A device for discharging anti-disproportionation resin and adsorption resin and a method of using the device
By designing an automated resin unloading device for polycrystalline silicon production equipment, using silicon tetrachloride replacement and nitrogen replacement technologies, the problems of low efficiency and high safety risks in the existing technology are solved, and high efficiency and safety are achieved The resin discharge process saves labor costs.
Patent Information
- Application Number
- CN202011370777.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2020-11-30
- Publication Date
- 2025-02-25
- Estimated Expiration
- 2040-11-30
AI Technical Summary
In existing polysilicon production equipment, the resin unloading process is inefficient, has high safety risks, and requires a large amount of manpower, resulting in high labor costs and frequent safety accidents.
Design a device that includes adsorption components and discharge components, replace trichlorosilicon and dichlorosilicon by silicon tetrachloride, and treat resins with nitrogen replacement and hydrolyzed components to achieve automated control and reduce human participation.
It improves the efficiency of resin unloading, reduces safety risks, saves labor costs, and shortens the time for nitrogen replacement to prevent static electricity and explosion accidents.
Smart Images

Figure CN112494990B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of polysilicon production equipment, and in particular to a device for discharging anti-disproportionation resin and adsorption resin and a method for using the device. Background Art
[0002] In the past decade, the photovoltaic industry has developed rapidly in China. As the front end of the photovoltaic industry, the scale of polysilicon has also grown from thousands of tons to the current 50,000 tons. Since polysilicon requires extremely high purity, the removal of impurities in the raw materials during the production process is mainly carried out by distillation. Considering the limitations of operating costs and distillation purification accuracy, the by-product trichlorosilane in the production process needs to be processed, and various manufacturers have introduced a large amount of adsorption resins. At the same time, the by-product dichlorosilane in the production process needs to be processed, and anti-disproportionate resins will be used.
[0003] When the scale of a single polysilicon unit is at the thousand-ton level, the capacity of the adsorption and deproportionation resins used is relatively small. As the scale of a single unit becomes larger and larger, the capacity of the adsorption and deproportionation device also becomes larger and larger. Currently, the industry can load dozens of cubic meters of resin per unit. When the resin needs to be replaced by a waste discharge system, the process of replacing and unloading the resin is time-consuming, labor-intensive, and inefficient. There are also safety risks. From the perspective of polysilicon manufacturers in recent years, there has been no shortage of safety accidents caused by resin unloading.
[0004] In the prior art, the resin unloading method mainly includes the following two stages:
[0005] The first stage: After the service life of the resin ends, nitrogen is used directly to replace the process medium with the three wastes. After the sampling is qualified, the resin is discharged. In this stage, the single adsorption column is small, the replacement and discharge time is short, the manpower is not much, and there are fewer safety accidents. As the capacity of the adsorption column increases, the replacement time of this method becomes longer and longer, and a large amount of manpower cost is required. At the same time, the risk gradually increases. The phenomenon of resin burning often occurs during the discharge process, so the resin unloading develops to the second stage.
[0006] The second stage: After the service life of the resin is over, the trichlorosilane medium in the adsorption column is first replaced with silicon tetrachloride. After the silicon tetrachloride concentration is greater than 99% after analysis and sampling, nitrogen is used to replace the silicon tetrachloride in the adsorption column to the three wastes for treatment. Since silicon tetrachloride is non-flammable, the risk is relatively small compared to the first stage. However, after the capacity of the adsorption column is further increased, if you want to completely replace the adsorption column with nitrogen, it will take a long time, possibly up to 20 days. The nitrogen flow blows the resin for a long time, and the resin keeps rolling and rubbing inside, which will generate static electricity. Since the resin itself is flammable, static electricity can easily cause the resin to burn and decompose. Summary of the invention
[0007] In view of this, an embodiment of the present invention provides a device for unloading anti-disproportionation resin and adsorption resin and a method for using the device. The main purpose is to provide a device for unloading anti-disproportionation resin and adsorption resin that can improve the efficiency of unloading adsorption resin and anti-disproportionation resin and the safety of the unloading process, while saving labor costs.
[0008] In order to achieve the above object, the present invention mainly provides the following technical solutions:
[0009] On the one hand, an embodiment of the present invention provides a device for discharging anti-disproportionation resin and adsorption resin, the device comprising:
[0010] An adsorption component, the adsorption component comprises an adsorption tank body, a silicon tetrachloride feed pipe, a first silicon tetrachloride discharge pipe and a second silicon tetrachloride discharge pipe, the silicon tetrachloride feed pipe is connected to the adsorption tank body and is used to pass silicon tetrachloride into the adsorption tank body, the first silicon tetrachloride discharge pipe and the second silicon tetrachloride discharge pipe are respectively connected to the adsorption tank body;
[0011] A discharge component, the discharge component comprises a discharge tank body, a silicon tetrachloride collecting box, a filter, a hydrolysis component and a first nitrogen feed pipe, the other end of the second silicon tetrachloride discharge pipe is connected to the discharge tank body, a first valve is arranged on the second silicon tetrachloride discharge pipe, the first nitrogen feed pipe is connected to the discharge tank body, a second valve is arranged on the first nitrogen feed pipe, one end of the filter is connected to the discharge tank body, and the other end is connected to the silicon tetrachloride collecting box, a third valve is arranged between the filter and the silicon tetrachloride collecting box, a resin discharge pipe is arranged between the discharge tank body and the hydrolysis component, and a fourth valve is arranged on the resin discharge pipe.
