Microchannel apparatus for amination reactions

Abstract

The utility model belongs to the technical field of reaction device, concretely relates to a kind of microchannel device of ammoniation reaction, including ammonia liquid tank, ammonia liquid tank is connected with reactor, reactor is connected with raw material tank, reactor bottom is connected with product storage tank, pH detector is arranged between reactor and product storage tank, pH detector is connected with controller, controller is electrically connected with the peristaltic pump one between reactor and ammonia liquid tank and the peristaltic pump two between reactor and raw material tank, peristaltic pump three and peristaltic pump four;Reactor is internally provided with several pear-shaped microchannels, several pear-shaped microchannels are sequentially connected in head and tail, and several pear-shaped microchannels are divided into three groups and are connected by first feed pipe, second feed pipe and third feed pipe.The utility model realizes continuous microchannel reaction by the microchannel device of ammoniation reaction, can effectively improve ammoniation selectivity and purity in aluminium phosphonate production process, and simultaneously improves the production capacity and quality of aluminium phosphonate product.

Description

Technical Field

[0001] This invention belongs to the field of reaction device technology, specifically relating to a microchannel device for ammoniation reaction. Background Technology

[0002] The ammonia chemical section of the traditional ethylphosphine aluminum process is operated intermittently, requiring the addition of excess ammonia water. The molar ratio of ethylphosphine aluminum to ammonia water is 1:1.2, and the process takes more than 9 hours, severely restricting production efficiency and product quality. Furthermore, the crude reaction conditions result in a raw material utilization rate of less than 80%, with unreacted ammonia water being wasted. Strict pH control within the range of 8±0.2 is also necessary. When pH > 9, aluminum ions easily hydrolyze to form aluminum hydroxide precipitate during metathesis, while pH < 7 leads to incomplete ammoniation, resulting in high levels of residual phosphite byproducts, directly affecting the stability of subsequent metathesis reactions. This crude pH control further exacerbates side reactions; manual adjustment relies on experience and has a delayed response, failing to accurately avoid the risk of aluminum ion hydrolysis.

[0003] Secondly, safety and environmental issues are prominent. When the liquid holding capacity of traditional reactors increases, the accumulated ammonia and ethanol vapors in the system increase the risk of explosion. These defects make traditional processes lag behind continuous microchannel technology in terms of production efficiency, environmental protection, and reaction controllability. Utility Model Content

[0004] In view of the shortcomings of the prior art, the technical problem to be solved by this utility model is to provide a microchannel device for ammoniation reaction, which improves the yield and purity of finished product, reduces the content of phosphorous acid, adjusts the feed amount of raw materials by the change of pH value in the product, and reduces labor costs and safety.

[0005] The technical solution adopted by this utility model to solve its technical problem is:

[0006] The microchannel device for ammoniation reaction described in this utility model includes an ammonia tank, a reactor connected to the ammonia tank, a raw material tank connected to the reactor, a product storage tank connected to the bottom of the reactor, a pH detector installed between the reactor and the product storage tank, a controller connected to the pH detector, and a peristaltic pump connected electrically to a peristaltic pump 1 between the reactor and the ammonia tank, and peristaltic pumps 2, 3 and 4 between the reactor and the raw material tank. The reactor contains a plurality of pear-shaped microchannels connected end to end, and the pear-shaped microchannels are divided into three groups, which are connected by a first feed pipe, a second feed pipe and a third feed pipe, respectively.

[0007] in:

[0008] The first, second, and third feed pipes are all connected to the raw material tank.

[0009] A peristaltic pump 2 is installed between the first feed pipe and the raw material tank; a peristaltic pump 3 is installed between the second feed pipe and the raw material tank; and a peristaltic pump 4 is installed between the third feed pipe and the raw material tank.

[0010] The pear-shaped microchannel includes a large opening and a small opening. Several pear-shaped microchannels connected in sequence have an inlet pipe at the large opening end and an outlet pipe at the small opening end.

[0011] The inlet pipe is connected to the ammonia tank, and the outlet pipe is connected to the product storage tank.

[0012] A peristaltic pump is installed between the inlet pipe and the ammonia tank.

[0013] The pear-shaped microchannel is provided with a delivery pipe, one end of which is connected to the inside of the small opening of the pear-shaped microchannel, and the diameter of the connection between the delivery pipe and the pear-shaped microchannel is smaller than the diameter of the delivery pipe.

[0014] The other end of the conveying pipe is provided with a connecting pipe, which is arranged in a U-shape and the bottom end of the connecting pipe is connected to the conveying pipe.

[0015] The connecting pipe has a short pipe vertically installed at the end away from the conveying pipe, and the top of the short pipe is connected to the first feed pipe, the second feed pipe or the third feed pipe.

[0016] The delivery pipe and the connecting pipe are connected perpendicularly.

