaft 35 penetrates through the crystallization tank 1 and the first heat preservation tank 2. The upper end of the stirring shaft 35 is connected to the output end of a stirring motor 34.

[0019] In order to prevent the crystals from falling when they are not dried, U-shaped rods 20 are fixedly connected to the inner wall of the drying tank 2. Rotating position shafts 33 are respectively rotationally connected to both sides of the U-shaped rods 20. One end of the rotating shaft 33 is fixedly connected to an eccentric wheel 31, and the other end is connected to the output end of an eccentric wheel motor 32. A connecting rod 30 is fixedly connected to the eccentric wheel 31. The connecting rod 30 is fixedly connected to a baffle 19. The baffle 19 is located below the aggregate hopper 18.

[0020] In order to prevent the grinding navel 23 and the connecting rod 25 from being fixedly connected during the rotation of the rotating disk 27, a reinforcing rib 24 is fixedly connected between them.

[0021] In order to facilitate the feeding of crystals, a feeding port is provided on the rotating disk 27.

[0022] In order to facilitate the separate treatment of the products in the crystallization tank after crystallization, a valve is fixedly connected between the main pipe and the branch pipe of the three-way pipe 11.

[0023] In order to facilitate the observation of the crystallization process in the crystallization tank 1, observation windows are provided on the first heat preservation tank 3 and the crystallization tank 1.

[0024] To facilitate the extraction of the ground DMAP finished product, the second heat preservation tank 12 and the lower part of the drying tank 2 are hermetically hinged with tank doors.

[0025] The working process of this embodiment is as follows:

[0026] Take light yellow DMAP crude product, add organic solvent to dissolve, add activated carbon for decolorization, and take the filtrate for standby. Pass nitrogen from the nitrogen inlet pipe 7 into the crystallization tank 1. The nitrogen enters the drying tank 2 through one port of the three-way pipe 11. After nitrogen is introduced for a certain period of time, place a safely burning flame at the ends of the first oxygen outlet pipe 8 and the second oxygen outlet pipe 16, and place clear lime water at the first carbon dioxide outlet pipe 9 and the second carbon dioxide outlet pipe 17. When the flame goes out, close the first oxygen outlet pipe 8 and the second oxygen outlet pipe 16. After the clear lime water does not become turbid, close the first carbon dioxide outlet pipe 9 and the second carbon dioxide outlet pipe 17, and stop introducing nitrogen. Pass cooling water from the cooling water inlet pipe 5 into the cooling water area 4 and then leave through the cooling water outlet pipe 6 to form a cycle. When the temperature in the crystallization tank 1 drops to 0 °C, let the standby filtrate enter the crystallization tank 1 through the filtrate inlet pipe 10. Turn on the stirring motor 34 to make the stirring shaft 35 and the stirring blades 36 rotate to accelerate the crystallization of the filtrate. After observing the completion of crystallization through the viewing window, turn the valve of the three-way pipe 11 to make the secondary filtrate enter the collecting bottle. After the secondary filtrate is concentrated, it enters the crystallization tank 1 again through the filtrate inlet pipe 10 for crystallization to achieve the maximum utilization rate of the filtrate. After the secondary filtrate has drained out, turn the valve of the three-way pipe 11 to make the crystal enter the collecting hopper 18 of the drying tank 2 from the other end. Pass the hot steam from the steam inlet pipe 14 into the steam area 13 and then leave through the steam outlet pipe 15 to form a cycle. At this time, continue to introduce nitrogen from the nitrogen inlet pipe 7 and open the second oxygen outlet pipe 16 to make nitrogen circulate in the crystallization tank 1 and the drying tank 2. At this time, set a nitrogen collection device at the second oxygen outlet pipe 16. After drying is completed, turn on the eccentric wheel motor 32 to make the eccentric wheel 31 rotate, drive the connecting rod 30 and the baffle 19 to translate, expose the lower outlet of the collecting hopper 18, and make the dried crystal fall into the lower guiding hopper 21 and enter the feeding port of the rotating disk 27 through the guiding hopper 21. Turn on the grinding disk motor 22 to drive the connecting rod 25 and the fixed rod 26 to rotate, thereby making the rotating disk 27 rotate. Under the action of the rotating disk 27 and the stationary disk 29, the crystal is ground into powder. The crystal powder falls into the collecting trough 28. After drying and grinding are completed, stop introducing steam and nitrogen. After the steam and nitrogen are exhausted, open the tank doors on the second heat preservation tank 12 and the drying tank 2, take out the powder, bottle it, and store it.

