A separation device for a mixed reaction solution produced in the preparation of a high molecular flame retardant

Abstract

The utility model belongs to the high polymer flame retardant auxiliary preparation technical field, concretely relates to a kind of high polymer flame retardant preparation produces mixed reaction solution separating device, and the mixed reaction solution includes water, alcohol and flame retardant granular substance.Raw material storage tank, first machine pump, high-speed centrifuge, feed heater, negative pressure rectifying column, second machine pump, vacuum unit, overhead condenser, overhead receiving tank and third machine pump, the first machine pump is connected between raw material storage tank, the high-speed centrifuge is connected between first machine pump, the feed heater is connected between high-speed centrifuge, the negative pressure rectifying column is connected between feed heater, the second machine pump is connected between negative pressure rectifying column, the vacuum unit is connected between negative pressure rectifying column, the utility model can realize high polymer flame retardant recovery by the process, while realizing the separation of methanol and water, and produce methanol with purity reaching more than 99% purity, to further improve the utilization of resources.

Description

Technical Field

[0001] This utility model belongs to the field of polymer flame retardant preparation technology, specifically relating to a device for separating mixed reaction solutions generated during the preparation of polymer flame retardants. Background Technology

[0002] Flame retardants are functional chemical additives that can inhibit the combustion of polymer materials or delay the spread of combustion. They are widely used in materials such as plastics, rubber, and fibers. According to their form, they can be divided into powder, granules, and liquid. The appropriate type should be selected according to the characteristics of the substrate. With the increasing requirements for safety and environmental protection, flame retardant materials are required to have both good flame retardant properties and good environmental performance.

[0003] Currently, in order to place higher demands on the existing polymer flame retardant additive preparation technology in terms of safe production, environmental protection and product application, this application requires that the polymerization process be precisely controlled in terms of safe production, and that the reaction liquid and solvent generated be recycled in terms of environmental protection to improve the environmental protection level of the entire production plant. Therefore, these requirements put forward new requirements for the industrial production line of coated polymer flame retardant additives. Utility Model Content

[0004] The purpose of this invention is to provide a device for separating the mixed reaction solution generated during the preparation of polymeric flame retardants. This device aims to impose higher requirements on existing polymeric flame retardant additive preparation technologies in terms of safe production, environmental protection, and product application. In terms of safe production, this application requires precise control of the polymerization process, and in terms of environmental protection, it requires the recovery of the generated reaction liquid and solvent to improve the environmental protection level of the entire production device. Therefore, these requirements place new demands on the industrial production line of coated polymeric flame retardant additives.

[0005] To achieve the above objectives, this utility model provides the following technical solution: a separation device for a mixed reaction solution generated during the preparation of a polymer flame retardant, comprising a raw material storage tank, a first pump, a high-speed centrifuge, a feed heater, a negative pressure distillation column, a second pump, a vacuum unit, a column top condenser, a column top receiving tank, and a third pump, wherein the first pump is connected to the raw material storage tank; The high-speed centrifuge is connected to the first pump, the feed heater is connected to the high-speed centrifuge, the negative pressure distillation column is connected to the feed heater, the second pump is connected to the negative pressure distillation column, the vacuum unit is connected to the negative pressure distillation column, the top condenser is connected to the negative pressure distillation column, the top receiving tank is connected to the top condenser, and the third pump is connected to the top receiving tank.

[0006] In order to allow the centrifuged liquid to directly enter the heat exchanger of the negative pressure distillation column for heating, as a separation device for the mixed reaction solution generated during the preparation of a polymer flame retardant according to this invention, preferably, the feed rate of the high-speed centrifuge is 5-10 m / s. 3 / h, maximum speed is less than 5000rpm.

[0007] To heat the alcohol-water mixture to 60-75℃, as part of the separation device for the mixed reaction solution generated during the preparation of a polymeric flame retardant according to this invention, preferably, the heat exchange area of ​​the feed heater is 20-30 m². 2 Furthermore, the pressure of the feed heater is less than 1 MPa.

[0008] To control the reflux ratio of the receiving tank at the top of the column, and as a separation device for the mixed reaction solution generated during the preparation of a polymer flame retardant according to this invention, preferably, the negative pressure distillation column is a packed column with a feed rate of 5-10 m / s. 3 / h.

