Aminopropyl silane rectification separation device

Abstract

The utility model discloses an aminopropyl silane rectification separation device which comprises a rectification kettle, a rectification tower and a heat exchanger, a liquid distributor is arranged at the top in the rectification tower, the liquid distributor comprises a distributor liquid inlet pipe, the distributor liquid inlet pipe is connected with a return pipeline and is provided with a liquid outlet, a liquid separation tank is arranged below the distributor liquid inlet pipe, and the liquid separation tank is connected with the heat exchanger. The shape of the liquid separation tank corresponds to that of the liquid inlet pipe of the distributor, an overflow port is formed in the upper part of the liquid separation tank, and a filler is arranged below the liquid separation tank. Compared with the prior art, the liquid distributor is additionally arranged at the top in the rectifying tower, reflux liquid returning to the rectifying tower enters through the liquid distributor, and the reflux liquid is uniformly distributed on the top layer of the filler through the liquid distributor, so that the liquid is ensured to be uniformly distributed in the filler, and the phenomena of channeling and wall flowing of the liquid are avoided; the mass and heat exchange of gas and liquid in the tower is greatly improved, and the separation effect of heavy components and light components is good.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical rectification equipment, in particular to an amino silane rectification and separation device. Background Technique

[0002] Generally, after the reaction in a high-pressure synthesis kettle, the crude product analysis of aminopropyl silane shows that it contains 2% ethanol, 4% unknown substances, 75% crude product, and 10% diamine. Through the traditional rectification process, using a rectification tower with a diameter of 4 meters and a height of 3.2 meters, and using 220°C heat transfer oil as the heat source, the crude product in the rectification kettle is heated to boiling. After the crude product is heated to the bubble point temperature, it boils and turns into a gas, rising along the tower. Through the gas-liquid exchange in the packed rectification tower, the light components are condensed by the heat exchanger at the top of the tower. Part of it flows back to the rectification tower, and part of it is drawn out to the product tank to obtain the product. The product contains about 0.5% ethanol, 1% unknown substances, 98% product, and 0.5% diamine, and the rectification takes about 16 hours.

[0003] The deficiencies of the above process are that the obtained product has a low content, the long rectification time is likely to cause the polymerization of heavy component salts, affecting the product quality, and the product yield is low. To improve the product quality, the height of the rectification tower can be increased to improve the rectification effect, but this method is limited by the equipment layout space and has high costs, causing troubles to the production workshop.

[0004] Patent CN203458822U discloses an N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane rectification device, which installs a set of distillation tower and condensation receiving device on the original rectification kettle equipment, which can shorten the production time and improve the product yield. However, for the existing amino silane rectification and separation device, the transformation cost is relatively high. Content of the Utility Model

[0005] In order to solve the above technical problems, the utility model provides an amino silane rectification and separation device, and a liquid distributor is added at the top in the rectification tower to make up for the deficiency of the separation effect of the existing rectification and separation device.

[0006] To achieve this technical purpose, the utility model adopts the following scheme:

[0007] An amino silane rectification and separation device includes a rectification kettle. A rectification tower is arranged at the top of the rectification kettle. A heat exchanger is connected to the top of the rectification tower. The heat exchanger is connected to the rectification tower through a liquid phase pipeline, a reflux ratio controller, and a reflux pipeline. A liquid distributor is arranged at the top in the rectification tower. The liquid distributor includes a distributor inlet pipe, and the distributor inlet pipe is connected to the reflux pipeline. The distributor inlet pipe is provided with a liquid outlet. A liquid separation tank is arranged below the distributor inlet pipe. The shape of the liquid separation tank corresponds to the shape of the distributor inlet pipe. An overflow port is arranged at the upper part of the liquid separation tank. Packing is arranged below the liquid separation tank.

[0008] Compared with the prior art, the beneficial effects of the present utility model are as follows:

[0009] A liquid distributor is added at the top inside the rectification column of the present utility model, and the reflux liquid returning to the rectification column enters through the liquid distributor. The liquid distributor is arranged to evenly distribute the reflux liquid on the top layer of the packing, ensuring that the liquid is evenly distributed in the packing, avoiding the phenomena of liquid channeling and wall flow, greatly increasing the mass and heat exchange of gas and liquid inside the column, and achieving good separation effects for heavy components and light components; through the control of the bottom temperature of the column kettle, a product with a content of more than 99.5% is separated out. The rectification time is about 8 hours, which is shortened by 50%, greatly improving the product yield, reducing the unit consumption of the product, and saving the transformation cost.

