CN112494990A - Device for discharging anti-disproportionation resin and adsorption resin and use method - Google Patents
Device for discharging anti-disproportionation resin and adsorption resin and use method Download PDFInfo
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- CN112494990A CN112494990A CN202011370777.9A CN202011370777A CN112494990A CN 112494990 A CN112494990 A CN 112494990A CN 202011370777 A CN202011370777 A CN 202011370777A CN 112494990 A CN112494990 A CN 112494990A
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Abstract
The invention discloses a device for discharging anti-disproportionation resin and adsorption resin and a using method thereof, relates to the technical field of crystal silicon production equipment, and mainly aims to provide a device capable of improving the efficiency of discharging adsorption resin and anti-disproportionation resin and the safety of a discharging process and saving labor cost. The main technical scheme of the invention is as follows: an apparatus for discharging an anti-disproportionation resin and an adsorption resin comprising: the adsorption part is characterized in that a first silicon tetrachloride discharging pipe and a second silicon tetrachloride discharging pipe are respectively connected to the adsorption tank body; the part of unloading, the other end that the pipe was arranged to second silicon tetrachloride is connected in the jar body of unloading, and second silicon tetrachloride is arranged and is set up first valve on the pipe, and first nitrogen gas inlet pipe is connected in the jar body of unloading, sets up the second valve on the first nitrogen gas inlet pipe, and the one end of filter is connected in the jar body of unloading, sets up the third valve between filter and the silicon tetrachloride collecting box, sets up the fourth valve on the resin is arranged the material pipe. The invention is mainly used for discharging resin.
Description
Technical Field
The invention relates to the technical field of polycrystalline silicon production equipment, in particular to a device for discharging reverse disproportionation resin and adsorption resin and a using method thereof.
Background
In the last decade, the photovoltaic industry is rapidly developed at home, polycrystalline silicon materials are used as the front end of the photovoltaic industry, a single set of polycrystalline silicon materials is also developed from thousands of tons to 5 thousands of tons at present, the purity of polycrystalline silicon is extremely high, impurities in raw materials are mainly removed in the production process by adopting a rectification mode, the limitation of operation cost and rectification and purification precision is considered, trichlorosilane serving as a byproduct in the production process needs to be treated, adsorption resin is introduced into each production manufacturer in a large quantity, meanwhile, dichlorosilane serving as a byproduct in the production process needs to be treated, and anti-disproportionation resin is used.
When the scale of a single polysilicon set is in the kiloton level, the single capacity of the used adsorption and anti-disproportionation resin is smaller, along with the increasing of the scale of the single set, the single capacity of an adsorption and anti-disproportionation device is also increased, the loading amount of the single resin in the industry can reach dozens of parties currently, when the resin needs to be discarded and discharged out of a system for replacement, the resin replacement and discharge process is time-consuming and labor-consuming, the efficiency is lower, and meanwhile, the safety risk exists, and in recent years, the safety accident caused by resin discharge is avoided for polysilicon manufacturers.
In the prior art, the resin discharge mode mainly comprises the following two stages:
the first stage is as follows: after the service life of the resin is finished, the process medium is replaced to three wastes by directly using nitrogen, after sampling is qualified, the resin is discharged, a single adsorption column is small in the stage, the replacement and discharge time is short, the use labor is not much, safety accidents are fewer, along with the increase of the capacity of the adsorption column, the replacement time is longer and longer, a large amount of labor cost is needed, meanwhile, the risk is gradually increased, the phenomenon of resin combustion in the discharge process is often caused, and then the resin discharge is developed to the second stage.
And in the second stage, after the service life of the resin is finished, firstly, the trichlorosilane medium in the adsorption column is completely replaced by silicon tetrachloride, after the concentration of the analyzed and sampled silicon tetrachloride is more than 99%, nitrogen is used for replacing the silicon tetrachloride in the adsorption column to the three-waste treatment, the risk is relatively small in the first stage, but after the capacity of the adsorption column is further increased, if the nitrogen is used for completely replacing the adsorption column, the required time is very long and can reach 20 days, the nitrogen airflow blows the resin for a long time, the resin is continuously rolled and rubbed in the resin, static electricity is generated, and the resin belongs to an inflammable product, so that the static electricity easily causes the resin to be combusted and decomposed.
Disclosure of Invention
In view of this, the embodiment of the present invention provides a device for discharging an anti-disproportionation resin and an adsorption resin and a use method thereof, and mainly aims to provide a device for discharging an anti-disproportionation resin and an adsorption resin, which can improve the efficiency of discharging an adsorption resin and an anti-disproportionation resin and the safety of a discharging process, and can save labor cost.
