Pressurized conversion device for preparing high-purity red phosphorus
By using high-strength protective containers and inert gas balance system in high-pressure conversion devices, automatic balance of internal and external pressures of the conversion container is achieved, solving the problem of easy breakage of the conversion container, and improving the conversion efficiency and product quality.
Patent Information
- Application Number
- CN202422301271.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-20
- Publication Date
- 2025-07-25
- Estimated Expiration
- 2034-09-20
AI Technical Summary
In the prior art, when high-pressure conversion method produces electronic grade red phosphorus, the conversion container is prone to shattering, resulting in low conversion efficiency and high safety risks, making it difficult to achieve efficient production of high-purity red phosphorus.
A pressure-bearing conversion device is designed, using a high-strength protective container and an inflation system, balancing the internal and external pressures through inert gas, and using a pressure sensor and a valve controller to achieve the internal and external pressure balance of the conversion container to avoid breakage.
It improves conversion efficiency, shortens production time, increases the density of red phosphorus, increases the added value of the product, and solves the problem of easy breakage of the conversion container.
Smart Images
Figure CN223144659U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of high-purity red phosphorus preparation, and particularly relates to a pressure conversion device for preparing high-purity red phosphorus. Background Technique
[0002] High-purity red phosphorus, that is, electronic-grade red phosphorus, is a dopant and diffuser for semiconductors and the main raw material for semiconductor black phosphorus, GaP, and InP. The purity requirement of electronic-grade red phosphorus reaches 6N or 7N (99.9999% - 99.99999%), especially the content of As reaches below 0.2 ppm, and even 0.05 ppm.
[0003] Currently, the methods for producing electronic-grade red phosphorus basically involve directly converting electronic-grade yellow phosphorus into red phosphorus. The conversion forms are roughly divided into two types: one is atmospheric pressure conversion, where electronic-grade yellow phosphorus is gradually heated in a gradient manner and gradually converted into electronic-grade red phosphorus within the temperature range of 170°C to 355°C by the method of gradual heating. The process is simple, but this method takes a long time, and one conversion requires continuous production for 5 - 8 days, and the production operation is complex. The other is high-pressure conversion, which is carried out at a temperature of about 300°C and a certain pressure. The entire heating and pressurization process is carried out step by step, with a maximum temperature of 325°C. Under the environment of a pressure as high as 10 atmospheres, electronic-grade yellow phosphorus is gradually converted into red phosphorus. This method can shorten the production cycle, but has high requirements for equipment, and the high-temperature conditions also pose a safety risk.
[0004] Our company currently uses the atmospheric pressure conversion method. Each conversion takes 7 - 8 days, with low conversion efficiency. The monthly output is only 20 kg, and the density is low. Only 50 - 60% of the density is above 2 g / m³, which is the key problem restricting the development of red phosphorus in the company. For this reason, the project team has carried out relevant basic research in the early stage and initially explored the high-pressure conversion method. During the experiment, when the pressure was increased to 2 kg, the quartz container used for conversion would break; when the material of the container was changed to ceramics, the ceramic container would also break as the pressure increased, and the conversion of yellow phosphorus to red phosphorus could not be completed. Content of the Utility Model
[0005] In view of this, the purpose of the utility model is to provide a pressure conversion device for preparing high-purity red phosphorus to solve the technical problem that the conversion container is easily broken when our company uses the high-pressure conversion method to produce electronic-grade red phosphorus.
[0006] The purpose of the utility model is achieved through the following technical solutions:
[0007] A pressure-conversion device for preparing high-purity red phosphorus, which comprises a heating container. A converter is arranged inside the heating container. The converter includes a high-strength protective container, and only an air inlet is provided on the protective container. Inside the protective container, there is a highly corrosion-resistant conversion container for containing electronic-grade yellow phosphorus and high-purity water. A sandwich layer with a uniform thickness is formed between the conversion container and the protective container. Only a feeding air inlet is provided on the conversion container. The feeding air inlet extends out of the protective container and is hermetically connected to the protective container. The feeding air inlet is connected to a feeding system. The air inlets on the protective container and the conversion container are both connected to an air-filling system that can fill inert gas into the protective container and the conversion container to balance the internal and external air pressures of the conversion container. The air-filling system includes an inert gas storage tank, a pump, a first valve, and a second valve. The pump is connected to the inert gas storage tank. The air inlet on the protective container is connected to the pump through a pipeline and the first valve. The air inlet on the conversion container is connected to the pump through a pipeline and the second valve. A first pressure sensor is arranged inside the protective container outside the conversion container, and a second pressure sensor is arranged inside the conversion container. The first pressure sensor, the second pressure sensor, the first valve, the second valve, and the pump are all connected to a controller.
