Purification device for electronic grade phosphorus oxychloride

Abstract

The utility model discloses a purification device for electronic grade phosphorus oxychloride. The purification device comprises a raw material tank, a first rectifying tower, a first complexing kettle, a second rectifying tower, a second complexing kettle and a finished product tank, the raw material tank is connected with the feeding end of the first complexing kettle through a pipeline; the discharge end of the first complexing kettle is connected with a first rectifying tower; the top of the first rectifying tower is connected with a first condenser; one end of the first condenser is connected with a first buffer tank through a pipeline; the first buffer tank is connected with the feeding end of the first complexing kettle through a pipeline; the discharging end of the second complexing kettle is connected with the feeding end of the second rectifying tower; the top of the second rectifying tower is connected with a second condenser; one end of the second condenser is connected with a second buffer tank through a pipeline; the second buffer tank is connected with the finished product tank through a pipeline; the device is simple in structure, convenient in preparation process, high in operability and good in purification effect; the operation energy consumption is low, the resources are effectively saved, and the purification cost is reduced.

Description

Technical Field

[0001] The utility model relates to the technical field of equipment related to material purification, in particular to a purification device for electronic-grade phosphorus oxychloride. Background Art

[0002] High-purity phosphorus oxychloride is a dopant in the production of integrated circuits and solar cells, and is one of the raw materials for manufacturing optical fiber preforms. Its purity is required to be as high as 99.9999% or above. In particular, phosphorus oxychloride used in large-scale integrated circuits is required to have a single metal impurity content of no more than 10ppb.

[0003] Currently, in the prior art, the purification device for phosphorus oxychloride has a complex structure and a cumbersome process flow.

[0004] Based on the above situation, our company proposed a purification device for electronic grade phosphorus oxychloride after sufficient comparison and demonstration. Utility Model Content

[0005] The purpose of the utility model is to provide a device for purifying electronic-grade phosphorus oxychloride to solve the problems in the prior art.

[0006] To achieve the above object, the technical solution adopted by the utility model is: an electronic grade phosphorus oxychloride purification device, comprising a raw material tank, a first distillation tower, a first complexing kettle, a second distillation tower, a second complexing kettle and a finished product tank;

[0007] The raw material tank is connected to the feed end of the first complexing kettle through a pipeline;

[0008] The discharge end of the first complexing kettle is connected to a first distillation tower;

[0009] A first condenser is connected to the top of the first distillation tower;

[0010] One end of the first condenser is connected to the first distillation tower through a pipeline, and the other end is connected to the first buffer tank through a pipeline;

[0011] The first buffer tank is connected to the feed end of the first complexing kettle through a pipeline, and the discharge end of the first complexing kettle is connected to the feed end of the second complexing kettle;

[0012] The discharge end of the second complexing kettle is connected to the feed end of the second distillation tower;

[0013] A second condenser is connected to the top of the second distillation tower;

[0014] One end of the second condenser is connected to the second distillation tower through a pipeline, and the other end is connected to the second buffer tank through a pipeline;

[0015] The second buffer tank is connected to the finished product tank through a pipeline.

[0016] In a preferred embodiment, the first distillation tower and the second distillation tower both include a tower kettle and a tower body; the tower kettle is arranged at the bottom of the tower body; and a reboiler is provided on one side of the tower kettle via a pipeline connection.

[0017] In a preferred embodiment, both the first distillation tower and the second distillation tower are packed towers, and structured packing trays are provided in the tower bodies.

[0018] In a preferred embodiment, the number of structured packing trays in the tower body of the first distillation tower is 80.

[0019] In a preferred embodiment, the number of structured packing trays in the tower body of the second distillation tower is 90.

[0020] In a preferred embodiment, both the first complexing kettle and the second complexing kettle are paddle-type stirred kettles.

[0021] In a preferred embodiment, the first complexing kettle and the second complexing kettle both comprise a motor and a reactor; the motor is arranged above the reactor.

[0022] Preferably, the raw material tank and the finished product tank are both glass bottles.

[0023] Due to the application of the above technical solution, the beneficial effects of this application compared with the prior art are:

[0024] The electronic-grade phosphorus oxychloride purification device of the present application comprises a raw material tank, a first complexing kettle, a first distillation tower, a second complexing kettle, a second distillation tower, and a finished product tank. The device has a simple structure, a convenient preparation process, high operability in actual production, and a good purification effect. At the same time, the operation of the double distillation tower has low energy consumption, effectively saving resources and reducing purification costs. Moreover, the provision of the first buffer tank and the second buffer tank better alleviates the problem of excessive pressure in the tank body, prevents the occurrence of tank explosion accidents, and has high safety, thereby playing a role in safety protection. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the specific implementation methods or the description of the prior art. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0026] Attachment Figure 1 This is a schematic structural diagram of a device for purifying electronic-grade phosphorus oxychloride according to the present invention;