In order to achieve the purpose, the invention mainly provides the following technical scheme:
in one aspect, an embodiment of the present invention provides an apparatus for discharging an anti-disproportionation resin and an adsorption resin, including:
the adsorption part comprises an adsorption tank body, a silicon tetrachloride feeding pipe, a first silicon tetrachloride discharging pipe and a second silicon tetrachloride discharging pipe, wherein the silicon tetrachloride feeding pipe is connected to the adsorption tank body and used for introducing silicon tetrachloride into the adsorption pipe body, and the first silicon tetrachloride discharging pipe and the second silicon tetrachloride discharging pipe are respectively connected to the adsorption tank body;
the part of unloading, the part of unloading is including the jar body of unloading, silicon tetrachloride collecting box, filter, the part of hydrolysising and first nitrogen gas inlet pipe, the second silicon tetrachloride arrange the other end of material pipe connect in the jar body of unloading, second silicon tetrachloride arrange the material pipe on set up first valve, first nitrogen gas inlet pipe connect in the jar body of unloading, set up the second valve on the first nitrogen gas inlet pipe, the one end of filter connect in the jar body of unloading, the other end connect in the silicon tetrachloride collecting box, the filter with set up the third valve between the silicon tetrachloride collecting box, the jar body of unloading with it arranges the material pipe to set up the resin between the part of hydrolysising, the resin is arranged and is gone up to set up the fourth valve.
Furthermore, the first nitrogen gas inlet pipe and the second silicon tetrachloride discharging pipe are respectively connected to the top of the discharging tank body.
Further, the resin discharge pipe is connected to the bottom of the discharge tank body.
Further, the control component is respectively connected to the first valve, the second valve, the third valve and the fourth valve, and is used for respectively controlling the opening or closing of the first valve, the second valve, the third valve and the fourth valve.
Further, a second nitrogen feeding pipe is connected to the resin discharging pipe and used for introducing nitrogen into the resin discharging pipe.
Furthermore, the explosion venting port is arranged at the top of the discharging tank body, and a rupture disc is arranged on the explosion venting port.
Further, a visual window is arranged on one side, close to the hydrolysis part, of the resin discharge pipe.
In another aspect, an embodiment of the present invention further provides a method for using an apparatus for discharging an anti-disproportionation resin and an adsorption resin, where the method includes the following steps:
(1) closing an inlet valve and an outlet valve of the adsorption tank body;
(2) opening a silicon tetrachloride feeding pipe and a first silicon tetrachloride discharging pipe, introducing silicon tetrachloride with the purity higher than 99% into the adsorption tank body through the silicon tetrachloride feeding pipe, replacing trichlorosilane and dichlorosilane in the adsorption tank body, and closing the first silicon tetrachloride discharging pipe when the purity of the silicon tetrachloride discharged by the first silicon tetrachloride discharging pipe is higher than 99%;
(3) opening a first valve to enable part of the mixed solution of silicon tetrachloride and resin to enter the discharging tank body through a second silicon tetrachloride discharging pipe, and opening a third valve to enable the silicon tetrachloride to enter the silicon tetrachloride collecting tank through the filter;
(4) closing the first valve, opening the second valve to enable nitrogen to enter the discharging tank body, replacing silicon tetrachloride in the discharging tank body with the nitrogen, closing the third valve after the silicon tetrachloride in the discharging tank body is replaced by the nitrogen, opening the fourth valve, and introducing resin in the discharging tank body into the hydrolysis part;
(5) and after the resin in the discharge tank body is discharged, closing the fourth valve, and circularly and sequentially performing the step 3 and the step 4 until the resin in the adsorption tank body is discharged.
Further, in the step 4, the time for replacing the silicon tetrachloride in the discharge tank body with the nitrogen is 20 minutes to 40 minutes.
Further, in the step 4, the resin in the discharge tank body is introduced into the hydrolysis part for 10 minutes to 20 minutes.