[0008] Further, both the conversion container and the protective container are ellipsoidal.
[0009] Furthermore, the heating container includes a heating tank filled with water. The heating tank is placed on a heating furnace. A temperature sensor is arranged inside the heating tank. The temperature sensor is connected to the controller, and the controller is connected to the heating furnace.
[0010] Still further, multiple converters are arranged inside the heating container at intervals.
[0011] The beneficial effects of the present utility model are as follows:
[0012] For the pressure-conversion device for preparing high-purity red phosphorus of the present utility model, by adding a protective container and an air-filling system, the internal and external pressures of the conversion container are made equal in real time and balanced, solving the problem that the conversion container is broken when the heating container heats up.
[0013] The first pressure sensor, the second pressure sensor, the first valve, the second valve, and the pump of the air-filling system, the protective container, and the conversion container are connected to the controller, realizing automatic adjustment of the pressure inside and outside the converter, always ensuring that the internal and external pressures of the converter are equal and balanced, and avoiding the breakage of the conversion container.
[0014] By setting a temperature sensor, the heating temperature of the heating furnace is automatically controlled according to the designed temperature.
[0015] Other advantages, objects and features of the present utility model will be set forth to some extent in the following description, and to some extent, will be apparent to those skilled in the art based on the study of the following text, or can be taught from the practice of the present utility model. The objects and other advantages of the present utility model can be realized and obtained through the following description. Brief Description of the Drawings
[0016] In order to make the objects, technical solutions and advantages of the present utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings, where:
[0017] Figure 1 is a schematic structural diagram of the present utility model.
[0018] Figure 2 is a schematic circuit diagram of the circuit part of the present utility model.
[0019] In the figure: heating container 1, protective container 2, inflation port 3, conversion container 4, feed inflation port 5. Detailed Description of the Preferred Embodiments
[0020] Hereinafter, the preferred embodiments of the present utility model will be described in detail with reference to the accompanying drawings. It should be understood that the preferred embodiments are only for explaining the present utility model, rather than for limiting the protection scope of the present utility model.
[0021] As Figure 1As shown in the figure, a pressure conversion device for preparing high-purity red phosphorus includes a heating container 1. The heating container 1 includes a heating tank filled with water. The heating tank is placed on a heating furnace. A temperature sensor is provided inside the heating tank. The temperature sensor is connected to a controller, and the controller is connected to the heating furnace to automatically control the heating temperature of the heating furnace. The top of the heating container 1 is open. There are two converters inside the heating container 1. The two converters are fixed on a bracket, and the bracket is fixed on a wall or other structures. The two converters do not touch the inner wall of the heating container 1 and are arranged at intervals. The converter includes a high-strength protective container 2. The protective container 2 is a metal container. The metal container is ellipsoidal and vertically arranged. Only an air inlet 3 is provided on the protective container 2. The air inlet 3 on the protective container 2 is connected to a pump through a pipeline and a first valve. The pump is connected to an inert gas storage tank. The inert gas is argon. A conversion container 4 is provided inside the protective container 2. The conversion container 4 is made of quartz, ceramic, or other materials lined with polytetrafluoroethylene. The conversion container 4 has the same ellipsoidal shape as the protective container 2. The size of the conversion container 4 is smaller than that of the protective container 2. The conversion container 4 and the protective container 2 are coaxially arranged, that is, a uniformly thick interlayer is formed between the protective container 2 and the conversion container 4. The conversion container 4 contains electronic-grade yellow phosphorus and high-purity water. An inlet air charging port 5 is provided at the upper end of the conversion container 4. The inlet air charging port 5 extends out of the protective container 2 and is hermetically connected to the protective container 2 to seal the protective container 2 and the conversion container 4. The inlet air charging port 5 is connected to a storage tank through a pipeline and a valve. The inlet air charging port 5 is also connected to a pump through a pipeline and a second valve. A first pressure sensor is provided inside the protective container 2 outside the conversion container 4. A second pressure sensor is provided inside the conversion container 4. The first pressure sensor, the second pressure sensor, the first valve, the second valve, and the pump are all connected to the controller to automatically control the air charging volume so that the internal and external pressures of the conversion container 4 are the same and reach equilibrium, avoiding the conversion container 4 from cracking due to heating in the heating container 1. The amount of inert gas filled into the protective container 2 and the conversion container 4 shall not exceed 10 kg respectively. The first valve and the second valve are both electrically controlled valves.