[0010] Furthermore, a heat transfer oil heating coil is arranged outside the rectification kettle. The heat transfer oil in the heat transfer oil heating coil enters from the bottom and exits from the top, and valves are respectively arranged at the inlet and outlet of the heat transfer oil heating coil. A liquid level gauge is arranged on the side of the rectification kettle for detecting the liquid level in the rectification kettle. A bottom draw-off pipe is arranged at the top of the rectification kettle, and the bottom draw-off pipe extends to the bottom of the rectification kettle. The high-boiling substances after the rectification are discharged through the bottom draw-off pipe, reducing the occurrence of high-boiling substances blocking the discharge pipe and reducing on-site manual operation.

[0011] Furthermore, circulating water flowing from the bottom to the top is arranged outside the heat exchanger. The heat exchanger is connected to a vacuum system, and through the system vacuum, the boiling point of the rectified substance is reduced, thereby reducing the rectification temperature.

[0012] Furthermore, a reflux ratio controller is arranged between the liquid phase pipeline and the reflux pipeline. A reflux flowmeter and a reflux regulating valve are arranged on the reflux pipeline for controlling the reflux flow rate.

[0013] Furthermore, the liquid phase pipeline is connected to a product withdrawal pipeline through the reflux ratio controller. A product withdrawal regulating valve and a product withdrawal flowmeter are arranged on the product withdrawal pipeline for controlling the product withdrawal amount. Description of the Drawings

[0014] Figure 1 It is a schematic diagram of the amino silane rectification and separation device according to the embodiment of the present utility model;

[0015] Figure 2 It is a schematic diagram of the liquid distributor according to the embodiment of the present utility model;

[0016] Figure 3 It is Figure 2 View A-A in

[0017] Figure 4 It is Figure 2 View B-B in

[0018] The labels in the figure are: 1, rectifying still; 2, heat transfer oil heating coil; 3, liquid level gauge; 4, rectifying column; 5, packing; 6, liquid distributor; 7, reflux pipeline; 8, heat exchanger; 9, reflux flowmeter; 10, reflux regulating valve; 11, product withdrawal regulating valve; 12, product withdrawal flowmeter; 13, liquid phase pipeline; 14, reflux ratio controller; 15, bottom draw pipe; 16, liquid inlet pipe of the distributor; 17, liquid separation tank; 18, product withdrawal pipeline. Specific embodiments

[0019] To fully understand the purpose, features and effects of the present utility model, the following specific embodiments are used to describe the present utility model in detail, but the present utility model is not limited thereto.

[0020] See Figures 1 to 4 , the present utility model provides a technical solution: an amino silane rectifying and separating device, including a rectifying still 1, a heat transfer oil heating coil 2 is arranged outside the rectifying still 1, the heat transfer oil in the heat transfer oil heating coil 2 enters from the bottom and exits from the top, and valves are respectively arranged at the inlet and outlet of the heat transfer oil heating coil; a liquid level gauge 3 is arranged on the side of the rectifying still 1 for detecting the liquid level in the rectifying still 1; a bottom draw pipe 15 is arranged at the top of the rectifying still 1, and the bottom draw pipe 15 extends to the bottom of the rectifying still 1. The high-boiling substances after rectification are discharged through the bottom draw pipe 15, reducing the occurrence of blockage of the discharge pipe by high-boiling substances and reducing on-site manual operation.

[0021] A rectifying column 4 is arranged at the top of the rectifying still 1, a heat exchanger 8 is connected to the top of the rectifying column 4, circulating water that enters from the bottom and exits from the top is arranged outside the heat exchanger 8, and the heat exchanger 8 is connected to a vacuum system. Through the system vacuum, the boiling point of the rectifying substance is reduced, thereby reducing the rectifying temperature. The heat exchanger 8 is connected to the rectifying column 4 through a liquid phase pipeline 13, a reflux ratio controller 14 and a reflux pipeline 7, and a reflux flowmeter 9 and a reflux regulating valve 10 are arranged on the reflux pipeline 7.

[0022] A liquid distributor 6 is arranged at the top inside the rectifying column 4. The liquid distributor 6 includes a liquid inlet pipe 16 of the distributor. The liquid inlet pipe 16 of the distributor is connected to the reflux pipeline 7. The liquid inlet pipe 16 of the distributor is provided with 8 liquid outlets. A liquid separation tank 17 is arranged below the liquid inlet pipe 16 of the distributor. The shape of the liquid separation tank 17 corresponds to the shape of the liquid inlet pipe 16 of the distributor. An overflow port is arranged at the upper part of the liquid separation tank 17, and packing 5 is arranged below the liquid separation tank 17.

[0023] The liquid phase pipeline 13 is connected to a product withdrawal pipeline 18 through a reflux ratio controller 14, and a product withdrawal regulating valve 11 and a product withdrawal flowmeter 12 are arranged on the product withdrawal pipeline 18.