Compared with the prior art, the invention has the following technical effects:
in the technical scheme provided by the embodiment of the invention, the adsorption part is used for replacing trichlorosilane and dichlorosilane by silicon tetrachloride, the adsorption part comprises an adsorption tank body, a silicon tetrachloride feeding pipe, a first silicon tetrachloride discharging pipe and a second silicon tetrachloride discharging pipe, the silicon tetrachloride feeding pipe is connected to the adsorption tank body and is used for introducing silicon tetrachloride into the adsorption tank body, and the first silicon tetrachloride discharging pipe and the second silicon tetrachloride discharging pipe are respectively connected to the adsorption tank body; the discharging part is used for treating resin, the discharging part comprises a discharging tank body, a silicon tetrachloride collecting box, a filter, a hydrolysis part and a first nitrogen feeding pipe, the other end of a second silicon tetrachloride discharging pipe is connected with the discharging tank body, a first valve is arranged on the second silicon tetrachloride discharging pipe, the first nitrogen feeding pipe is connected with the discharging tank body, a second valve is arranged on the first nitrogen feeding pipe, one end of the filter is connected with the discharging tank body, the other end of the filter is connected with the silicon tetrachloride collecting box, a third valve is arranged between the filter and the silicon tetrachloride collecting box, a resin discharging pipe is arranged between the discharging tank body and the hydrolysis part, a fourth valve is arranged on the resin discharging pipe, compared with the prior art, the trichlorosilane medium in an adsorption column is completely replaced by silicon tetrachloride, after the concentration of the analyzed and sampled silicon tetrachloride is more than 99 percent, the silicon, in the technical scheme, firstly, silicon tetrachloride with the purity higher than 99 percent is introduced into the adsorption tank body through a silicon tetrachloride feeding pipe and replaces trichlorosilane and dichlorosilane in the adsorption tank body, when the purity of the silicon tetrachloride discharged by a first silicon tetrachloride discharging pipe is higher than 99 percent, a first valve is closed, and part of mixed solution of the silicon tetrachloride and the resin enters the discharging tank body through a second silicon tetrachloride discharging pipe, opening a third valve to enable silicon tetrachloride to enter a silicon tetrachloride collecting box through a filter, then closing the first valve, opening a second valve to enable nitrogen to enter the discharging tank body, replacing the silicon tetrachloride in the resin with the nitrogen, closing the third valve after the silicon tetrachloride in the discharging tank body is replaced with the nitrogen, opening a fourth valve, and introducing the resin in the discharging tank body into the hydrolysis part; after the resin in the discharging tank body is discharged, the fourth valve is closed, the first valve and the third valve are opened again to be circulated, the resin in the adsorption tank body is discharged, the opening and closing of the whole process valve are completed according to sequential control procedures through automatic valves, the valve does not need to be attended by a special person, a large amount of manpower is saved, the discharging efficiency is improved, the replacement time of nitrogen can be shortened, the resin balls are prevented from being blown and swept for a long time, the generation of static electricity is reduced, the technical effect of explosion prevention is achieved, and the effects of protection personnel and property are further achieved.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for discharging disproportionation resin and adsorption resin according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
In one aspect, as shown in fig. 1, an embodiment of the present invention provides an apparatus for discharging an anti-disproportionation resin and an adsorption resin, the apparatus comprising:
the adsorption part comprises an adsorption tank body 11, a silicon tetrachloride feeding pipe 12, a first silicon tetrachloride discharging pipe 13 and a second silicon tetrachloride discharging pipe 14, wherein the silicon tetrachloride feeding pipe 12 is connected to the adsorption tank body 11 and is used for introducing silicon tetrachloride into the adsorption pipe body, and the first silicon tetrachloride discharging pipe 13 and the second silicon tetrachloride discharging pipe 14 are respectively connected to the adsorption tank body 11;
the discharging part comprises a discharging tank body 21, a silicon tetrachloride collecting box 22, a filter 23, a hydrolysis part 24 and a first nitrogen feeding pipe 25, the other end of a second silicon tetrachloride discharging pipe 14 is connected to the discharging tank body 21, a first valve 51 is arranged on the second silicon tetrachloride discharging pipe 14, the first nitrogen feeding pipe 25 is connected to the discharging tank body 21, a second valve 52 is arranged on the first nitrogen feeding pipe 25, one end of the filter 23 is connected to the discharging tank body 21, the other end of the filter 23 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 discharging pipe 26 is arranged between the discharging tank body 21 and the hydrolysis part 24, and a fourth valve 54 is arranged on the resin discharging pipe 26.