[0012] Furthermore, the first nitrogen feed pipe and the second silicon tetrachloride discharge pipe are respectively connected to the top of the unloading tank body.
[0013] Furthermore, the resin discharge pipe is connected to the bottom of the discharge tank.
[0014] Furthermore, a control component is respectively connected to the first valve, the second valve, the third valve and the fourth valve, and is used to control the opening or closing of the first valve, the second valve, the third valve and the fourth valve respectively.
[0015] Furthermore, a second nitrogen feed pipe is connected to the resin discharge pipe and is used to feed nitrogen into the resin discharge pipe.
[0016] Furthermore, an explosion vent is provided at the top of the unloading tank body, and a bursting piece is provided on the explosion vent.
[0017] Furthermore, a visual window is provided on a side of the resin discharge pipe close to the hydrolysis component.
[0018] On the other hand, an embodiment of the present invention further provides a method for using a device for discharging an anti-disproportionated resin and an adsorption resin, the method comprising the following steps:
[0019] (1) Close the inlet valve and outlet valve of the adsorption tank;
[0020] (2) Opening the silicon tetrachloride feed pipe and the first silicon tetrachloride discharge pipe, passing silicon tetrachloride with a purity higher than 99% into the adsorption tank through the silicon tetrachloride feed pipe to replace the trichlorosilane and dichlorosilane in the adsorption tank, and when the purity of silicon tetrachloride discharged from the first silicon tetrachloride discharge pipe is higher than 99%, closing the first silicon tetrachloride discharge pipe;
[0021] (3) Open the first valve to allow part of the solid-liquid mixture of silicon tetrachloride and resin to enter the unloading tank through the second silicon tetrachloride discharge pipe, and open the third valve to allow silicon tetrachloride to enter the silicon tetrachloride collection box through the filter;
[0022] (4) Close the first valve and open the second valve to allow nitrogen to enter the unloading tank body, and replace the silicon tetrachloride in the unloading tank body with nitrogen. When the silicon tetrachloride in the unloading tank body is replaced by nitrogen, close the third valve and open the fourth valve to pass the resin in the unloading tank body into the hydrolysis component;
[0023] (5) After the resin in the unloading tank is completely discharged, the fourth valve is closed, and steps 3 and 4 are repeated in sequence until the resin in the adsorption tank is completely discharged.
[0024] Furthermore, in step 4, the time for replacing the silicon tetrachloride in the unloading tank with nitrogen is 20 minutes to 40 minutes.
[0025] Furthermore, in step 4, the time for passing the resin in the unloading tank into the hydrolysis component is 10 minutes to 20 minutes.
[0026] Compared with the prior art, the present invention has the following technical effects:
[0027] In the technical solution provided by the embodiment of the present invention, the function of the adsorption component is to replace trichlorosilane and dichlorosilane with silicon tetrachloride, the adsorption component includes an adsorption tank body, a silicon tetrachloride feed pipe, a first silicon tetrachloride discharge pipe and a second silicon tetrachloride discharge pipe, the silicon tetrachloride feed pipe is connected to the adsorption tank body and is used to pass silicon tetrachloride into the adsorption tank body, the first silicon tetrachloride discharge pipe and the second silicon tetrachloride discharge pipe are respectively connected to the adsorption tank body; the function of the discharge component is to process the resin, the discharge component includes a discharge tank body, a silicon tetrachloride collection box, a filter, a hydrolysis component and a first nitrogen feed pipe, the other end of the second silicon tetrachloride discharge pipe is connected to the discharge tank body, a first valve is arranged on the second silicon tetrachloride discharge pipe, and the first nitrogen feed pipe is connected to the discharge tank body. A second valve is arranged on the first nitrogen feed pipe, one end of the filter is connected to the discharge tank, and the other end is connected to the silicon tetrachloride collection box, a third valve is arranged between the filter and the silicon tetrachloride collection box, a resin discharge pipe is arranged between the discharge tank and the hydrolysis component, and a fourth valve is arranged on the resin discharge pipe. Compared with the prior art, the trichlorosilane medium in the adsorption column is replaced cleanly with silicon tetrachloride, and