Rectification device for 2-(1-acetyl-6-fluoro-1H-indazole-5-yl)-2, 2-ethyl difluoroacetate

Abstract

The utility model relates to the technical field of chemical equipment, in particular to a rectification device for 2-(1-acetyl-6-fluoro-1H-indazole-5-yl)-2, 2-ethyl difluoroacetate, which comprises a rectification tower and the like. A heating device is arranged at the bottom end of the rectifying tower, a rectifying pipe is connected to the top end of the rectifying tower, a condenser is connected to the other end of the rectifying pipe, a water inlet pipe is connected to the upper end of the condenser, a return pipe is connected to the lower end of the condenser, and a condensing pipe is mounted in the condenser. According to the utility model, the consumption of water resources is greatly reduced by recycling the cooling water, and the contact area between the condensation pipe and the cooling water is increased by combining with the spiral condensation pipe, so that the heat exchange efficiency is enhanced.

Description

Technical Field

[0001] This utility model relates to the field of chemical equipment technology, and in particular to a distillation apparatus for ethyl 2-(1-acetyl-6-fluoro-1H-indazole-5-yl)-2,2-difluoroethyl acetate. Background Technology

[0002] 2-(1-Acetyl-6-fluoro-1H-indazole-5-yl)-2,2-difluoroethyl ester is an important organic synthesis intermediate with broad application prospects in the fields of medicine and pesticides. Distillation is a key process in its separation and purification.

[0003] Traditional distillation units have significant drawbacks in their cooling circulation systems. Most units have simple cooling water flow designs, where cooling water is often directly discharged after absorbing heat in the condenser, resulting in water waste. Furthermore, these units lack optimized design for the cooling water circulation path, leading to low cooling efficiency and difficulty in meeting the demands of high-purity, large-scale production. Therefore, it is necessary to develop a distillation unit that can achieve efficient cooling water circulation, carrying away heat from the condenser and then orderly returning to the storage tank, thereby improving cooling efficiency and saving resources. Utility Model Content

[0004] In order to overcome the shortcomings of existing distillation devices such as water waste and low heat exchange efficiency, the technical problem of this utility model is to provide a distillation device for ethyl 2-(1-acetyl-6-fluoro-1H-indazole-5-yl)-2,2-difluoroacetate.

[0005] The technical solution of this utility model is as follows: a distillation apparatus for ethyl 2-(1-acetyl-6-fluoro-1H-indazol-5-yl)-2,2-difluoroacetate, comprising a distillation column, a heating device, a distillation tube, a condenser, a reflux pipe, a condenser tube, a water inlet pipe, a water pump, and a water storage tank. The bottom end of the distillation column is equipped with a heating device, the top end of the distillation column is connected to a distillation tube, the other end of the distillation tube is connected to a condenser, the upper end of the condenser is connected to a water inlet pipe, the lower end of the condenser is connected to a reflux pipe, a condenser tube is installed inside the condenser, a water pump is installed on the water inlet pipe, and the other end of the reflux pipe is connected to a water storage tank.

[0006] Furthermore, it is particularly preferred that the condenser tube is spiral-shaped and connects from the distillation tube at the top of the condenser to the outlet at the bottom of the condenser.

[0007] In addition, it is particularly preferred that the condenser also includes a settling cylinder and a measuring cylinder, with the settling cylinder provided at the discharge port at the bottom of the condenser and the measuring cylinder provided at the overflow pipe near the settling cylinder.

[0008] Furthermore, it is particularly preferred that a flame-collecting hood is also included, with the flame-collecting hood installed at the bottom of the distillation column.

[0009] In addition, it is particularly preferred that a filter is included, with a filter installed at the end of the water inlet pipe that extends into the water storage tank.

[0010] Furthermore, it is particularly preferred that the distillation column also includes a temperature gauge and a pressure gauge, which are installed at the top of the distillation column.

[0011] Compared with the prior art, the present invention has the following advantages:

[0012] 1. This utility model greatly reduces water consumption by circulating cooling water. In addition, the spiral condenser tube increases the contact area between the condenser tube and the cooling water, prolongs the gas-liquid and liquid-liquid heat transfer path and contact time, and significantly enhances the heat exchange efficiency.