[0017] The beneficial effects of this utility model are:

[0018] In this invention, the pear-shaped microchannel adopts a segmented, grouped structure, with an independent peristaltic pump at the inlet of each group of esterification solutions. Combined with real-time monitoring by a pH-linked controller, the pH value of the reaction solution can be strictly controlled within an extremely narrow range of ±0.1. This operation changes the traditional, extensive mode of one-time feeding and avoids side reactions caused by local over-acidity and aluminum sulfate hydrolysis during metathesis due to local over-alkaliness by staged feeding.

[0019] The pear-shaped microchannel achieves forced backmixing through a symmetrical flow channel design, making it particularly suitable for the synergistic use of fully mixed structures containing high-viscosity materials such as diethyl phosphite. This can reduce the ammoniation reaction time from the traditional 3 hours and minutes to 90 seconds, while increasing the product purity from 96% to 98.5%.

[0020] The reactor employs three reaction units connected in series, each capable of independently controlling the flow rate and mixing intensity of the esterification liquid. When production expansion is required, simply increasing the number of units in the existing units linearly increases capacity, improving equipment utilization. If the pear-shaped microchannels in a unit become blocked or corroded, the individual unit can be replaced without a complete shutdown, reducing maintenance costs. Traditional processes require several hours of downtime for cleaning, while this invention allows for restoration of operation within 2 hours by replacing the faulty structure, significantly minimizing production losses.

[0021] This invention utilizes a microchannel device for the ammoniation reaction, achieving a continuous microchannel reaction that effectively improves the selectivity and purity of ammoniation in the production process of ethyl phosphonate aluminum, while simultaneously increasing the production capacity and quality of the ethyl phosphonate aluminum product. Furthermore, by adding esterification solution three times, the pH value during ammoniation is stabilized, side reactions are reduced, and the phosphorous acid content in the product is significantly decreased. This invention can increase the product yield to over 95.3% and the purity to over 98%, offering the advantages of high yield and high purity, while reducing the phosphorous acid content in the product from 1.0% to 0.2%. Attached Figure Description

[0022] Figure 1 This is a schematic diagram of the structure of this utility model;

[0023] Figure 2 This is a schematic diagram of the pear-shaped microchannel structure of this utility model;

[0024] Figure 3 This is a schematic diagram of the pear-shaped micro-through cross-sectional structure of this utility model.

[0025] In the diagram: 1. Ammonia tank; 2. Raw material tank; 3. Peristaltic pump one; 4. Peristaltic pump two; 5. Peristaltic pump three; 6. Peristaltic pump four; 7. Reactor; 8. Controller; 9. pH detector; 10. Product storage tank; 701. First feed pipe; 702. Inlet pipe; 703. Second feed pipe; 704. Third feed pipe; 705. Outlet pipe; 706. Pear-shaped microchannel; 7061. Connecting pipe; 7062. Delivery pipe. Detailed Implementation

[0026] The embodiments of this utility model will be further described below with reference to the accompanying drawings.

[0027] Example 1

[0028] like Figure 1-3As shown, the microchannel device for ammoniation reaction of this utility model includes an ammonia tank 1, a reactor 7 connected to the ammonia tank 1, a raw material tank 2 connected to the reactor 7, a product storage tank 10 connected to the bottom of the reactor 7, a pH detector 9 installed between the reactor 7 and the product storage tank 10, a controller 8 connected to the pH detector 9, and a peristaltic pump 3 connected to the reactor 7 and the ammonia tank 1, as well as peristaltic pumps 4, 5, and 6 connected to the reactor 7 and the raw material tank 2. The reactor 7 has a plurality of pear-shaped microchannels 706 installed inside, which are connected end to end and divided into three groups, which are connected through a first feed pipe 701, a second feed pipe 703, and a third feed pipe 704, respectively.

[0029] The first feed pipe 701, the second feed pipe 703, and the third feed pipe 704 are all connected to the raw material tank 2.

[0030] A peristaltic pump 4 is installed between the first feed pipe 701 and the raw material tank 2; a peristaltic pump 5 is installed between the second feed pipe 703 and the raw material tank 2; and a peristaltic pump 6 is installed between the third feed pipe 704 and the raw material tank 2.

[0031] The pear-shaped microchannel 706 includes a large opening and a small opening. The large opening of the pear-shaped microchannels 706 connected in sequence is provided with an inlet pipe 702, and the small opening of the pear-shaped microchannels 706 connected in sequence is provided with an outlet pipe 705.

[0032] The inlet pipe 702 is connected to the ammonia tank 1, and the outlet pipe 705 is connected to the product storage tank 10.

[0033] A peristaltic pump 3 is installed between the inlet pipe 702 and the ammonia tank 1.

[0034] A delivery pipe 7062 is provided on the pear-shaped microchannel 706. One end of the delivery pipe 7062 is connected to the inner side of the small opening end of the pear-shaped microchannel 706, and the diameter of the connection between the delivery pipe 7062 and the pear-shaped microchannel 706 is smaller than the diameter of the delivery pipe 7062.