after analyzing and sampling that the silicon tetrachloride concentration is greater than 99%, nitrogen is used to replace the silicon tetrachloride in the adsorption column to the three wastes for treatment. Since silicon tetrachloride is non-flammable, the risk is relatively small compared to the first stage. However, after the capacity of the adsorption column is further increased, if you want to completely replace the adsorption column with nitrogen, it will take a long time, which may be as long as 20 days. Nitrogen gas When the resin is blown for a long time, the resin will keep rolling and rubbing inside, which will generate static electricity. Since the resin itself is easy to burn, once the static electricity causes the resin to burn and decompose, the adsorption column will have the risk of explosion. In this technical scheme, silicon tetrachloride with a purity higher than 99% is first introduced into the adsorption tank through the silicon tetrachloride feed pipe to replace the trichlorosilane and dichlorosilane in the adsorption tank. When the purity of silicon tetrachloride discharged from the first silicon tetrachloride discharge pipe is higher than 99%, the first silicon tetrachloride discharge pipe is closed, and then the first valve is opened to allow part of the solid-liquid mixture of silicon tetrachloride and resin to enter the discharge tank through the second silicon tetrachloride discharge pipe, and the third valve is opened to allow silicon tetrachloride to pass through the filter into the silicon tetrachloride collection box, and then the first valve is closed and the second valve is opened. The valve allows nitrogen to enter the unloading tank body, and replaces the silicon tetrachloride in the resin with nitrogen. When the silicon tetrachloride in the unloading tank body is completely replaced by nitrogen, the third valve is closed, and the fourth valve is opened to pass the resin in the unloading tank body into the hydrolysis component; after the resin in the unloading tank body is completely discharged, the fourth valve is closed, and the first valve and the third valve are opened again to cycle until the resin in the adsorption tank body is completely discharged. The opening and closing of the valves in the whole process are completed by the automatic valve according to the sequential control program, and no special person is required to be on duty, which not only saves a lot of manpower and improves the unloading efficiency, but also shortens the replacement time of nitrogen, prevents nitrogen from blowing the resin balls for a long time, and reduces the generation of static electricity, thereby achieving the technical effect of preventing explosions, and then achieving the role of protecting personnel and property. BRIEF DESCRIPTION OF THE DRAWINGS
[0028] Figure 1 A schematic structural diagram of a device for discharging anti-disproportionation resin and adsorption resin provided in an embodiment of the present invention. DETAILED DESCRIPTION
[0029] The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.
[0030] On the one hand, if Figure 1 As shown, an embodiment of the present invention provides a device for discharging anti-disproportionation resin and adsorption resin, the device comprising:
[0031] An adsorption component, the adsorption component includes an adsorption tank body 11, a silicon tetrachloride feed pipe 12, a first silicon tetrachloride discharge pipe 13 and a second silicon tetrachloride discharge pipe 14, the silicon tetrachloride feed pipe 12 is connected to the adsorption tank body 11, and is used to pass silicon tetrachloride into the adsorption tank body, and the first silicon tetrachloride discharge pipe 13 and the second silicon tetrachloride discharge pipe 14 are respectively connected to the adsorption tank body 11;
[0032] The unloading component includes a unloading tank body 21, a silicon tetrachloride collecting box 22, a filter 23, a hydrolysis component 24 and a first nitrogen feed pipe 25. The other end of the second silicon tetrachloride discharge pipe 14 is connected to the unloading tank body 21, and a first valve 51 is arranged on the second silicon tetrachloride discharge pipe 14. The first nitrogen feed pipe 25 is connected to the unloading tank body 21, and a second valve 52 is arranged on the first nitrogen feed pipe 25. One end of the filter 23 is connected to the unloading tank body 21, and the other end is connected to the silicon tetrachloride collecting box 22. A third valve 53 is arranged between the filter 23 and the silicon tetrachloride collecting box 22. A resin discharge pipe 26 is arranged between the unloading tank body 21 and the hydrolysis component 24, and a fourth valve 54 is arranged on the resin discharge pipe 26.
