A method for filling adsorption / deproportionation resin

Abstract

The present invention relates to the technical field of polysilicon production, and specifically to a method for loading an adsorption / deproportionation resin, comprising: adding the resin to a loading tank, with the resin volume accounting for 70-90% of the tank volume; introducing nitrogen into the loading tank for drying; adding silicon tetrachloride to an adsorption column in an amount of 1 / 2 to 2 / 3 of the total volume of the adsorption column, and releasing the pressure to below 0.03 MPa; replenishing the pressure of the loading tank with nitrogen; pressing the resin in the loading tank into the adsorption column; reducing the injection speed or stopping the injection when the temperature is above 50°C; maintaining the pressure of the loading tank at 0.3-0.4 MPa during the injection process; after a predetermined amount of resin has been injected into the adsorption column, introducing silicon tetrachloride into the adsorption column again; and allowing the resin to soak and swell for a predetermined time to complete the resin treatment. The present invention can improve loading efficiency, reduce safety risks, and prevent the resin from agglomerating.

Description

Technical Field

[0001] The present invention relates to the technical field of polysilicon production, and in particular to a method for filling an adsorption / deproportionation resin. Background Art

[0002] With the promotion of adsorption resins in the polysilicon industry, resin usage continues to increase, and equipment is becoming larger. Due to factors such as catalyst properties and water content, the mixing of resin and chlorosilane during adsorption / deproportionation resin loading releases heat, posing a significant risk.

[0003] In the existing filling technology, the resin that has been dried and qualified is loaded into the adsorption column. After nitrogen replacement, the dew point and oxygen content of the replacement gas are analyzed and qualified. Then, cold silicon tetrachloride is introduced into the adsorption column to swell the resin. During the swelling process, if a rapid temperature rise occurs, the introduction of silicon tetrachloride is stopped in time. After the temperature and pressure return to normal, silicon tetrachloride is introduced again for swelling. In this filling method, silicon tetrachloride is introduced into the adsorption column filled with resin for swelling. During the filling process, the temperature rise and pressure are difficult to control. If the temperature is too high, the resin will be damaged and deactivated. If the pressure is too high, chlorosilane and resin will leak and catch fire, which poses a great safety risk. The swelling process is slow, time-consuming and labor-intensive. At the same time, the resin is prone to agglomeration, which greatly affects the unloading of the resin after it expires. Especially after the equipment is large-scale, the capacity of the adsorption column is large. This method has extremely high safety risks of overheating and overpressure. Summary of the Invention

[0004] In view of this, the present invention provides a method for filling an adsorption / deproportionation resin, the main purpose of which is to improve filling efficiency, improve resin filling quality, reduce safety risks, and improve the agglomeration phenomenon during the resin swelling process.

[0005] To achieve the above objectives, the present invention mainly provides the following technical solutions:

[0006] In one aspect, an embodiment of the present invention provides a method for loading an adsorption / deproportionation resin, comprising:

[0007] Add resin to the filling tank, with the volume of resin accounting for 70-90% of the filling tank volume;

[0008] Introduce nitrogen into the filling tank to dry it until the moisture content of the resin meets the requirements;

[0009] Add silicon tetrachloride to the adsorption column in an amount of 1 / 2 to 2 / 3 of the total volume of the adsorption column, and release the pressure to below 0.03 MPa;

[0010] Repressurize the filling tank with nitrogen to at least 0.3MPa;

[0011] Press the resin in the filling tank into the adsorption column; when the temperature is higher than 50°C, reduce the pressing speed or stop pressing; during the pressing process, maintain the pressure of the filling tank at 0.3-0.4MPa; maintain the pressure of the adsorption column at no more than 0.1MPa;

[0012] After a predetermined amount of resin is pressed into the adsorption column, silicon tetrachloride is introduced into the adsorption column again; the resin is soaked and swelled for a predetermined time to complete the resin treatment.

[0013] Furthermore, the filling tank is dried until the nitrogen dew point in the filling tank is less than -60°C and the oxygen content in the filling tank is less than 0.1%; and nitrogen pressure is maintained.

[0014] Furthermore, the speed at which the resin in the filling tank is pressed into the adsorption column is controlled automatically or manually;

[0015] After the resin in the filling tank is compressed, the filling tank is vented to 10-50 KPa and the filling tank is protected by nitrogen.

[0016] Furthermore, the adsorption column is one or more;

[0017] The filling tank and the adsorption column are connected through a metal hose.

[0018] Further, after adding silicon tetrachloride to the adsorption column, the pressure was released to 0.02 MPa;

[0019] The filling tank is pressurized with nitrogen to 0.3 MPa.