In the technical scheme provided by the embodiment of the invention, an adsorption part is used for replacing trichlorosilane and dichlorosilane, the adsorption part comprises an adsorption tank body 11, a silicon tetrachloride feeding pipe 12, a first silicon tetrachloride discharging pipe 13 and a second silicon tetrachloride discharging pipe 14, the silicon tetrachloride feeding pipe 12 is connected to the adsorption tank body 11 and is used for introducing silicon tetrachloride into the adsorption tank body, and the first silicon tetrachloride discharging pipe 13 and the second silicon tetrachloride discharging pipe 14 are respectively connected to the adsorption tank body 11; the discharging part is used for treating resin, the discharging part comprises a discharging tank body 21, a silicon tetrachloride collecting box 22, a filter 23, a hydrolysis part 24 and a first nitrogen feeding pipe 25, the other end of a second silicon tetrachloride discharging pipe 14 is connected with the discharging tank body 21, a first valve 51 is arranged on the second silicon tetrachloride discharging pipe 14, the first nitrogen feeding pipe 25 is connected with the discharging tank body 21, a second valve 52 is arranged on the first nitrogen feeding pipe 25, one end of the filter 23 is connected with the discharging tank body 21, the other end of the filter 23 is connected with 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 discharging pipe 26 is arranged between the discharging tank body 21 and the hydrolysis part 24, a fourth valve 54 is arranged on the resin discharging pipe 26, compared with the prior art, the trichlorosilane medium in an adsorption column is completely replaced by silicon tetrachloride, after the concentration, then, replacing silicon tetrachloride in the adsorption column by using nitrogen until three wastes are treated, wherein the risk is relatively small in the first stage because the silicon tetrachloride is incombustible, but after the capacity of the adsorption column is further increased, if the nitrogen is used for completely replacing the adsorption column, the required time is long and can be as long as 20 days, the nitrogen airflow blows resin for a long time, the resin continuously rolls and rubs in the adsorption column to generate static electricity, the resin is easy to burn, once the static electricity causes the resin to be burnt and decomposed, the adsorption column has an explosion risk, in the technical scheme, firstly, the silicon tetrachloride with the purity higher than 99 percent is led into the adsorption tank body 11 through the silicon tetrachloride feeding pipe 12 to replace the trichlorosilane and the dichlorosilane in the adsorption tank body 11, when the purity of the silicon tetrachloride discharged from the first silicon tetrachloride discharging pipe 13 is higher than 99 percent, the first silicon tetrachloride discharging pipe 13 is closed, then, opening a first valve 51 to enable part of the mixed solution of silicon tetrachloride and resin to enter the discharging tank 21 through a second silicon tetrachloride discharging pipe 14, opening a third valve 53 to enable the silicon tetrachloride to enter the silicon tetrachloride collecting tank 22 through a filter 23, then closing the first valve 51, opening a second valve 52 to enable nitrogen to enter the discharging tank 21, replacing the silicon tetrachloride in the discharging tank 21 with the nitrogen, closing the third valve 53 after the silicon tetrachloride in the discharging tank 21 is replaced with the nitrogen, opening a fourth valve 54, and introducing the resin in the discharging tank 21 into the hydrolysis part 24; after the resin in the unloading tank body 21 is discharged, the fourth valve 54 is closed, the first valve 51 and the third valve 53 are opened again for circulation, and the resin in the adsorption tank body 11 is discharged completely, so that the replacement time of nitrogen can be shortened, the discharge efficiency is improved, the labor is saved, meanwhile, the nitrogen can be prevented from purging resin balls for a long time, the generation of static electricity is reduced, the technical effect of explosion is achieved, and the effect of protecting personnel and property is further achieved.
The adsorption part is used for replacing trichlorosilane and dichlorosilane, the adsorption part comprises an adsorption tank body 11, a silicon tetrachloride feeding pipe 12, a first silicon tetrachloride discharging pipe 13 and a second silicon tetrachloride discharging pipe 14, the silicon tetrachloride feeding pipe 12 is connected with the adsorption tank body 11 and is used for introducing silicon tetrachloride into the adsorption pipe body, the first silicon tetrachloride discharging pipe 13 and the second silicon tetrachloride discharging pipe 14 are respectively connected with the adsorption tank body 11, the silicon tetrachloride feeding pipe 12 is arranged at the side part of the adsorption tank body 11, the first silicon tetrachloride discharging pipe 13 is arranged at the bottom part of the adsorption tank body 11, the second silicon tetrachloride discharging pipe 14 is arranged at the top part of the adsorption tank body 11, in addition, no filter cap is used for filtering the silicon tetrachloride, so that resin can enter the discharging tank body 21 through the second silicon tetrachloride discharging pipe 14, a plurality of pressure detection tables 3 and temperature detection tables 4 can also be arranged around the adsorption tank, the temperature and the pressure value in the adsorption tank body 11 are displayed in real time, electromagnetic valves or other types of valves are arranged on the silicon tetrachloride feeding pipe 12 and the first silicon tetrachloride discharging pipe 13, so that the silicon tetrachloride can be conveniently and automatically controlled to enter and discharge, and the adsorption tank body 11 usually adopts a traditional adsorption column, so that the adsorption tank body 11 is also provided with the feeding pipe and the