[0009] In order to control the reflux ratio of the receiving tank at the top of the column, as a separation device for the mixed reaction solution generated during the preparation of a polymer flame retardant according to this utility model, preferably, the pressure inside the negative pressure distillation column is between -0.03 and 0.06 MPa.

[0010] In order to control the reflux ratio of the top receiving tank, as a separation device for the mixed reaction solution generated during the preparation of polymer flame retardants according to this utility model, preferably, the temperature of the top receiving tank is controlled at 55-65℃.

[0011] In order to reflux a portion of the methanol in the top receiving tank into the negative pressure distillation column as needed, as a separation device for the mixed reaction solution generated during the preparation of a polymer flame retardant according to this utility model, preferably, the third pump is a reflux pump, and the end of the third pump away from the top receiving tank is connected to the negative pressure distillation column.

[0012] Compared with the prior art, the beneficial effects of this utility model are: The raw materials in the storage tank are added to a high-speed centrifuge in proportion by a first pump, which then completely separates the solid polymer flame retardant from the material. The separated solid polymer flame retardant is recycled. The centrifuged alcohol-water mixture is heated by the feed heater of a negative pressure distillation column and then enters the negative pressure distillation column. The negative pressure distillation column is connected to a vacuum unit. The top receiving tank at the top of the negative pressure distillation column collects methanol with a purity of over 99%. Liquid water is generated at the bottom of the negative pressure distillation column. The liquid water generated at the bottom of the column can be discharged by a second pump, and a portion can be output as methanol product by a third pump. A portion of the methanol can be returned to the negative pressure distillation column as needed. Thus, this process can achieve the recovery of polymer flame retardant while separating methanol and water, and produce methanol with a purity of over 99%, thereby improving resource utilization. Attached Figure Description

[0013] The accompanying drawings are provided to further illustrate the present invention and form part of the specification. They are used together with the embodiments of the present invention to explain the present invention, but do not constitute a limitation thereof. In the drawings: Figure 1 This is a schematic diagram of the process flow provided for an embodiment of this application.

[0014] In the diagram: 1. Raw material storage tank; 2. First pump; 3. High-speed centrifuge; 4. Feed heater; 5. Negative pressure distillation column; 6. Second pump; 7. Vacuum unit; 8. Top condenser; 9. Top receiving tank; 10. Third pump. Detailed Implementation

[0015] 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.

[0016] Please see Figure 1 The present invention provides the following technical solution: a separation device for a mixed reaction solution generated during the preparation of a polymer flame retardant, comprising a raw material storage tank 1, a first pump 2, a high-speed centrifuge 3, a feed heater 4, a negative pressure distillation column 5, a second pump 6, a vacuum unit 7, a column top condenser 8, a column top receiving tank 9, and a third pump 10, wherein the first pump 2 is connected to the raw material storage tank 1; The high-speed centrifuge 3 is connected to the first pump 2, the feed heater 4 is connected to the high-speed centrifuge 3, the negative pressure distillation column 5 is connected to the feed heater 4, the second pump 6 is connected to the negative pressure distillation column 5, the vacuum unit 7 is connected to the negative pressure distillation column 5, the top condenser 8 is connected to the negative pressure distillation column 5, the top receiving tank 9 is connected to the top condenser 8, and the third pump 10 is connected to the top receiving tank 9.

[0017] Preferably, the feeding speed of the high-speed centrifuge 3 is 5-10 m / s. 3 / h, maximum speed is less than 5000rpm.

[0018] In practical use, the centrifuged liquid after centrifugation by the high-speed centrifuge 3 directly enters the negative pressure distillation column 5 and is heated by the feed heater 4; Preferably, the heat exchange area of ​​the feed heater 4 is 20-30m². 2 Furthermore, the pressure of the feed heater 4 is less than 1 MPa.

[0019] In practical use, the alcohol-water mixture is heated to 60-75℃ by the feed heater 4, where the heat source can be medium-pressure steam or heat transfer oil.

[0020] Preferably, the negative pressure distillation column 5 is a packed column with a feed rate of 5-10 m / s. 3 / h, the pressure inside the negative pressure distillation column 5 is -0.03-0.06Mpa, the temperature of the top receiving tank 9 is controlled at 55-65℃, the third pump 10 is a reflux pump, and the end of the third pump 10 away from the top receiving tank 9 is connected to the negative pressure distillation column 5.