[0020] On the other hand, an embodiment of the present invention provides a filling device for adsorption / deproportionation resin, comprising: a filling tank and an adsorption column;

[0021] The top of the filling tank is provided with a material inlet for adding resin material;

[0022] The filling tank is provided with a nitrogen pressure replenishing port; the nitrogen pressure replenishing port is used to connect to a nitrogen source;

[0023] The filling tank is provided with a pressure relief port 1;

[0024] The filling tank is provided with a pressure transmitter 1 for detecting the pressure in the filling tank;

[0025] The upper, middle and lower parts of the filling tank are respectively provided with temperature transmitters 1 for detecting the temperature inside the filling tank;

[0026] The bottom of the filling tank is provided with a material outlet;

[0027] A material inlet is provided at the bottom of the adsorption column;

[0028] The bottom of the adsorption column is provided with a drain port;

[0029] The top and bottom of the adsorption column are respectively provided with a second pressure transmitter for detecting the pressure in the adsorption column;

[0030] The upper, middle and lower parts of the adsorption column are respectively provided with a second temperature transmitter for detecting the temperature inside the adsorption column;

[0031] The adsorption column is provided with an inner extension tube; the inner extension tube extends into the adsorption column; the resin feeding port of the inner extension tube is located at the top of the adsorption column; the resin feeding port is connected to the material outlet of the filling tank through a connecting pipe;

[0032] A material discharge port is provided on the top of the adsorption column;

[0033] A second pressure relief port is provided on the top of the adsorption column.

[0034] Furthermore, a temperature meter is provided on the filling tank for displaying the temperature inside the filling tank;

[0035] The filling tank is provided with an on-site pressure gauge for displaying the pressure inside the filling tank.

[0036] Furthermore, there are multiple adsorption columns;

[0037] The resin feeding ports of the plurality of adsorption columns are respectively connected to the material outlets of the filling tank.

[0038] Furthermore, the connecting pipe is a metal hose.

[0039] Furthermore, the lower end of the inner extension tube extends to the lower part of the adsorption column.

[0040] By means of the above technical solution, the method for loading the adsorption / deproportionation resin of the present invention has at least the following advantages:

[0041] It can improve filling efficiency, improve resin filling quality, reduce safety risks, and solve the problem of resin agglomeration.

[0042] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and implement it according to the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 A schematic diagram of a device for loading an adsorption / deproportionation resin according to an embodiment of the present invention;

[0044] Figure 2 for Figure 1 A partial enlarged schematic diagram;

[0045] Figure 3 for Figure 1 A partial enlarged schematic diagram.

[0046] As shown in the figure:

[0047] 1 is the filling tank, 1-1 is the nitrogen pressure replenishing port, 1-2 is the temperature transmitter 1, 1-3 is the material inlet, 1-4 is the temperature instrument, 1-5 is the on-site pressure gauge, 1-6 is the material outlet, 2 is the connecting pipe, 3 is the adsorption column, 3-1 is the pressure transmitter 2, 3-2 is the temperature transmitter 2, 3-3 is the inner extension pipe, 3-31 is the resin feeding port, 3-4 is the material inlet, 3-5 is the drain port, 3-6 is the material discharge port, and 3-7 is the pressure relief port 2. DETAILED DESCRIPTION

[0048] To further illustrate the technical means and effects employed by the present invention to achieve its intended objectives, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention is provided in conjunction with the accompanying drawings and preferred embodiments. In the following description, different references to "one embodiment" or "embodiment" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.

[0049] In one aspect, an embodiment of the present invention provides a method for loading an adsorption / deproportionation resin, comprising:

[0050] Add the resin to the filling tank, and the volume of the resin accounts for 70% to 90% of the volume of the filling tank; preferably, the volume of the resin accounts for 80% of the volume of the filling tank to leave room for expansion.

[0051] Nitrogen is introduced into the filling tank to dry the filling tank until the moisture content of the resin meets the requirements; preferably, the filling tank is dried until the nitrogen dew point in the filling tank is less than -60°C and the oxygen content in the filling tank is less than 0.1%; and nitrogen pressure is maintained.

[0052] Add silicon tetrachloride to the adsorption column in an amount of 1 / 2 to 2 / 3 of the total volume of the adsorption column, and release the pressure to below 0.03 MPa; preferably, after adding silicon tetrachloride to the adsorption column, release the pressure to 0.02 MPa to reduce the pressure inside the adsorption column.

[0053] The filling tank is pressurized with nitrogen to at least 0.3 MPa; The filling tank is pressurized with nitrogen to 0.3 MPa so that the resin can be smoothly pressed into the adsorption column.