[0013] 2. The settling cylinder and measuring cylinder of this utility model enable effective separation and precise measurement of distillation products, which helps to accurately control product quality and meet the requirements of different production processes for product purity and yield. Attached Figure Description

[0014] Figure 1 This is a three-dimensional structural diagram of the present invention.

[0015] Figure 2 This is a three-dimensional structural diagram of the distillation column of this utility model.

[0016] Figure 3 This is a three-dimensional structural diagram of the condenser of this utility model.

[0017] Figure 4 This is a three-dimensional structural diagram of the condenser of this utility model.

[0018] Figure 5 This is a three-dimensional structural diagram of the water storage tank of this utility model.

[0019] The above-mentioned attached drawings include the following reference numerals: 1-distillation column, 2-flame hood, 3-heating device, 4-distillation tube, 5-condenser, 6-settling cylinder, 7-measuring cylinder, 8-reflux pipe, 9-condenser tube, 10-water inlet pipe, 11-water pump, 12-filter, 13-water storage tank, 14-thermometer, 15-pressure gauge. Detailed Implementation

[0020] To make the objectives, technical solutions, and advantages of this utility model clearer, the present utility model will be further described in detail below with reference to specific embodiments and accompanying drawings. It should be understood that these descriptions are merely exemplary and not intended to limit the scope of this utility model. Furthermore, descriptions of well-known structures and technologies are omitted in the following description to avoid unnecessarily obscuring the concept of this utility model.

[0021] Example: A distillation apparatus for ethyl 2-(1-acetyl-6-fluoro-1H-indazol-5-yl)-2,2-difluoroacetate, such as Figure 1-5 As shown, the system includes a distillation column 1, a heating device 3, a distillation tube 4, a condenser 5, a reflux pipe 8, a condenser tube 9, a water inlet pipe 10, a water pump 11, and a water storage tank 13. The bottom of the distillation column 1 is equipped with the heating device 3, the top of the distillation column 1 is connected to the distillation tube 4, the other end of the distillation tube 4 is connected to the condenser 5, the upper end of the condenser 5 is connected to the water inlet pipe 10, the lower end of the condenser 5 is connected to the reflux pipe 8, the condenser tube 9 is installed inside the condenser 5, the water pump 11 is installed on the water inlet pipe 10, and the other end of the reflux pipe 8 is connected to the water storage tank 13.

[0022] The condenser tube 9 is spiral-shaped and connects from the distillation tube 4 at the top of the condenser 5 to the outlet at the bottom of the condenser 5. This design increases the contact area and contact time between the gas and liquid phases, prolongs the heat transfer path and contact time between the gas and liquid and the liquid and liquid phases, and significantly enhances the heat exchange efficiency.

[0023] A settling cylinder 6 is provided at the discharge port at the bottom of the condenser 5, and a measuring cylinder 7 is provided near the overflow pipe of the settling cylinder 6. This enables effective separation and precise measurement of the distillation products, which helps to accurately control product quality and meet the requirements of different production processes for product purity and yield.

[0024] The bottom of the distillation column 1 is equipped with a heat-concentrating hood 2, which can effectively concentrate the heat generated by the heating device, reduce the heat loss to the surrounding environment, and improve heating efficiency.

[0025] A filter 12 is installed at one end of the water inlet pipe 10 that extends into the water storage tank 13. This filter can effectively intercept impurities in the cooling water and prevent these impurities from entering the condenser 5, thus avoiding pipe blockage or affecting the heat exchange effect due to the accumulation of impurities.

[0026] The top of the distillation column 1 is equipped with a thermometer 14 and a pressure gauge 15. During the entire distillation process, if the temperature or pressure becomes abnormal, the operator can adjust the power of the heating device 3, the flow rate of the water pump 11, or the reflux ratio and other parameters in a timely manner based on the monitoring data to ensure that the distillation process continues under safe and stable conditions.

[0027] The material containing ethyl 2-(1-acetyl-6-fluoro-1H-indazol-5-yl)-2,2-difluoroacetate is fed into distillation column 1. The heating device 3 at the bottom of distillation column 1 is turned on, and under the action of the heat-concentrating shroud 2, the heat is concentrated on the material inside the column. Due to the difference in boiling points of the components in the mixture, the lower boiling point components vaporize first after being heated and rise from bottom to top in distillation column 1.