[0033] In the technical solution provided in the embodiment of the present invention, the function of the adsorption component is to replace trichlorosilane and dichlorosilane, and the adsorption component includes an adsorption tank body 11, a silicon tetrachloride feed pipe 12, a first silicon tetrachloride discharge pipe 13 and a second silicon tetrachloride discharge pipe 14, the silicon tetrachloride feed pipe 12 is connected to the adsorption tank body 11, and is used to pass silicon tetrachloride into the adsorption tank body, and the first silicon tetrachloride discharge pipe 13 and the second silicon tetrachloride discharge pipe 14 are respectively connected to the adsorption tank body 11; the function of the discharge component is to process the resin, and the discharge component includes a discharge tank body 21, a silicon tetrachloride collecting box 22, a filter 23, a hydrolysis component 24 and a first nitrogen feed pipe 25, and the other end of the second silicon tetrachloride discharge pipe 14 The invention is connected to the unloading tank 21, a first valve 51 is arranged on the second silicon tetrachloride discharge pipe 14, a first nitrogen feed pipe 25 is connected to the unloading tank 21, a second valve 52 is arranged on the first nitrogen feed pipe 25, one end of the filter 23 is connected to the unloading tank 21, and the other end is connected to the silicon tetrachloride collection box 22, a third valve 53 is arranged between the filter 23 and the silicon tetrachloride collection box 22, a resin discharge pipe 26 is arranged between the unloading tank 21 and the hydrolysis component 24, and a fourth valve 54 is arranged on the resin discharge pipe 26. Compared with the prior art, the trichlorosilane medium in the adsorption column is replaced cleanly with silicon tetrachloride, and after the silicon tetrachloride concentration is greater than 99% after analysis and sampling, nitrogen is used to clean the adsorption column. The silicon tetrachloride in the column is replaced with three wastes for treatment. Since silicon tetrachloride is non-flammable, the risk is relatively small compared to the first stage. However, after the capacity of the adsorption column is further increased, if you want to completely replace the adsorption column with nitrogen, it will take a long time, which may be as long as 20 days. The nitrogen gas flow blows the resin for a long time, and the resin keeps rolling and rubbing inside, which will generate static electricity. Since the resin itself is easy to burn, once the static electricity causes the resin to burn and decompose, the adsorption column will have the risk of explosion. In this technical solution, silicon tetrachloride with a purity higher than 99% is first introduced into the adsorption tank body 11 through the silicon tetrachloride feed pipe 12 and replaces the trichlorosilane and dichlorosilane in the adsorption tank body 11. When the first silicon tetrachloride discharge pipe When the purity of the silicon tetrachloride discharged from the discharging tank 21 is higher than 99%, the first silicon tetrachloride discharge pipe 13 is closed, and then the first valve 51 is opened to allow part of the solid-liquid mixture of silicon tetrachloride and resin to enter the discharging tank 21 through the second silicon tetrachloride discharge pipe 14, and the third valve 53 is opened to allow silicon tetrachloride to enter the silicon tetrachloride collecting box 22 through the filter 23, and then the first valve 51 is closed, and the second valve 52 is opened to allow nitrogen to enter the discharging tank 21, and the silicon tetrachloride in the discharging tank 21 is replaced with nitrogen. When the silicon tetrachloride in the discharging tank 21 is replaced with nitrogen, the third valve 53 is closed, and the fourth valve 54 is opened to pass the resin in the discharging tank 21 into the hydrolysis component 24;After the resin in the unloading tank 21 is discharged, the fourth valve 54 is closed, and the first valve 51 and the third valve 53 are opened again to cycle until the resin in the adsorption tank 11 is discharged. This can not only shorten the nitrogen replacement time, improve the discharge efficiency, and save manpower, but also prevent nitrogen from blowing the resin balls for a long time, reduce the generation of static electricity, thereby achieving the technical effect of preventing explosions, and further achieving the effect of protecting personnel and property. ;
[0034] The function of the adsorption component is to replace trichlorosilane and dichlorosilane. The adsorption component includes an adsorption tank body 11, a silicon tetrachloride feed pipe 12, a first silicon tetrachloride discharge pipe 13 and a second silicon tetrachloride discharge pipe 14. The silicon tetrachloride feed pipe 12 is connected to the adsorption tank body 11 and is used to pass silicon tetrachloride into the adsorption tank body. The first silicon tetrachloride discharge pipe 13 and the second silicon tetrachloride discharge pipe 14 are respectively connected to the adsorption tank body 11. The silicon tetrachloride feed pipe 12 is arranged on the side of the adsorption tank body 11, the first silicon tetrachloride discharge pipe 13 is arranged at the bottom of the adsorption tank body 11, and the second silicon tetrachloride discharge pipe 14 is arranged at the top of the adsorption tank body 11. In addition, there is no filter cap to filter the silicon tetrachloride, so that the resin can pass through the second silicon tetrachloride discharge pipe 14. After entering the unloading tank 21, a plurality of pressure detection gauges 3 and temperature detection gauges 4 will be arranged around the adsorption tank 11 to display the temperature and pressure value in the adsorption tank 11 in real time, and electromagnetic valves or other types of valves will be arranged on the silicon tetrachloride feed pipe 12 and the first silicon tetrachloride discharge pipe 13 to facilitate automatic control of the entry and discharge of silicon tetrachloride. Of course, the adsorption tank 11 usually adopts a traditional adsorption column, so the adsorption tank 11 will also