discharging pipe, which is not described in detail herein; the discharging part is used for processing resin and comprises a discharging tank body 21, a silicon tetrachloride collecting box 22, a filter 23, a hydrolysis part 24 and a first nitrogen feeding pipe 25, the other end of a second silicon tetrachloride discharging pipe 14 is connected with the discharging tank body 21, a first valve 51 is arranged on the second silicon tetrachloride discharging pipe 14, the first nitrogen feeding pipe 25 is connected with the discharging tank body 21, a second valve 52 is arranged on the first nitrogen feeding pipe 25, one end of the filter 23 is connected with the discharging tank body 21, the other end of the filter 23 is connected with 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 discharging pipe 26 is arranged between the discharging tank body 21 and the hydrolysis part 24, a fourth valve 54 is arranged on the resin discharging pipe 26, a plurality of pressure detection tables 3 and 4 are arranged on the discharging tank body 21, and the temperature and pressure values in the discharging tank, the second silicon tetrachloride discharging pipe 14 is connected to the top of the discharging tank body 21, the first valve 51 is opened, the silicon tetrachloride feeding pipe 12 always feeds silicon tetrachloride into the adsorption tank body 11, by utilizing the characteristic of the floating state of resin in the silicon tetrachloride, the silicon tetrachloride and the resin can enter the discharging tank body 21 through the second silicon tetrachloride discharging pipe 14, the third valve 53 is opened, the silicon tetrachloride enters the silicon tetrachloride collecting box 22 through the filter 23, the resin is intercepted by the filter 23 and stays in the discharging tank body 21, the first valve 51 is closed after the resin and the silicon tetrachloride enter the discharging tank body 21 for a certain time, the certain time is usually about 30 minutes and can be adjusted according to the volume of the discharging tank body 21 and the overflow time, then the second valve 52 is opened to feed nitrogen into the discharging tank body 21, and the first nitrogen feeding pipe 25 is connected to the top of the discharging tank body 21, the method comprises the following steps of enabling nitrogen to enter from the top of an unloading tank body 21, replacing silicon tetrachloride in the unloading tank body 21 with the nitrogen, closing a third valve 53 after the replacement of the silicon tetrachloride in the unloading tank body 21 is completed, opening a fourth valve 54, discharging the nitrogen from the bottom, reducing static aggregation caused by rolling friction of resin pellets, pressing the resin into a hydrolysis tank by using the pressure of the nitrogen, closing the fourth valve 54 after the resin in the unloading tank body 21 is discharged, circularly opening a first valve 51, introducing part of the silicon tetrachloride and the resin in the adsorption tank body 11 into the unloading tank body 21 again until the resin in the adsorption tank body 11 is completely discharged, in the technical scheme, firstly introducing the silicon tetrachloride with the purity higher than 99% into the adsorption tank body 11 through a feeding pipe 12, replacing trichlorosilane and dichlorosilane in the adsorption tank body 11, and when the purity of the silicon tetrachloride discharged from a first silicon tetrachloride discharging pipe 13 is higher than 99%, closing the first silicon tetrachloride discharge pipe 13, then opening the first valve 51, enabling part of the mixed solution of silicon tetrachloride and resin to enter the discharging tank 21 through the second silicon tetrachloride discharge pipe 14, opening the third valve 53, enabling the silicon tetrachloride to enter the silicon tetrachloride collecting box 22 through the filter 23, then closing the first valve 51, opening the second valve 52, enabling nitrogen to enter the discharging tank 21, hydrolyzing the resin in the discharging tank 21, after the silicon tetrachloride in the discharging tank 21 is replaced by the nitrogen, closing the third valve 53, opening the fourth valve 54, and introducing the resin in the discharging tank 21 into the hydrolysis part 24; after the resin in the unloading tank body 21 is discharged, the fourth valve 54 is closed, the first valve 51 and the third valve 53 are opened again for circulation, the resin in the adsorption tank body 11 is discharged, the whole valve is automatically controlled by the control part to be opened and closed, a specially-assigned person is not needed, the efficiency is improved, the manpower resource is saved, the replacement time of nitrogen can be shortened, meanwhile, the nitrogen can be prevented from blowing the resin balls for a long time to generate static electricity, the technical effect of explosion prevention is achieved, and the effects of protecting personnel and property are further achieved.
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 for controlling 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 adopts 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, and of course, the control component may also be connected to other valves, the pressure detection meter 3, the temperature detection meter 4 and other components, so as to monitor the resin or flow data in the discharge tank 21 or the adsorption tank 11 in real time, and upload the data to the overall control system.
Further, a second nitrogen gas feed pipe 6, the second nitrogen gas feed pipe 6 is connected to the resin discharge pipe 26 for introducing nitrogen gas into the resin discharge pipe 26. In this embodiment, second nitrogen inlet pipe 6 has been increased, and second nitrogen inlet pipe 6's effect lets in nitrogen gas in arranging material pipe 26 to the resin, prevents to be blocked by silicon dioxide at the resin and arranges the hookup location in material pipe 26 and the pond of hydrolysising to reach and keep the unobstructed technological effect of material pipe 26 to the resin.