[0054] Press the resin from the tank into the adsorption column. When the temperature exceeds 50°C, reduce the injection speed or stop the injection. During the injection process, maintain the tank pressure at 0.3-0.4 MPa. Maintain the pressure in the adsorption column below 0.1 MPa. If it exceeds 0.1 MPa, open the pressure relief port at the top of the adsorption column to release the pressure. The speed at which the resin from the tank is injected into the adsorption column is automatically or manually controlled. After the resin in the tank is fully injected, vent the tank to 10-50 kPa and protect the tank with nitrogen. After the predetermined amount of resin is injected into the adsorption column, silicon tetrachloride is again introduced into the adsorption column until the column is full. After the resin is allowed to soak and swell for a predetermined period of time, preferably 24 hours, the resin treatment is complete and the system can be put into use.

[0055] After the resin filling tank is pressurized, open the top pressure relief valve to release the filling tank to normal pressure. There are one or more adsorption columns. The filling tank and the adsorption column are connected by a metal hose to facilitate switching between multiple adsorption columns. If there are multiple adsorption columns, repeat the above steps to operate the next filling tank.

[0056] The embodiments of the present invention provide a method for filling an adsorption / deproportionation resin, which greatly improves filling efficiency and reduces labor intensity.

[0057] The embodiments of the present invention provide a method for filling an adsorption / deproportionation resin, which can improve filling efficiency, improve resin filling quality, solve the agglomeration phenomenon during the resin swelling process, and reduce safety risks.

[0058] The embodiments of the present invention provide a method for filling an adsorption / deproportionation resin, which solves the problem of uncontrollable temperature rise of the resin during the swelling process of silicon tetrachloride, and protects the resin from deactivation and agglomeration during the filling and swelling process.

[0059] The embodiments of the present invention provide a method for filling an adsorption / deproportionation resin, which solves the problem of uncontrollable pressure of the resin during the swelling process of silicon tetrachloride, avoids overpressure of the container during the filling process, which may cause equipment damage and personal injury, and controls the safety risks of the filling process.

[0060] The embodiments of the present invention provide a method for filling an adsorption / deproportionation resin, which greatly improves the resin filling efficiency, effectively solves the resin filling swelling problem after the adsorption column is enlarged, and solves the problem of resin agglomeration during the swelling process.

[0061] like Figures 1 to 3 As shown, an embodiment of the present invention provides a filling device for adsorption / deproportionation resin, including: a filling tank 1 and an adsorption column 3; a material inlet 1-3 is provided on the top of the filling tank 1 for adding resin material; the material inlet 1-3 is used to add resin, and purchased resin is added through the material inlet 1-3; the material inlet 1-3 can be a manhole to facilitate operation.

[0062] Filling tank 1 is provided with a nitrogen boost port 1-1. This port is used to connect to a nitrogen source to introduce nitrogen into filling tank 1 for nitrogen boosting during resin pressing. A nitrogen boost valve is provided on this port. Opening this valve boosts the nitrogen pressure in filling tank 1 to 0.3 MPa.

[0063] Filling tank 1 is equipped with a pressure relief port 1, located at the top of the tank. A pressure relief valve 1 is installed on the port to relieve pressure within the tank. After the resin is added, the pressure in the tank 1 is released. If the resin moisture content is below standard, cold nitrogen gas can be introduced to dry the resin until the moisture content meets the requirements, fully ensuring filling safety.

[0064] The filling tank 1 is provided with a pressure transmitter 1 for detecting the pressure inside the filling tank 1 ; the pressure transmitter 1 is provided at the top of the filling tank 1 to monitor the pressure of the filling tank 1 when the resin is pressed.

[0065] Temperature transmitters 1-2 are located at the top, middle, and bottom of the tank 1 to monitor the temperature inside. A material outlet 1-6 is located at the bottom of the tank 1 for discharging resin. This outlet 1-6 can be connected to nitrogen gas via a pipeline to dry or replace the resin in the tank 1.

[0066] A material inlet 3-4 is provided at the bottom of the adsorption column 3; silicon tetrachloride with a purity greater than 99% is added through the material inlet 3-4, and the added amount is 1 / 2 to 2 / 3 of the total volume of the adsorption column 3.

[0067] A drain port 3 - 5 is provided at the bottom of the adsorption column 3 ; a drain valve is provided on the drain port 3 - 5 to control the opening and closing of the drain port 3 - 5 .

[0068] The top and bottom of the adsorption column 3 are respectively provided with a pressure transmitter 3-1 for detecting the pressure inside the adsorption column 3;

[0069] The upper, middle and lower parts of the adsorption column 3 are respectively provided with temperature transmitters 3-2 for detecting the temperature inside the adsorption column 3;

[0070] Adsorption column 3 is equipped with an inner extension tube 3-3, which extends into the adsorption column 3. A resin feed port 3-31 of the inner extension tube 3-3 is located at the top of the adsorption column 3. A feeding valve is provided on the resin feed port 3-31 to regulate the flow rate of the resin. During the swelling process, the temperature and pressure at various points within the adsorption column 3 are monitored at all times, and the opening of the feeding valve is used to control the rate of resin addition. The resin feed port 3-31 is connected to the material outlet 1-6 via a connecting tube 2.