be provided with their feed pipe and discharge pipe, which will not be described in detail here; the function of the unloading component is to process the resin, and the unloading component includes the unloading tank 21, the silicon tetrachloride collection box 22, the filter 23, the hydrolysis component 24 and the first nitrogen feed pipe 25, and the other of the second silicon tetrachloride discharge pipe 14 The first end of the filter 23 is connected to the unloading tank body 21, the second silicon tetrachloride discharge pipe 14 is provided with a first valve 51, the first nitrogen feed pipe 25 is connected to the unloading tank body 21, the first nitrogen feed pipe 25 is provided with a second valve 52, one end of the filter 23 is connected to the unloading tank body 21, and the other end is connected to the silicon tetrachloride collecting box 22, a third valve 53 is provided between the filter 23 and the silicon tetrachloride collecting box 22, a resin discharge pipe 26 is provided between the unloading tank body 21 and the hydrolysis component 24, and a fourth valve 54 is provided on the resin discharge pipe 26, a plurality of pressure detection gauges 3 and temperature detection gauges 4 are provided on the unloading tank body 21, and the temperature and pressure value in the unloading tank body 21 are displayed in real time, the second silicon tetrachloride discharge pipe 14 is connected to the top of the unloading tank body 21, and the first Valve 51, silicon tetrachloride feed pipe 12 is continuously introduced into adsorption tank 11, and the characteristic of resin floating in silicon tetrachloride is utilized to allow silicon tetrachloride and resin to enter into discharge tank 21 through second silicon tetrachloride discharge pipe 14, and the third valve 53 is opened, silicon tetrachloride enters silicon tetrachloride collection box 22 through filter 23, and resin is intercepted by filter 23 and stays in discharge tank 21, and after resin and silicon tetrachloride enter discharge tank 21 for a certain period of time, the first valve 51 is closed, and the certain period of time referred to here is usually about 30 minutes, and can be adjusted according to the volume of discharge tank 21 and overflow time, and then the second valve 52 is opened, and nitrogen is introduced into discharge tank 21,The first nitrogen feeding pipe 25 is connected to the top of the unloading tank body 21, so that nitrogen enters from the top of the unloading tank body 21, and the silicon tetrachloride in the unloading tank body 21 is replaced by nitrogen. When the silicon tetrachloride in the unloading tank body 21 is replaced, the third valve 53 is closed, and the fourth valve 54 is opened, and the nitrogen is discharged from the bottom, which can reduce the static electricity accumulation of the resin balls due to the rolling friction. At the same time, the resin is pressed into the hydrolysis tank by the nitrogen pressure. After the resin in the unloading tank body 21 is discharged, the fourth valve 54 is closed, and the third valve 53 is opened and closed in a cycle. A valve 51 is used to pass part of the silicon tetrachloride and resin in the adsorption tank 11 into the discharge tank 21 again until all the resin in the adsorption tank 11 is discharged. In this technical solution, silicon tetrachloride with a purity higher than 99% is firstly passed into the adsorption tank 11 through the silicon tetrachloride feeding pipe 12 to replace the trichlorosilane and dichlorosilane in the adsorption tank 11. When the purity of silicon tetrachloride discharged from the first silicon tetrachloride discharge pipe 13 is higher than 99%, the first silicon tetrachloride discharge pipe 13 is closed, and then the first valve 51 is opened to make the silicon tetrachloride discharged from the first silicon tetrachloride discharge pipe 13 be discharged from the adsorption tank 11. Part of the solid-liquid mixture of silicon tetrachloride and resin enters the discharge tank 21 through the second silicon tetrachloride discharge pipe 14, and the third valve 53 is opened to allow silicon tetrachloride to enter the silicon tetrachloride collection box 22 through the filter 23, and then the first valve 51 is closed, and the second valve 52 is opened to allow nitrogen to enter the discharge tank 21, and the resin is hydrolyzed in the discharge tank 21. When the silicon tetrachloride in the discharge tank 21 is replaced with nitrogen, the third valve 53 is closed, and the fourth valve 54 is opened to pass the resin in the discharge tank 21 into the hydrolysis component 24; after the resin in the discharge tank 21 is discharged, the fourth valve 54 is closed, and the first valve 51 and the third valve 53 are opened again to cycle until the resin in the adsorption tank 11 is discharged. The entire valve opening and closing is automatically controlled by the control component, and no special person is required to be on duty, which improves efficiency and saves human resources. It can not only shorten the replacement time of nitrogen, but also prevent the static electricity generated by nitrogen blowing the resin balls for a long time, thereby achieving the technical effect of preventing explosions, and then achieving the role of protecting personnel and property.
[0035] Further, the control component is connected to the first valve 51, the second valve 52, the third valve 53 and the fourth valve 54 respectively, and is used to control the opening or closing of the first valve 51, the second valve 52, the third valve 53 and the fourth valve 54 respectively. In this embodiment, a control component is added, and the control component usually uses a PLC control system to control the opening or closing of the first valve 51, the second valve 52, the third valve 53 and the fourth valve 54, so as to achieve the technical effect of automatic control. Of course, the control component can also be connected to other valves, pressure detection gauges 3 and temperature detection gauges 4 and other components to monitor the data such as resin or flow in the unloading tank 21 or the adsorption tank 11 in real time, and upload the data to the master control system.