[0021] In practical use, the methanol distilled from the top of the negative pressure distillation column 5 is cooled to 35-40°C by the top condenser 8, and then enters the top receiving tank 9. A portion of the methanol is then output as a finished product by the third pump 10 at the top of the column, and a portion of the methanol can be refluxed into the negative pressure distillation column 5 as needed.

[0022] Working principle: First, the raw materials for preparing the polymer flame retardant are put into the raw material storage tank 1. Then, the raw materials in the raw material storage tank 1 are added to the high-speed centrifuge 3 in proportion by the first pump 2. Then, the solid polymer flame retardant in the material is completely separated and the separated solid polymer flame retardant is recycled. Next, the centrifuged alcohol-water mixture is heated to 60-75°C by the feed heater 4 before entering the negative pressure distillation column 5, and the feed rate of the negative pressure distillation column 5 is controlled at 5-10 m / s. 3 / h, and the internal pressure is controlled between -0.03 and 0.06 MPa; Then, the methanol distilled from the top of the negative pressure distillation column 5 is cooled to 35-40°C by the top condenser 8 and enters the top receiving tank 9. The temperature of the top receiving tank 9 is controlled at 55-65°C. Meanwhile, bottom liquid water will be generated at the bottom of the negative pressure distillation column 5. The bottom liquid water generated at the bottom of the column can be discharged outward by the second pump 6. Finally, the third pump 10 can output a portion of the methanol as finished product to the outside, and a portion of the methanol can be refluxed into the negative pressure distillation tower 5 as needed. Thus, this process can achieve the recovery of polymer flame retardants while separating methanol and water, and produce methanol with a purity of over 99%, thereby improving resource utilization.

[0023] Finally, it should be noted that the above are merely preferred embodiments of this utility model and are not intended to limit the utility model. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. A device for separating a mixed reaction solution generated during the preparation of a polymer flame retardant, comprising a raw material storage tank (1), a first pump (2), a high-speed centrifuge (3), a feed heater (4), a negative pressure distillation column (5), a second pump (6), a vacuum unit (7), a column top condenser (8), a column top receiving tank (9), and a third pump (10), characterized in that, The first pump (2) is connected to the raw material storage tank (1); The high-speed centrifuge (3) is connected to the first pump (2), the feed heater (4) is connected to the high-speed centrifuge (3), the negative pressure distillation column (5) is connected to the feed heater (4), the second pump (6) is connected to the negative pressure distillation column (5), the vacuum unit (7) is connected to the negative pressure distillation column (5), the top condenser (8) is connected to the negative pressure distillation column (5), the top receiving tank (9) is connected to the top condenser (8), and the third pump (10) is connected to the top receiving tank (9).

2. The apparatus for separating the mixed reaction solution generated during the preparation of a polymeric flame retardant according to claim 1, characterized in that: The feeding speed of the high-speed centrifuge (3) is 5-10 m / s. 3 / h, maximum speed is less than 5000rpm.

3. The apparatus for separating the mixed reaction solution generated during the preparation of a polymeric flame retardant according to claim 1, characterized in that: The heat exchange area of ​​the feed heater (4) is 20-30m². 2 And the pressure of the feed heater (4) is less than 1 MPa.

4. The apparatus for separating the mixed reaction solution generated during the preparation of a polymeric flame retardant according to claim 1, characterized in that: The negative pressure distillation column (5) is a packed column with a feed rate of 5-10 m / s. 3 / h.

5. The apparatus for separating the mixed reaction solution generated during the preparation of a polymeric flame retardant according to claim 4, characterized in that: The pressure inside the negative pressure distillation column (5) is between -0.03 and 0.06 MPa.

6. The apparatus for separating the mixed reaction solution generated during the preparation of a polymeric flame retardant according to claim 1, characterized in that: The temperature of the receiving tank (9) at the top of the tower is controlled at 55-65℃.

7. The apparatus for separating the mixed reaction solution generated during the preparation of a polymeric flame retardant according to claim 1, characterized in that: The third pump (10) is a reflux pump, and the end of the third pump (10) away from the top receiving tank (9) is connected to the negative pressure distillation column (5).

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