Further, let out and explode mouth 7 and set up at the top of unloading jar body 21, let out and explode the mouth 7 and set up the rupture disk. In the embodiment, the explosion venting port 7 is added, the explosion venting port 7 is used for discharging the pressure in the discharging tank body 21, when an uncontrollable state occurs in the discharging tank body 21, the resin amount in the discharging tank body 21 is small, so that an overpressure part is easily discharged from the explosion venting port 7, safety accidents caused by overpressure of equipment are avoided, the equipment and personnel are protected, the explosion venting port 7 is provided with the explosion piece, the explosion pressure of the explosion piece is lower than the design pressure of the discharging tank body 21, and the technical effect of conveniently discharging the pressure in the discharging tank body 21 is achieved.
Further, a viewing window 8 is provided on a side of the resin discharge pipe 26 adjacent to the hydrolysis member 24. In this embodiment, visual window 8 has been increased, can make things convenient for personnel to observe whether the resin in the resin row material pipe 26 is discharged and is accomplished, then opens first valve 51 and get into new resin again.
In another aspect, an embodiment of the present invention further provides a method for using an apparatus for discharging an anti-disproportionation resin and an adsorption resin, where the method includes the following steps:
(1) closing an inlet valve and an outlet valve of the adsorption tank body 11;
(2) opening a silicon tetrachloride feeding pipe 12 and a first silicon tetrachloride discharging pipe 13, introducing silicon tetrachloride with the purity higher than 99% into an adsorption tank body 11 through the silicon tetrachloride feeding pipe 12, replacing trichlorosilane and dichlorosilane in the adsorption tank body 11, and closing the first silicon tetrachloride discharging pipe 13 when the purity of the silicon tetrachloride discharged from the first silicon tetrachloride discharging pipe 13 is higher than 99%;
(3) opening a first valve 51 to enable part of the mixed solution of silicon tetrachloride and resin to enter the discharging tank body 21 through a second silicon tetrachloride discharging pipe 14, and opening a third valve 53 to enable the silicon tetrachloride to enter the silicon tetrachloride collecting tank 22 through a filter 23;
(4) closing the first valve 51, opening the second valve 52 to enable nitrogen to enter the discharging tank 21, replacing silicon tetrachloride in the discharging tank 21 with the nitrogen, closing the third valve 53 and opening the fourth valve 54 after the silicon tetrachloride in the discharging tank 21 is replaced with the nitrogen, and introducing resin in the discharging tank 21 into the hydrolysis part 24;
(5) and after the resin in the discharging tank body 21 is discharged, closing the fourth valve 54, and circularly and sequentially performing the step 3 and the step 4 until the resin in the adsorption tank body 11 is discharged.
In the technical scheme provided by the embodiment of the invention, an adsorption part is used for replacing trichlorosilane and dichlorosilane, the adsorption part comprises an adsorption tank body 11, a silicon tetrachloride feeding pipe 12, a first silicon tetrachloride discharging pipe 13 and a second silicon tetrachloride discharging pipe 14, the silicon tetrachloride feeding pipe 12 is connected to the adsorption tank body 11 and is used for introducing silicon tetrachloride into the adsorption tank body, and the first silicon tetrachloride discharging pipe 13 and the second silicon tetrachloride discharging pipe 14 are respectively connected to the adsorption tank body 11; the discharging part is used for treating resin, the discharging part comprises a discharging tank body 21, a silicon tetrachloride collecting box 22, a filter 23, a hydrolysis part 24 and a first nitrogen feeding pipe 25, the other end of a second silicon tetrachloride discharging pipe 14 is connected with the discharging tank body 21, a first valve 51 is arranged on the second silicon tetrachloride discharging pipe 14, the first nitrogen feeding pipe 25 is connected with the discharging tank body 21, a second valve 52 is arranged on the first nitrogen feeding pipe 25, one end of the filter 23 is connected with the discharging tank body 21, the other end of the filter 23 is connected with 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 discharging pipe 26 is arranged between the discharging tank body 21 and the hydrolysis part 24, a fourth valve 54 is arranged on the resin discharging pipe 26, compared with the prior art, the trichlorosilane medium in an adsorption column is completely replaced by silicon tetrachloride, after the concentration, then, replacing silicon tetrachloride in the adsorption column by using nitrogen until three wastes are treated, wherein the risk is relatively small in the first stage because the silicon tetrachloride is incombustible, but after the capacity of the adsorption column is further increased, if the nitrogen is used for completely replacing the adsorption column, the required time is long and can be as long as 20 days, the nitrogen airflow blows resin for a long time, the resin continuously rolls and rubs in the adsorption column to generate static electricity, the resin is easy to burn, once the static electricity causes the resin to be burnt and decomposed, the adsorption column has an explosion risk, in the technical scheme, firstly, the silicon tetrachloride with the purity higher than 99 percent is led into the adsorption tank body 11 through the silicon tetrachloride feeding pipe 12 to replace the trichlorosilane and the dichlorosilane in the adsorption tank body 11, when the purity of the silicon tetrachloride discharged from the first silicon tetrachloride discharging pipe 