[0036] Further, a second nitrogen feed pipe 6 is connected to the resin discharge pipe 26 and is used to introduce nitrogen into the resin discharge pipe 26. In this embodiment, a second nitrogen feed pipe 6 is added, and the function of the second nitrogen feed pipe 6 is to introduce nitrogen into the resin discharge pipe 26 to prevent the connection position between the resin discharge pipe 26 and the hydrolysis tank from being blocked by silicon dioxide, thereby achieving the technical effect of keeping the resin discharge pipe 26 unobstructed.
[0037] Furthermore, the explosion vent 7 is arranged at the top of the discharge tank body 21, and a bursting disc is arranged on the explosion vent 7. In this embodiment, the explosion vent 7 is added, and the function of the explosion vent 7 is to discharge the pressure in the discharge tank body 21. When an uncontrollable state occurs in the discharge tank body 21, since the amount of resin in the discharge tank body 21 is small, the overpressure part can be easily discharged from the explosion vent 7, thereby avoiding safety accidents caused by equipment overpressure, thereby achieving the function of protecting equipment and personnel. A bursting disc is arranged on the explosion vent 7, and the bursting pressure of the bursting disc is lower than the design pressure of the discharge tank body 21, thereby achieving the technical effect of conveniently discharging the pressure in the discharge tank body 21.
[0038] Furthermore, a visual window 8 is provided on one side of the resin discharge pipe 26 close to the hydrolysis component 24. In this embodiment, the visual window 8 is added to facilitate personnel to observe whether the resin in the resin discharge pipe 26 has been discharged, and then open the first valve 51 to enter new resin.
[0039] On the other hand, an embodiment of the present invention further provides a method for using a device for discharging an anti-disproportionated resin and an adsorption resin, the method comprising the following steps:
[0040] (1) Close the inlet valve and outlet valve of the adsorption tank 11;
[0041] (2) Open the silicon tetrachloride feed pipe 12 and the first silicon tetrachloride discharge pipe 13, and introduce silicon tetrachloride with a purity higher than 99% into the adsorption tank body 11 through the silicon tetrachloride feed pipe 12 to replace the trichlorosilane and dichlorosilane in the adsorption tank body 11. When the purity of silicon tetrachloride discharged from the first silicon tetrachloride discharge pipe 13 is higher than 99%, close the first silicon tetrachloride discharge pipe 13;
[0042] (3) Open the first valve 51 to allow part of the solid-liquid mixture of silicon tetrachloride and resin to enter the discharge tank 21 through the second silicon tetrachloride discharge pipe 14, and open the third valve 53 to allow silicon tetrachloride to enter the silicon tetrachloride collection box 22 through the filter 23;
[0043] (4) Close the first valve 51 and open the second valve 52 to allow nitrogen to enter the unloading tank 21 and replace the silicon tetrachloride in the unloading tank 21 with nitrogen. When the silicon tetrachloride in the unloading tank 21 is replaced with nitrogen, close the third valve 53 and open the fourth valve 54 to pass the resin in the unloading tank 21 into the hydrolysis component 24;
[0044] (5) After the resin in the unloading tank 21 is completely discharged, the fourth valve 54 is closed, and steps 3 and 4 are repeated in sequence until the resin in the adsorption tank 11 is completely discharged.
[0045] In the technical solution provided in the embodiment of the present invention, the function of the adsorption component is to replace trichlorosilane and dichlorosilane, and the adsorption component includes an adsorption tank body 11, a silicon tetrachloride feed pipe 12, a first silicon tetrachloride discharge pipe 13 and a second silicon tetrachloride discharge pipe 14, the silicon tetrachloride feed pipe 12 is connected to the adsorption tank body 11, and is used to pass silicon tetrachloride into the adsorption tank body, and the first silicon tetrachloride discharge pipe 13 and the second silicon tetrachloride discharge pipe 14 are respectively connected to the adsorption tank body 11; the function of the discharge component is to process the resin, and the discharge component includes a discharge tank body 21, a silicon tetrachloride collection box 22, a filter 23, a hydrolysis component 24 and a first nitrogen feed pipe 25, and another of the second silicon tetrachloride discharge pipe 14 is connected to the adsorption tank body 11. The first end of the filter 23 is connected to the unloading tank 21, the second silicon tetrachloride discharge pipe 14 is provided with a first valve 51, the first nitrogen feed pipe 25 is connected to the unloading tank 21, the first nitrogen feed pipe 25 is provided with a second valve 52, one end of the filter 23 is connected to the unloading tank 21, and the other end is connected to the silicon tetrachloride collection box 22, a third valve 53 is provided between the filter 23 and the silicon tetrachloride collection box 22, a resin discharge pipe 26 is provided between the unloading tank 21 and the hydrolysis component 24, and a fourth valve 54 is provided on the resin discharge pipe 26. Compared with the prior art, the trichlorosilane medium in the adsorption column is replaced cleanly with silicon tetrachloride, and after the silicon tetrachloride concentration is greater than 99% after analysis and sampling, nitrogen is used to clean the trichlorosilane medium in the