Claims

1. A DMAP finished product anti-caking treatment device, comprising a crystallization tank (1) and a drying tank (2), characterized in that: The upper part of one side of the crystallizer (1) is fixedly connected to a first oxygen outlet pipe (8), and the lower part is fixedly connected to a first carbon dioxide outlet pipe (9); the middle part of the other side of the crystallizer (1) is fixedly connected to a nitrogen inlet pipe (7), and the upper part is fixedly connected to a filtrate inlet pipe (10); the lower end of the crystallizer (1) is fixedly connected to a main pipe of a three-way pipe (11); one branch of the three-way pipe (11) is connected to a liquid collecting bottle, and the other branch is connected to the drying tank (2); the drying tank (2) is fixedly connected with a collecting hopper (18), a guide hopper (21), and a collecting trough (28) in sequence from top to bottom; the upper part of one side of the drying tank (2) is fixedly connected to a second oxygen outlet pipe (16), and the lower part is fixedly connected to a second carbon dioxide outlet pipe (17); the outer sides of the crystallizer (1) and the drying tank (2) are respectively fixedly connected to the main pipe of a three-way pipe (11); A first heat-insulating tank (3) and a second heat-insulating tank (12) are connected; the first heat-insulating tank (3) is respectively fixedly connected with a cooling water inlet pipe (5) and a cooling water outlet pipe (6) at the upper and lower ends; the second heat-insulating tank (12) is respectively fixedly connected with a steam inlet pipe (14) and a steam outlet pipe (15) at both sides; a fixed disk (29) is fixedly connected in the collecting trough (28); the fixed disk (29) is rotatably connected to the rotating disk (27) through a grinding navel (23); the upper part of the grinding navel (23) is fixedly connected to a connecting rod (25); the upper end of the grinding navel (23) passes through a supporting frame (37) and is connected to the output end of a grinding disc motor (22); one side of the rotating disk (27) is fixedly connected with a fixing rod (26); the fixing rod (26) is fixedly connected to the connecting rod (25).

2. The device for preventing agglomeration of a DMAP finished product according to claim 1, characterized in that: The crystallization tank (1) is provided with a stirring shaft (35), the lower part of the stirring shaft (35) is fixedly connected to a stirring blade (36), the upper part of the stirring shaft (35) passes through the crystallization tank (1) and the first heat preservation tank (3), and the upper end of the stirring shaft (35) is connected to the output end of the stirring motor (34).

3. The anti-caking treatment device for DMAP finished product according to claim 1, characterized in that: A U-shaped rod (20) is fixedly connected to the inner wall of the drying tank (2), and rotating shafts (33) are rotatably connected to both sides of the U-shaped rod (20), one end of the rotating shaft (33) is fixedly connected to the eccentric wheel (31), and the other end is connected to the output end of the eccentric wheel motor (32), and a connecting rod (30) is fixedly connected to the eccentric wheel (31), and the connecting rod (30) is fixedly connected to the baffle (19), and the baffle (19) is located below the collecting hopper (18).

4. The device for preventing agglomeration of a DMAP finished product according to claim 1, characterized in that: A reinforcing rib (24) is fixedly connected between the grinding navel (23) and the connecting rod (25).

5. The device for preventing agglomeration of a DMAP finished product according to claim 1, characterized in that: The rotating disk (27) is provided with a feed inlet.

6. The device for preventing agglomeration of a DMAP finished product according to claim 1, characterized in that: A valve is fixedly connected between the main pipe and the branch pipe of the three-way pipe (11).