[0022] The temperature sensor detects the temperature inside the heating tank and transmits the temperature information to the controller. The controller controls the heating temperature of the heating furnace in real time according to the designed temperature. As the conversion container 4 is heated, the internal air pressure changes. The second pressure sensor detects the pressure inside the conversion container 4 in real time and transmits the pressure information to the controller. The first pressure sensor detects the pressure change inside the protective container 2 in real time and transmits the pressure information to the controller. The controller controls the first valve, the second valve, and the pump to charge the conversion container 4 and the protective container 2 with air respectively so that the internal and external pressures of the conversion container 4 are kept the same and reach equilibrium.
[0023] As the temperature in the heating container 1 changes, the air pressure in the conversion container 4 changes accordingly. Inflate the inside and outside of the converter 4 respectively to ensure that the pressures inside and outside the conversion container are equal at all times, and avoid the breaking of the conversion container 4. The use of this device enables the production of red phosphorus by the high-pressure conversion method, improves the conversion efficiency, shortens the conversion time, which only takes 2-3 days for one conversion, increases the density of red phosphorus, and enhances the added value of red phosphorus.
[0024] Of course, the heating container 1 can also be of other structures. The heating temperature of the heating container 1 can be manually controlled. The shapes of the protective container 2 and the conversion container 4 can be tubular or other shapes.
[0025] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit them. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the spirit and scope of the technical solutions, and they should all be covered within the scope of the claims of the present invention.
Claims
1. A pressure-conversion device for preparing high-purity red phosphorus, characterized in that: It includes a heating container (1), inside which there is a converter. The converter includes a high-strength protective container (2). There is only an inflation port (3) on the protective container (2). Inside the protective container (2), there is a highly corrosion-resistant conversion container (4) for containing electronic-grade yellow phosphorus and high-purity water. A uniformly thick interlayer is formed between the conversion container (4) and the protective container (2). There is only a feed inflation port (5) on the conversion container (4). The feed inflation port (5) extends out of the protective container (2) and is hermetically connected to the protective container (2). The feed inflation port (5) is connected to a feed system. The inflation ports on the protective container (2) and the conversion container (4) are both connected to an inflation system that can inflate inert gas into the protective container (2) and the conversion container (4) to balance the internal and external air pressures of the conversion container (4). The inflation system includes an inert gas storage tank, a pump, a first valve, and a second valve. The pump is connected to the inert gas storage tank. The inflation port (3) on the protective container (2) is connected to the pump through a pipeline and the first valve. The inflation port on the conversion container (4) is connected to the pump through a pipeline and the second valve. A first pressure sensor is provided inside the protective container (2) outside the conversion container (4), and a second pressure sensor is provided inside the conversion container (4). The first pressure sensor, the second pressure sensor, the first valve, the second valve, and the pump are all connected to a controller.
2. The pressure-conversion device for preparing high-purity red phosphorus according to claim 1, wherein: Both the conversion container (4) and the protective container (2) are ellipsoidal.
3. The pressure-conversion device for preparing high-purity red phosphorus according to claim 1, wherein: The heating container (1) includes a heating tank filled with water. The heating tank is placed on a heating furnace. A temperature sensor is provided inside the heating tank. The temperature sensor is connected to the controller, and the controller is connected to the heating furnace.
4. The pressure-conversion device for preparing high-purity red phosphorus according to any one of claims 1-3, characterized in that: There are multiple converters inside the heating container (1) and they are arranged at intervals.