adsorption column. Silicon tetrachloride in the adsorption column is replaced with three wastes for treatment. Since silicon tetrachloride is non-flammable, the risk is relatively small compared to the first stage. However, after the capacity of the adsorption column is further increased, if you want to completely replace the adsorption column with nitrogen, it will take a long time, which may be as long as 20 days. The nitrogen gas flow blows the resin for a long time, and the resin keeps rolling and rubbing inside, which will generate static electricity. Since the resin itself is easy to burn, once the static electricity causes the resin to burn and decompose, the adsorption column will have the risk of explosion. In this technical solution, silicon tetrachloride with a purity higher than 99% is first introduced into the adsorption tank body 11 through the silicon tetrachloride feed pipe 12 and replaces the trichlorosilane and dichlorosilane in the adsorption tank body 11. When the first silicon tetrachloride is discharged When the purity of silicon tetrachloride discharged from the material pipe 13 is higher than 99%, the first silicon tetrachloride discharge pipe 13 is closed, and then the first valve 51 is opened to allow part of the solid-liquid mixture of silicon tetrachloride and resin to enter the discharge tank body 21 through the second silicon tetrachloride discharge pipe 14, and the third valve 53 is opened to allow silicon tetrachloride to enter the silicon tetrachloride collection box 22 through the filter 23, and then the first valve 51 is closed, and the second valve 52 is opened to allow nitrogen to enter the discharge tank body 21, and the silicon tetrachloride in the discharge tank body 21 is replaced with nitrogen. After the silicon tetrachloride in the discharge tank body 21 is replaced with nitrogen, the third valve 53 is closed, and the fourth valve 54 is opened to pass the resin in the discharge tank body 21 into the hydrolysis component 24;After the resin in the unloading tank 21 is discharged, the fourth valve 54 is closed, and the first valve 51 and the third valve 53 are opened again to cycle until the resin in the adsorption tank 11 is discharged. This can not only shorten the nitrogen replacement time, but also prevent nitrogen from blowing the resin balls for a long time, reduce the generation of static electricity, and thus achieve the technical effect of preventing explosions, thereby protecting personnel and property. ;
[0046] In the above step 1, the inlet valve and the outlet valve of the adsorption tank body 11 are closed. The inlet valve and the outlet valve mainly refer to other feed or discharge valves, such as the valve for entering the resin raw material, or the valve for entering the silicon material. In step 2, the silicon tetrachloride feed pipe 12 and the first silicon tetrachloride discharge pipe 13 are opened, and silicon tetrachloride with a purity higher than 99% is introduced into the adsorption tank body 11 through the silicon tetrachloride feed pipe 12 to replace the trichlorosilane and dichlorosilane in the adsorption tank body 11. When the purity of the silicon tetrachloride discharged from the first silicon tetrachloride discharge pipe 13 is higher than 99%, Close the first silicon tetrachloride discharge pipe 13, so that the trichlorosilane and dichlorosilane in the adsorption tank body 11 are replaced by silicon tetrachloride; in step 3, open the first valve 51, so that part of the solid-liquid mixture of silicon tetrachloride and resin enters the discharge tank body 21 through the second silicon tetrachloride discharge pipe 14, open the third valve 53, so that silicon tetrachloride enters the silicon tetrachloride collection box 22 through the filter 23, and the front hand valve and the rear hand valve are arranged around the first valve 51 and the third valve 53, and the front hand valve and the rear hand valve are usually in the open state; in step 4, close the first valve 51, open the third valve 53, and the front hand valve and the rear hand valve are usually in the open state. The second valve 52 allows nitrogen to enter the unloading tank body 21, and the silicon tetrachloride in the unloading tank body 21 is replaced by nitrogen. When the silicon tetrachloride in the unloading tank body 21 is replaced by nitrogen, the third valve 53 is closed, and the fourth valve 54 is opened to pass the resin in the unloading tank body 21 into the hydrolysis component 24. The time for replacing the silicon tetrachloride in the unloading tank body 21 with nitrogen is 20 minutes to 40 minutes. The specific time can be set according to the capacity of the unloading tank body 21. The time for passing the resin in the unloading tank body 21 into the hydrolysis component 24 is 10 minutes to 20 minutes. The specific time can be set according to the capacity of the unloading tank body 21. The time can be set according to the capacity of the unloading tank body 21. In step 5, after the resin in the unloading tank body 21 is discharged, the fourth valve 54 is closed, and steps 3 and 4 are repeated in sequence until the resin in the adsorption tank body 11 is discharged, thereby achieving the effect of quickly and safely discharging the resin; in this technical solution, by discharging large quantities of resin from the adsorption tank body 11 in batches, the amount of resin replaced in a single time is reduced, which not only reduces the time of nitrogen replacement, but also avoids safety accidents caused by equipment overpressure, thereby improving the discharge efficiency and saving manpower and material resources.