[0071] A material discharge port 3-6 is provided at the top of the adsorption column 3 to discharge the material.

[0072] A pressure relief port 3-7 is provided at the top of the adsorption column 3 to relieve pressure when the pressure exceeds a predetermined value.

[0073] Embodiments of the present invention provide a filling device for adsorption / deproportionation resin, which can improve filling efficiency, improve resin filling quality, solve the problem of resin agglomeration during the swelling process, and reduce safety risks.

[0074] As a preference of the above embodiment, a temperature meter 1-4 is provided on the filling tank 1 for displaying the temperature inside the filling tank 1 so as to facilitate the operator to observe at any time.

[0075] The filling tank 1 is provided with on-site pressure gauges 1-5 for displaying the pressure inside the filling tank 1 so that the operator can observe it at any time. The filling tank 1 is also called a feeding tank.

[0076] As a preference of the above embodiment, there are multiple adsorption columns 3; the resin feeding ports 3-31 of the multiple adsorption columns 3 are respectively connected to the material outlets 1-6 of the filling tank 1, so that the material in the filling tank 1 can be pressed into the multiple adsorption columns 3; they can be pressed into different adsorption columns 3 separately, or they can be pressed into multiple adsorption columns 3 at the same time, which can improve the pressing efficiency.

[0077] As a preference of the above embodiment, the connecting pipe 2 is a metal hose, so that different adsorption columns 3 can be connected through the connecting pipe 2 to facilitate switching between different adsorption columns 3.

[0078] As a preferred embodiment of the above, the lower end of the inner extension tube 3-3 extends to the lower part of the adsorption column 3, so that when adding resin, the resin is directly passed into the bottom of the adsorption column 3, and then the silicon tetrachloride liquid is added.

[0079] The embodiments of the present invention provide a device for filling an adsorption / deproportionation resin, wherein the temperature rise during the filling process is small and safe and controllable;

[0080] An embodiment of the present invention provides a filling device for adsorption / deproportionation resin, wherein during the filling process, the pressure change tends to be slow and the pressure is controllable.

[0081] Further explanation, although the terms first, second, etc. can be used to describe various elements in this article, these terms should not limit these elements. These terms are only used to distinguish one element from another element. For example, the first element can be called the second element, and, similarly, the second element can be called the first element, and these terms are only used to distinguish one element from another element. This does not depart from the scope of exemplary embodiments. Similarly, element one and element two do not represent the order of elements, and these terms are only used to distinguish one element from another element. As used herein, the term "and / or" includes any combination and all combinations of one or more associated listed items.

[0082] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Any simple modifications, equivalent changes and modifications made to the above embodiment based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A method for filling an adsorption / deproportionation resin, characterized in that: include: S1: Add resin into the filling tank, and the volume of the resin occupies 70-90% of the volume of the filling tank; S2: nitrogen is introduced into the filling tank to dry the filling tank until the moisture content of the resin meets the requirements; S3: Add silicon tetrachloride to the adsorption column in an amount of 2 / 3 of the total volume of the adsorption column, and release the pressure to below 0.03 MPa; S4: Pressurize the filling tank with nitrogen to at least 0.3 MPa; S5: Press the resin in the filling tank into the adsorption column; when the temperature is higher than 50°C, reduce the pressing speed or stop pressing; during the pressing process, maintain the pressure of the filling tank at 0.3-0.4MPa; maintain the pressure of the adsorption column at no more than 0.1MPa; S6: After a predetermined amount of resin is pressed into the adsorption column, silicon tetrachloride is introduced into the adsorption column again; the resin is soaked and swelled for a predetermined time to complete the resin treatment.

2. The method for filling the adsorption / deproportionation resin according to claim 1, characterized in that: In S2, the filling tank is dried until the nitrogen dew point in the filling tank is less than -60°C and the oxygen content in the filling tank is less than 0.1%, and nitrogen pressure is maintained.

3. The method for filling the adsorption / deproportionation resin according to claim 1, characterized in that: In S5, the speed at which the resin in the filling tank is pressed into the adsorption column is controlled automatically or manually; In S5, after the resin in the filling tank is completely compressed, the filling tank is vented to 10-50 KPa and nitrogen is protected in the filling tank.

4. The method for filling the adsorption / deproportionation resin according to claim 1, characterized in that: There are one or more adsorption columns; The filling tank and the adsorption column are connected through a metal hose.

5. The method for filling the adsorption / deproportionation resin according to claim 1, characterized in that: In S3, after adding silicon tetrachloride to the adsorption column, the pressure is released to 0.02 MPa; In S4, the filling tank is pressurized with nitrogen to 0.3 MPa.

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