[0024] The working process of the utility model is as follows: The crude aminopropylsilane enters the rectification kettle 1 and is heated by the heat-conducting oil heating coil 2. After reaching the boiling temperature, it vaporizes and enters the rectification column 4. Passing through the packing 5 in the column, the gas phase rises and enters the heat exchanger 8, where it undergoes heat exchange and becomes a liquid phase. Through the liquid pipeline 13 and the reflux ratio controller 14, a part of the liquid enters the liquid distributor 6 through the reflux pipeline 7. After the liquid enters the liquid distributor 6, it is divided into 8 branch streams through the liquid inlet pipe 16 of the distributor, so that the liquid is evenly distributed in the liquid separation tank 17. When the liquid in the liquid separation tank 17 is full, it flows out through the overflow hole at the upper part of the liquid separation tank 17 and is evenly distributed on the lower packing 5. Such a design makes the liquid channel not restricted by the rising gas, increases the density of liquid distribution, and makes it easier to control the ratio of the gas-liquid channels. The liquid undergoes mass and heat exchange with the gas rising in the column, greatly improving the rectification effect; the light components are further purified and rise, while the heavy components descend, preventing the phenomena of liquid channeling and wall flow in the rectification column 4, achieving the effect of full separation and purification. Another part of the liquid enters the product tank through the extraction pipeline 18. At the end of rectification, the high-boiling substances in the kettle bottom are not discharged from the bottom discharge port, but are discharged from the kettle bottom through the kettle bottom extraction pipe 15, reducing the phenomenon of high-boiling substances blocking the discharge pipe and reducing on-site manual operation.

[0025] After the transformation, through the distribution of the liquid distributor 6, the gas-liquid exchange effect in the rectification column 4 is obvious. Combining the characteristics of the viscosity change of aminopropylsilane with heat, the product content is increased to ethanol 0.05%, unknown 0.05%, product 99.5%, diamine 0.01%. After rectification for about 8 hours, the rectification effect in the column is obvious, the rectification time is short, greatly reducing the risk of thermal decomposition and polymerization of amino salts in the kettle, and reducing the on-site manual treatment of blocked pipelines, bringing very favorable effects to the production of amino silane.

[0026] Finally, it should be noted that: The above-listed are only the preferred embodiments of the utility model. Of course, those skilled in the art can make changes and modifications to the utility model. Provided that these modifications and variations fall within the scope of the claims of the utility model and its equivalent technologies, they shall be considered as within the protection scope of the utility model.

Claims

1. An ammonia propyl silane rectification and separation device, comprising a rectification kettle (1), a rectification tower (4) is arranged at the top of the rectification kettle (1), a heat exchanger (8) is connected to the top of the rectification tower (4), the heat exchanger (8) is connected to the rectification tower (4) through a liquid phase pipeline (13), a reflux ratio controller (14) and a reflux pipeline (7), and is characterized in that, A liquid distributor (6) is provided at the top inside the rectifying column (4). The liquid distributor (6) includes a distributor inlet pipe (16). The distributor inlet pipe (16) is connected to the reflux pipeline (7). The distributor inlet pipe (16) is provided with a liquid outlet. A liquid separation tank (17) is provided below the distributor inlet pipe (16). The shape of the liquid separation tank (17) corresponds to the shape of the distributor inlet pipe (16). An overflow port is provided at the upper part of the liquid separation tank (17). Packing (5) is provided below the liquid separation tank (17).

2. The ammonia propyl silane rectifying and separating device according to claim 1, wherein A heat-conducting oil heating coil (2) is provided outside the rectifying kettle (1). A liquid level gauge (3) is provided at the side of the rectifying kettle (1). A bottom draw-off pipe (15) is provided at the top of the rectifying kettle (1), and the bottom draw-off pipe (15) extends to the bottom of the rectifying kettle (1).

3. The ammonia propyl silane rectification and separation device according to claim 1, characterized in that, Circulating water flowing in from the bottom and flowing out from the top is provided outside the heat exchanger (8). The heat exchanger (8) is connected to the vacuum system.

4. The ammonia propyl silane rectification and separation device according to claim 1, characterized in that, A reflux ratio controller (14) is provided between the liquid phase pipeline (13) and the reflux pipeline (7). A reflux flowmeter (9) and a reflux regulating valve (10) are provided on the reflux pipeline (7).

5. The ammonia propyl silane rectification and separation device according to claim 1, characterized in that, The liquid phase pipeline (13) is connected to a product withdrawal pipeline (18) through the reflux ratio controller (14). A product withdrawal regulating valve (11) and a product withdrawal flowmeter (12) are provided on the product withdrawal pipeline (18).

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