[0027] Attachment Figure 2This is a schematic structural diagram of the first distillation tower and the second distillation tower of the present invention;

[0028] Attachment Figure 3 This is a schematic diagram of the structure of the first complexing kettle and the second complexing kettle of the utility model

[0029] Among them: 1. Raw material tank; 2. First distillation tower; 3. First complexing kettle; 4. Second distillation tower; 5. Second complexing kettle; 6. Finished product tank; 7. First condenser; 8. First buffer tank; 9. Second condenser; 10. Second buffer tank; 11. Tower kettle; 12. Tower body; 13. Reboiler; 14. Motor; 15. Reactor. DETAILED DESCRIPTION

[0030] In order to enable those skilled in the art to better understand the present invention, the following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts should fall within the scope of protection of this application.

[0031] It should be noted that the terms "first", "second", etc. in the specification and claims of the present application and the above-mentioned drawings are used to distinguish similar objects and are not necessarily used to describe a specific order or sequential order. It should be understood that the data used in this way can be interchanged where appropriate, so that the embodiments of the present application described here. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions. For example, a process, method, system, product or device that includes a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or devices.

[0032] In this application, terms such as "upper," "lower," "left," "right," "front," "back," "top," "bottom," "inner," "outer," "center," "vertical," "horizontal," "transverse," and "longitudinal" indicate positions or locations based on the positions or locations shown in the accompanying drawings. These terms are primarily intended to better describe the present invention and its embodiments and are not intended to limit the devices, elements, or components indicated to having a specific orientation, or to being constructed or operated in a specific orientation.

[0033] Furthermore, some of the above terms may be used to express other meanings besides indicating a position or location. For example, the term "on" may also be used to indicate a dependency or connection in certain circumstances. Those skilled in the art will understand the specific meanings of these terms in this utility model based on the specific circumstances.

[0034] Furthermore, the terms "installed," "disposed," "provided with," "connected," "connected," and "socketed" should be interpreted broadly. For example, they can refer to fixed connections, removable connections, or integral structures; mechanical connections or electrical connections; direct connections, indirect connections through an intermediary, or internal communication between two devices, elements, or components. Those skilled in the art will understand the specific meanings of these terms in this utility model based on the specific circumstances.

[0035] It should be noted that, in the absence of conflict, the embodiments and features of the embodiments in this application can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0036] Example 1

[0037] Attachment Figure 1-3 The electronic grade phosphorus oxychloride purification device of the utility model comprises a raw material tank 1, a first distillation tower 2, a first complexing kettle 3, a second distillation tower 4, a second complexing kettle 5 and a finished product tank 6;

[0038] The raw material tank 1 is connected to the feed end of the first complexing kettle 3 through a pipeline; the raw material tank 1 is used to store the raw material, that is, low-purity phosphorus oxychloride;

[0039] The discharge end of the first complexing kettle 3 is connected to the first distillation tower 2;

[0040] The top of the first distillation tower 2 is connected to a first condenser 7;

[0041] One end of the first condenser 7 is connected to the first distillation tower 2 through a pipeline, and the other end is connected to the first buffer tank 8 through a pipeline;

[0042] The first buffer tank 8 is connected to the feed end of the first complexing kettle 3 through a pipeline, and the discharge end of the first complexing kettle 3 is connected to the feed end of the second complexing kettle 5;

[0043] The discharge end of the second complexing kettle 5 is connected to the feed end of the second distillation tower 4;

[0044] The top of the second distillation tower 4 is connected to a second condenser 9;

[0045] One end of the second condenser 9 is connected to the second distillation tower 4 through a pipeline, and the other end is connected to the second buffer tank 10 through a pipeline;

[0046] The second buffer tank 10 is connected to the finished product tank 6 through a pipeline; the finished product tank 6 is used to store the purified phosphorus oxychloride.

[0047] The first distillation tower 2 and the second distillation tower 4 both include a tower bottom 11 and a tower body 12; the tower bottom 11 is arranged at the bottom of the tower body 12; a reboiler 13 is provided on one side of the tower bottom 11 via a pipeline.

[0048] The first distillation tower 2 and the second distillation tower 4 are both packed towers, and structured packing trays are arranged in their tower bodies 12; the number of structured packing trays in the tower body 12 of the first distillation tower 2 is 80; the number of structured packing trays in the tower body 12 of the second distillation tower 4 is 90.

[0049] The first complexing kettle 3 and the second complexing kettle 5 are both paddle-type stirring kettles; the first complexing kettle 3 and the second complexing kettle 5 both include a motor 14 and a reactor 15 for complexing reaction; the motor 14 is arranged above the reactor 15.

[0050] In order to better store raw materials and products, the raw material tank 1 and the finished product tank 6 are both glass bottles.