13 is higher than 99 percent, the first silicon tetrachloride discharging pipe 13 is closed, then, opening a first valve 51 to enable part of the mixed solution of silicon tetrachloride and resin to enter the discharging tank 21 through a second silicon tetrachloride discharging pipe 14, opening a third valve 53 to enable the silicon tetrachloride to enter the silicon tetrachloride collecting box 22 through a filter 23, then closing the first valve 51, opening a second valve 52 to enable nitrogen to enter the discharging tank 21, replacing the silicon tetrachloride in the discharging tank 21 with the nitrogen, closing the third valve 53 after the silicon tetrachloride in the discharging tank 21 is replaced with the nitrogen, opening a fourth valve 54, and introducing the resin in the discharging tank 21 into the hydrolysis part 24; after the resin in the unloading tank body 21 is discharged, the fourth valve 54 is closed, the first valve 51 and the third valve 53 are opened again for circulation, and the replacement time of nitrogen can be shortened until the resin in the adsorption tank body 11 is discharged, and meanwhile, the nitrogen can be prevented from purging resin balls for a long time, so that the generation of static electricity is reduced, the technical effect of explosion prevention is achieved, and the effect of protecting personnel and property is further achieved.
In the step 1, an inlet valve and an outlet valve of the adsorption tank body 11 are closed, wherein the inlet valve and the outlet valve mainly refer to other feeding or discharging valves, such as a valve for entering a resin raw material or a valve for entering a silicon material, in the step 2, a silicon tetrachloride feeding pipe 12 and a first silicon tetrachloride discharging pipe 13 are opened, silicon tetrachloride with the purity higher than 99% is fed into the adsorption tank body 11 through the silicon tetrachloride feeding pipe 12 and is used for replacing trichlorosilane and dichlorosilane in the adsorption tank body 11, and when the purity of the silicon tetrachloride discharged from the first silicon tetrachloride discharging pipe 13 is higher than 99%, the first silicon tetrachloride discharging pipe 13 is closed, so that the trichlorosilane and dichlorosilane in the adsorption tank body 11 are replaced by silicon tetrachloride; in the step 3, opening the first valve 51 to allow part of the mixed solution of silicon tetrachloride and resin to enter the discharging tank 21 through the second silicon tetrachloride discharging pipe 14, opening the third valve 53 to allow silicon tetrachloride to enter the silicon tetrachloride collecting tank 22 through the filter 23, and arranging a front hand valve and a rear hand valve around the first valve 51 and the third valve 53, wherein the front hand valve and the rear hand valve are normally in an open state; in the step 4, the first valve 51 is closed, the second valve 52 is opened, nitrogen enters the discharge tank 21, silicon tetrachloride in the discharge tank 21 is replaced by nitrogen, after the silicon tetrachloride in the discharge tank 21 is replaced by nitrogen, the third valve 53 is closed, the fourth valve 54 is opened, resin in the discharge tank 21 is introduced into the hydrolysis part 24, the replacement time of the silicon tetrachloride in the discharge tank 21 by nitrogen is 20 to 40 minutes, the specific time can be set according to the capacity of the discharge tank 21, the time for introducing the resin in the discharge tank 21 into the hydrolysis part 24 is 10 to 20 minutes, the specific time can be set according to the capacity of the discharge tank 21, in the step 5, after the resin in the discharge tank 21 is completely discharged, the fourth valve 54 is closed, and the steps 3 and 4 are cyclically and sequentially performed until the resin in the adsorption tank 11 is completely discharged, thereby achieving the effect of discharging the resin quickly and safely; in the technical scheme, large batches of resin are discharged from the adsorption tank body 11 in batches, so that the resin amount of single replacement is reduced, the nitrogen replacement time can be shortened, and safety accidents caused by overpressure of equipment can be avoided, so that the discharge efficiency is improved, and manpower and material resources are saved.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. An apparatus for discharging an anti-disproportionation resin and an adsorption resin, comprising:
the adsorption part comprises an adsorption tank body, a silicon tetrachloride feeding pipe, a first silicon tetrachloride discharging pipe and a second silicon tetrachloride discharging pipe, wherein the silicon tetrachloride feeding pipe is connected to the adsorption tank body and used for introducing silicon tetrachloride into the adsorption pipe body, and the first silicon tetrachloride discharging pipe and the second silicon tetrachloride discharging pipe are respectively connected to the adsorption tank body;
the part of unloading, the part of unloading is including the jar body of unloading, silicon tetrachloride collecting box, filter, the part of hydrolysising and first nitrogen gas inlet pipe, the second silicon tetrachloride arrange the other end of material pipe connect in the jar body of unloading, second silicon tetrachloride arrange the material pipe on set up first valve, first nitrogen gas inlet pipe connect in the jar body of unloading, set up the second valve on the first nitrogen gas inlet pipe, the one end of filter connect in the jar body of unloading, the other end connect in the silicon tetrachloride collecting box, the filter with set up the third valve between the silicon tetrachloride collecting box, the jar body of unloading with it arranges the material pipe to set up the resin between the part of hydrolysising, the resin is arranged and is gone up to set up the fourth valve.