[0047] The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.
Claims
1. A method for discharging an anti-disproportionation resin and an adsorption resin device, characterized in that: The device for discharging the anti-disproportionation resin and the adsorption resin comprises: An adsorption component, the adsorption component comprises an adsorption tank body, a silicon tetrachloride feed pipe, a first silicon tetrachloride discharge pipe and a second silicon tetrachloride discharge pipe, the silicon tetrachloride feed pipe is connected to the adsorption tank body and is used to pass silicon tetrachloride into the adsorption tank body, the first silicon tetrachloride discharge pipe and the second silicon tetrachloride discharge pipe are respectively connected to the adsorption tank body; A discharge component, the discharge component comprises a discharge tank, a silicon tetrachloride collecting box, a filter, a hydrolysis component and a first nitrogen feed pipe, the other end of the second silicon tetrachloride discharge pipe is connected to the discharge tank, a first valve is arranged on the second silicon tetrachloride discharge pipe, the first nitrogen feed pipe is connected to the discharge tank, a second valve is arranged on the first nitrogen feed pipe, one end of the filter is connected to the discharge tank, and the other end is connected to the silicon tetrachloride collecting box, a third valve is arranged between the filter and the silicon tetrachloride collecting box, a resin discharge pipe is arranged between the discharge tank and the hydrolysis component, and a fourth valve is arranged on the resin discharge pipe; The method comprises the following steps: (1) Close the inlet valve and outlet valve of the adsorption tank; (2) Opening the silicon tetrachloride feed pipe and the first silicon tetrachloride discharge pipe, passing silicon tetrachloride with a purity higher than 99% into the adsorption tank through the silicon tetrachloride feed pipe to replace the trichlorosilane and dichlorosilane in the adsorption tank, and when the purity of silicon tetrachloride discharged from the first silicon tetrachloride discharge pipe is higher than 99%, closing the first silicon tetrachloride discharge pipe; (3) Open the first valve to allow part of the solid-liquid mixture of silicon tetrachloride and resin to enter the unloading tank through the second silicon tetrachloride discharge pipe, and open the third valve to allow silicon tetrachloride to enter the silicon tetrachloride collection box through the filter; (4) Close the first valve and open the second valve to allow nitrogen to enter the unloading tank body, and replace the silicon tetrachloride in the unloading tank body with nitrogen. When the silicon tetrachloride in the unloading tank body is replaced by nitrogen, close the third valve and open the fourth valve to pass the resin in the unloading tank body into the hydrolysis component; (5) After the resin in the unloading tank is completely discharged, the fourth valve is closed, and steps (3) and (4) are repeated in sequence until the resin in the adsorption tank is completely discharged.
2. The method for using the device for discharging anti-disproportionation resin and adsorption resin according to claim 1, characterized in that: The first nitrogen feed pipe and the second silicon tetrachloride discharge pipe are respectively connected to the top of the unloading tank body.
3. The method for using the device for discharging anti-disproportionation resin and adsorption resin according to claim 1, characterized in that: The resin discharge pipe is connected to the bottom of the discharge tank.
4. The method for using the device for discharging anti-disproportionation resin and adsorption resin according to claim 1, characterized in that: Also includes: A control component, wherein the control component is respectively connected to the first valve, the second valve, the third valve and the fourth valve, and is used to respectively control the opening or closing of the first valve, the second valve, the third valve and the fourth valve.
5. The method for using the device for discharging anti-disproportionation resin and adsorption resin according to claim 1, characterized in that: Also includes: A second nitrogen feed pipe, wherein the second nitrogen feed pipe is connected to the resin discharge pipe and is used for introducing nitrogen into the resin discharge pipe.
6. The method for using the device for discharging anti-disproportionation resin and adsorption resin according to claim 1, characterized in that: Also includes: An explosion vent is arranged at the top of the unloading tank body, and a bursting piece is arranged on the explosion vent.
7. The method for using the device for discharging anti-disproportionated resin and adsorption resin according to claim 1, characterized in that: A visual window is arranged on one side of the resin discharge pipe close to the hydrolysis component.
8. The method for using the device for discharging anti-disproportionated resin and adsorption resin according to claim 1, characterized in that: In the step (4), the time for replacing the silicon tetrachloride in the unloading tank with nitrogen is 20 minutes to 40 minutes.
9. The method for using the device for discharging anti-disproportionation resin and adsorption resin according to claim 1, characterized in that: In the step (4), the time for passing the resin in the unloading tank into the hydrolysis component is 10 minutes to 20 minutes.
Citation Information
Patent Citations
Device for discharging anti-disproportionated resin and adsorption resin
CN213912450U