[0051] When used specifically, the low-purity phosphorus oxychloride in the raw material tank 1 is first introduced into the first complexing kettle 3 through a pipeline, a complexing agent is added to complex the low-purity phosphorus oxychloride, the complexing reaction temperature is controlled at 30-60°C, preferably at 50°C, and the complexed phosphorus oxychloride is then gravity-flowed into the first distillation tower 2; the complexed phosphorus oxychloride is then introduced into the first distillation tower 2, and the phosphorus oxychloride is distilled in the first distillation tower 2. Before distillation, the first distillation tower 2 is first replaced and purged, and the index content in the tower, such as water content, is measured. After the index is qualified, the first distillation tower 2 is pressure-maintained. After the pressure-maintaining treatment is completed, the phosphorus oxychloride is distilled to remove impurities in the phosphorus oxychloride; the temperature of the tower bottom 11 of the first distillation tower 2 is controlled at 100-130°C, the tower top temperature is controlled at 80-100°C, and the reflux ratio is 15-20; a preferred embodiment is that the number of plates of the first distillation tower 2 is 80, the temperature of the bottom 11 is 120 ℃, the top temperature is 90 ℃, and the reflux ratio is 20; the phosphorus oxychloride from which the heavy components are removed enters the second complexing kettle 5 for complexation, the complexation reaction temperature is controlled at 30-50 ℃, preferably at a temperature of 40 ℃, to remove trace impurities therein; the phosphorus oxychloride after complexation enters the second distillation tower 4, the phosphorus oxychloride is distilled in the second distillation tower 4, the bottom 11 temperature of the second distillation tower 4 is controlled at 100-130 ℃, the top temperature is 80-100 ℃, a preferred embodiment, the number of plates of the second distillation tower 4 is 90, the bottom 11 temperature is 110 ℃, the top temperature is 80 ℃, the reflux ratio is 30, and impurities in the phosphorus oxychloride are further removed; finally, the electronic grade phosphorus oxychloride obtained after purification is passed into the finished product tank 6.

[0052] The electronic-grade phosphorus oxychloride purification device of the present application comprises a raw material tank 1, a first complexing kettle 3, a first distillation tower 2, a second complexing kettle 5, a second distillation tower 4, and a finished product tank 6. The device has a simple structure, a convenient preparation process, high operability in actual production, and a good purification effect. At the same time, the operation of the double distillation tower has low energy consumption, effectively saving resources and reducing purification costs. Moreover, the provision of the first buffer tank 8 and the second buffer tank 10 better alleviates the problem of excessive pressure in the tank body, prevents the occurrence of tank explosion accidents, has high safety, and plays a role in safety protection.

[0053] Finally, it should be noted that the above are only preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or make equivalent replacements for some of the technical features therein. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A purification device for electronic grade phosphorus oxychloride, characterized in that: It includes a raw material tank, a first distillation tower, a first complexing kettle, a second distillation tower, a second complexing kettle and a finished product tank; The raw material tank is connected to the feed end of the first complexing kettle through a pipeline; The discharge end of the first complexing kettle is connected to a first distillation tower; A first condenser is connected to the top of the first distillation tower; One end of the first condenser is connected to the first distillation tower through a pipeline, and the other end is connected to the first buffer tank through a pipeline; The first buffer tank is connected to the feed end of the first complexing kettle through a pipeline, and the discharge end of the first complexing kettle is connected to the feed end of the second complexing kettle; The discharge end of the second complexing kettle is connected to the feed end of the second distillation tower; A second condenser is connected to the top of the second distillation tower; One end of the second condenser is connected to the second distillation tower through a pipeline, and the other end is connected to the second buffer tank through a pipeline; The second buffer tank is connected to the finished product tank through a pipeline.

2. A purification device for electronic-grade phosphorus oxychloride as claimed in claim 1, characterized in that: The first distillation tower and the second distillation tower both include a tower kettle and a tower body; the tower kettle is arranged at the bottom of the tower body; a reboiler is provided on one side of the tower kettle via a pipeline.

3. A purification device for electronic-grade phosphorus oxychloride as claimed in claim 2, characterized in that: The first distillation tower and the second distillation tower are both packed towers, and structured packing trays are arranged in the tower bodies.

4. A purification device for electronic-grade phosphorus oxychloride as claimed in claim 3, characterized in that: The number of structured packing trays in the tower body of the first distillation tower is 80.

5. A purification device for electronic-grade phosphorus oxychloride as claimed in claim 3, characterized in that: The number of structured packing trays in the tower body of the second distillation tower is 90.

6. The device for purifying electronic-grade phosphorus oxychloride according to claim 1, wherein: The first complexing kettle and the second complexing kettle are both paddle-type stirring kettles.

7. The device for purifying electronic-grade phosphorus oxychloride according to claim 6, wherein: The first complexing kettle and the second complexing kettle both include a motor and a reactor; the motor is arranged on the reactor.

8. The device for purifying electronic-grade phosphorus oxychloride according to claim 1, wherein: The raw material tank and the finished product tank are both glass bottles.

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