[0035] The other end of the conveying pipe 7062 is provided with a connecting pipe 7061. The connecting pipe 7061 is arranged in a U-shape, and the bottom end of the connecting pipe 7061 is connected to the conveying pipe 7062.

[0036] A short pipe is vertically installed at the end of the connecting pipe 7061 away from the conveying pipe 7062, and the top of the short pipe is connected to the first feed pipe 701, the second feed pipe 703 or the third feed pipe 704.

[0037] The delivery pipe 7062 is perpendicularly connected to the connecting pipe 7061.

[0038] Working principle and process:

[0039] During the ammoniation reaction, a certain concentration of ammonia water is added to the ammonia tank 1 and then transported to the reactor 7. Subsequently, the esterification liquid in the raw material tank 2 is slowly added to the reactor 7 through the first feed pipe 701, the second feed pipe 703, and the third feed pipe 704. The ammonia water and the esterification liquid mix and react in the pear-shaped microchannels 706 inside the reactor 7. The ammonia water enters from the large end of the pear-shaped microchannel 706, where the flow rate is relatively slow. The esterification liquid and ammonia water meet and mix at the small end of the pear-shaped microchannel 706. Then, through a slow reaction, each pear-shaped microchannel 706 reacts individually and is interconnected, ensuring that the amount of esterification liquid added each time reacts exactly with the ammonia water. The quality of the resulting product can be effectively controlled. The pH value is monitored in real time by the pH detector 9, and the ammonia water feed rate, as well as the feed rate and flow rate of the esterification liquid, are adjusted by the controller 8 until the pH value of the resulting product meets the production requirements. The product is then transported to the product storage tank 10 for storage.

Claims

1. A microchannel device for an ammoniation reaction, comprising an ammonia tank (1), characterized in that, Ammonia tank (1) is connected to reactor (7), reactor (7) is connected to raw material tank (2), and product storage tank (10) is connected to the bottom of reactor (7). A pH detector (9) is installed between reactor (7) and product storage tank (10). The pH detector (9) is connected to controller (8). Controller (8) is electrically connected to peristaltic pump one (3) between reactor (7) and ammonia tank (1), and peristaltic pump two (4), peristaltic pump three (5) and peristaltic pump four (6) between reactor (7) and raw material tank (2). A number of pear-shaped microchannels (706) are installed inside reactor (7). The pear-shaped microchannels (706) are connected end to end. The pear-shaped microchannels (706) are divided into three groups and are connected through first feed pipe (701), second feed pipe (703) and third feed pipe (704) respectively.

2. The microchannel device for ammoniation reaction according to claim 1, characterized in that, The first feed pipe (701), the second feed pipe (703), and the third feed pipe (704) are all connected to the raw material tank (2).

3. The microchannel device for ammoniation reaction according to claim 2, characterized in that, A peristaltic pump 2 (4) is installed between the first feed pipe (701) and the raw material tank (2), a peristaltic pump 3 (5) is installed between the second feed pipe (703) and the raw material tank (2), and a peristaltic pump 4 (6) is installed between the third feed pipe (704) and the raw material tank (2).

4. The microchannel device for ammoniation reaction according to claim 1, characterized in that, The pear-shaped microchannel (706) includes a large opening and a small opening. The large opening of the pear-shaped microchannel (706) connected in sequence is provided with an inlet pipe (702), and the small opening of the pear-shaped microchannel (706) connected in sequence is provided with an outlet pipe (705).

5. The microchannel device for ammoniation reaction according to claim 4, characterized in that, The inlet pipe (702) is connected to the ammonia tank (1), and the outlet pipe (705) is connected to the product storage tank (10).

6. The microchannel device for ammoniation reaction according to claim 5, characterized in that, A peristaltic pump (3) is installed between the inlet pipe (702) and the ammonia tank (1).

7. The microchannel device for ammoniation reaction according to claim 4, characterized in that, A delivery pipe (7062) is provided on the pear-shaped microchannel (706). One end of the delivery pipe (7062) is connected to the inner side of the small opening of the pear-shaped microchannel (706), and the diameter of the connection between the delivery pipe (7062) and the pear-shaped microchannel (706) is smaller than the diameter of the delivery pipe (7062).

8. The microchannel device for ammoniation reaction according to claim 7, characterized in that, The other end of the conveying pipe (7062) is provided with a connecting pipe (7061). The connecting pipe (7061) is arranged in a U-shape, and the bottom end of the connecting pipe (7061) is connected to the conveying pipe (7062).

9. The microchannel device for ammoniation reaction according to claim 8, characterized in that, A short pipe is vertically installed at the end of the connecting pipe (7061) away from the conveying pipe (7062), and the top of the short pipe is connected to the first feed pipe (701), the second feed pipe (703) or the third feed pipe (704).

10. The microchannel device for ammoniation reaction according to claim 8, characterized in that, The delivery pipe (7062) is perpendicularly connected to the connecting pipe (7061).

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