2. The apparatus for discharging disproportionation resin and adsorption resin as claimed in claim 1,
the first nitrogen gas inlet pipe and the second silicon tetrachloride discharging pipe are respectively connected to the top of the discharging tank body.
3. The apparatus for discharging disproportionation resin and adsorption resin as claimed in claim 1,
the resin discharging pipe is connected to the bottom of the discharging tank body.
4. The apparatus for discharging disproportionation resin and adsorption resin of claim 1 further comprising:
and the control component is respectively connected with the first valve, the second valve, the third valve and the fourth valve and is used for respectively controlling the opening or closing of the first valve, the second valve, the third valve and the fourth valve.
5. The apparatus for discharging disproportionation resin and adsorption resin of claim 1 further comprising:
and the second nitrogen feeding pipe is connected to the resin discharging pipe and is used for introducing nitrogen into the resin discharging pipe.
6. The apparatus for discharging disproportionation resin and adsorption resin of claim 1 further comprising:
and the explosion venting port is arranged at the top of the discharging tank body, and a rupture disc is arranged on the explosion venting port.
7. The apparatus for discharging disproportionation resin and adsorption resin as claimed in claim 1,
and a visual window is arranged on one side of the resin discharge pipe close to the hydrolysis part.
8. A method for using an apparatus for discharging disproportionately-modified resin and adsorbent resin, wherein the apparatus for discharging disproportionately-modified resin and adsorbent resin as claimed in any one of claims 1 to 7 is used, the method comprising the steps of:
(1) closing an inlet valve and an outlet valve of the adsorption tank body;
(2) opening a silicon tetrachloride feeding pipe and a first silicon tetrachloride discharging pipe, introducing silicon tetrachloride with the purity higher than 99% into the adsorption tank body through the silicon tetrachloride feeding pipe, replacing trichlorosilane and dichlorosilane in the adsorption tank body, and closing the first silicon tetrachloride discharging pipe when the purity of the silicon tetrachloride discharged by the first silicon tetrachloride discharging pipe is higher than 99%;
(3) opening a first valve to enable part of the mixed solution of silicon tetrachloride and resin to enter the discharging tank body through a second silicon tetrachloride discharging pipe, and opening a third valve to enable the silicon tetrachloride to enter the silicon tetrachloride collecting tank through the filter;
(4) closing the first valve, opening the second valve to enable nitrogen to enter the discharging tank body, replacing silicon tetrachloride in the discharging tank body with the nitrogen, closing the third valve after the silicon tetrachloride in the discharging tank body is replaced by the nitrogen, opening the fourth valve, and introducing resin in the discharging tank body into the hydrolysis part;
(5) and after the resin in the discharge tank body is discharged, closing the fourth valve, and circularly and sequentially performing the step 3 and the step 4 until the resin in the adsorption tank body is discharged.
9. The use of a device for discharging reverse disproportionation resin and adsorption resin according to claim 8,
in the step 4, the silicon tetrachloride in the discharging tank body is replaced by nitrogen for 20 to 40 minutes.
10. The use of a device for discharging reverse disproportionation resin and adsorption resin according to claim 8,
in the step 4, the time for introducing the resin in the discharging tank body into the hydrolysis part is 10 minutes to 20 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011370777.9A CN112494990A (en) | 2020-11-30 | 2020-11-30 | Device for discharging anti-disproportionation resin and adsorption resin and use method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011370777.9A CN112494990A (en) | 2020-11-30 | 2020-11-30 | Device for discharging anti-disproportionation resin and adsorption resin and use method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112494990A true CN112494990A (en) | 2021-03-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011370777.9A Pending CN112494990A (en) | 2020-11-30 | 2020-11-30 | Device for discharging anti-disproportionation resin and adsorption resin and use method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112494990A (en) |
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2020
- 2020-11-30 CN CN202011370777.9A patent/CN112494990A/en active Pending
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