[0028] The gaseous material enters the condenser 5 through the distillation tube 4 at the top of the distillation column 1. At this time, the water pump 11 on the inlet pipe 10 is started. The cooling water in the water storage tank 13 flows into the condenser 5 along the inlet pipe 10 under the drive of the water pump 11. After the cooling water carries away the heat from the condenser tube 9, it returns to the water storage tank 13 through the return pipe 8. The spiral condenser tube 9 inside the condenser 5 greatly increases the contact area and time between the cooling water and the gaseous material. The cooling water continuously absorbs the heat from the gaseous material, causing it to gradually cool and liquefy. The liquefied material flows along the condenser tube 9 to the discharge port at the bottom of the condenser 5.

[0029] The liquid material discharged from the outlet enters the settling cylinder 6, where it settles. If the material contains solid impurities or liquids of different densities, solid-liquid separation or liquid stratification can be achieved through settling. After settling, the upper layer or the liquid that meets the requirements flows into the measuring cylinder 7 through the overflow pipe. The volume of the outflowing liquid is accurately measured through the measuring cylinder 7 to facilitate quantitative analysis and subsequent processing of the distillation products.

[0030] The present application has been described in detail above. Specific examples have been used to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only for the purpose of helping to understand the method and core ideas of the present application. At the same time, for those skilled in the art, there will be changes in the specific implementation methods and application scope based on the ideas of the present application. Therefore, the content of this specification should not be construed as a limitation of the present application.

Claims

1. A distillation apparatus for ethyl 2-(1-acetyl-6-fluoro-1H-indazol-5-yl)-2,2-difluoroacetate, comprising a distillation column (1), a heating device (3), a distillation tube (4), and a condenser (5), characterized in that: It also includes a reflux pipe (8), a condenser pipe (9), a water inlet pipe (10), a water pump (11), and a water storage tank (13). The bottom of the distillation column (1) is equipped with a heating device (3). The top of the distillation column (1) is connected to a distillation tube (4). The other end of the distillation tube (4) is connected to a condenser (5). The upper end of the condenser (5) is connected to a water inlet pipe (10). The lower end of the condenser (5) is connected to a reflux pipe (8). The condenser (5) is equipped with a condenser pipe (9). A water pump (11) is installed on the water inlet pipe (10). The other end of the reflux pipe (8) is connected to a water storage tank (13).

2. The distillation apparatus for ethyl 2-(1-acetyl-6-fluoro-1H-indazol-5-yl)-2,2-difluoroacetate as described in claim 1, characterized in that: The condenser tube (9) is spiral-shaped and connects from the distillation tube (4) at the top of the condenser (5) to the outlet at the bottom of the condenser (5).

3. The distillation apparatus for ethyl 2-(1-acetyl-6-fluoro-1H-indazol-5-yl)-2,2-difluoroacetate as described in claim 2, characterized in that: It also includes a settling cylinder (6) and a measuring cylinder (7). The settling cylinder (6) is provided at the discharge port at the bottom of the condenser (5), and the measuring cylinder (7) is provided at the overflow pipe near the settling cylinder (6).

4. The distillation apparatus for ethyl 2-(1-acetyl-6-fluoro-1H-indazol-5-yl)-2,2-difluoroacetate as described in claim 3, characterized in that: It also includes a flame hood (2), which is installed at the bottom of the distillation column (1).

5. The distillation apparatus for ethyl 2-(1-acetyl-6-fluoro-1H-indazol-5-yl)-2,2-difluoroacetate as described in claim 4, characterized in that: It also includes a filter (12), and the end of the water inlet pipe (10) that extends into the water storage tank (13) is equipped with a filter (12).

6. The distillation apparatus for ethyl 2-(1-acetyl-6-fluoro-1H-indazol-5-yl)-2,2-difluoroacetate as described in claim 5, characterized in that: It also includes a temperature gauge (14) and a pressure gauge (15), which are installed at the top of the distillation column (1).

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