Device and method capable of replacing catalyst on line for silane disproportionation reaction rectifying tower

The device and method for online catalyst replacement solve the problems of difficult catalyst replacement and production interruption, and realize safe and efficient catalyst replacement. It is applicable to reactive distillation and fixed-bed coupled systems, and improves the production efficiency of silane preparation.

CN120789691APending Publication Date: 2025-10-17SHANDONG XINGTAI SILICON MATERIAL TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202511028582.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-25
Publication Date
2025-10-17

AI Technical Summary

Technical Problem

Silane and chlorosilane systems are strictly prohibited from air and water. Catalyst replacement is difficult and may lead to combustion, explosion or corrosion. The replacement process also causes production interruption, especially in reactive distillation and fixed-bed coupled systems where the interruption is longer.

Method used

Design a device for online catalyst replacement in a silane disproportionation reactive distillation column, including a reactive distillation column, a catalyst storage tank, and a filter assembly. The old catalyst is carried out by liquid material and new catalyst is injected, achieving closed operation and preventing air and moisture leakage. It is suitable for reactive distillation and fixed-bed coupled systems.

Benefits of technology

It enables online catalyst replacement, avoids air and moisture leakage, improves production safety, shortens downtime, increases production efficiency, reduces production interruptions, and is suitable for silane preparation systems of different scales.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to a device and method for replacing a catalyst on line in a silane disproportionation reaction rectifying tower, and the device comprises a gas phase separation section, a catalysis section and a liquid phase separation section which are sequentially arranged in the reaction rectifying tower from top to bottom; the interior of the new catalyst storage tank is used for filling a new catalyst; the old catalyst storage tank is internally filled with a spent catalyst; the catalysis section comprises a cover plate and a bottom plate arranged below the cover plate, the outer edges of the cover plate and the bottom plate are both hermetically connected with the inner wall of the reactive distillation tower, a filling chamber for filling a solid catalyst is formed between the cover plate and the bottom plate, and a first hole group is formed in the cover plate; a catalyst inlet is formed in the upper portion of the filling chamber, and a first pipe opening of the catalyst inlet is connected with a discharging opening in the lower portion of the new catalyst storage tank through a first switch valve. According to the invention, not only can the requirements of contact and mixing of a catalyst and a reactant in the tower in the reactive distillation process be met, but also online disassembly of a failed catalyst and online installation of a new catalyst can be realized, and no air and moisture leakage risk exists in the whole process.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of reactive distillation column, in particular to a device and method for replacing catalysts of a silane disproportionation reactive distillation column on line. BACKGROUND

[0002] The main method for preparing silane is the chlorosilane disproportionation method: using trichlorosilane as raw material, three-step disproportionation reactions occur continuously, the first step of disproportionation reaction uses trichlorosilane as reactant to produce dichlorodisilane and silicon tetrachloride, the second step of disproportionation reaction uses dichlorodisilane as reactant to produce trichlorosilane and trichlorosilane, and the third step of disproportionation reaction uses trichlorosilane as reactant to produce silane and dichlorodisilane. The process of realizing the above three steps of disproportionation reaction mainly includes fixed bed process and reactive distillation process, and the reactive distillation process has more advantages in energy consumption.

[0003] The patent CN103172071A discloses that trichlorosilane is used as raw material, and silane and dichlorodisilane are obtained at the top of the reactive distillation column, silicon tetrachloride is obtained at the bottom of the column, and the mixed gas at the top is subjected to silicon tetrachloride absorption and fixed bed adsorption to obtain silane product; the patent CN103241743A discloses that high-purity trichlorosilane is used as raw material, the reactive distillation column is used to produce reaction products in gas phase at the top, the pressure difference is used to enter the silane column, and liquid silane product is obtained after separation, the mixed chlorosilane at the bottom is separated to obtain trichlorosilane which is returned to the reactive distillation column, and silicon tetrachloride is discharged; the patent CN115321540A discloses that trichlorosilane is used as raw material, and high-purity silane is prepared by using the reactive distillation technology, through disproportionation reaction distillation, multi-stage condensation separation, pressure increase of crude silane pump, and rectification separation and purification.

[0004] At present, the silane preparation technology by reactive distillation method has been put into industrial application, but there is still a very important problem: silane and chlorosilane system are strictly prohibited from air and water, and the catalyst installed in the column is extremely difficult to replace, trace air leakage may cause combustion and explosion in the column, and trace water leakage may cause serious corrosion in the column, which seriously limits the production scale and wide application of silane prepared by the reactive distillation method. In addition, even if the safety of catalyst replacement is ensured, the production process is interrupted for a long time due to shutdown and cooling and cooling operation in the replacement process, especially in the reaction distillation and fixed bed coupled reaction system, the production process is interrupted for a longer time due to the mismatching of the replacement period of the catalysts in the rectification column and the catalysts in the fixed bed. SUMMARY

[0005] To solve the technical problems in the background art, the present application provides a device and method for replacing catalysts of a silane disproportionation reactive distillation column on line.

[0006] The technical scheme of the present application is as follows: A device for online replacement of catalyst in a silane disproportionation reaction distillation tower, comprising: The reactive distillation tower has a gas separation section, a catalytic section and a liquid separation section arranged in sequence from top to bottom; A new catalyst storage tank, the interior of which is used to load new catalyst; Old catalyst storage tank, which is used to fill the spent catalyst; The catalytic section includes a cover plate and a bottom plate disposed thereunder. The outer edges of the cover plate and the bottom plate are sealed to the inner wall of the reaction distillation tower. A filling chamber for filling the solid catalyst is formed between the cover plate and the bottom plate. The cover plate is provided with a first hole group, and the first hole group is provided with a first filter screen having a pore size smaller than that of the catalyst particles. A catalyst inlet is provided at the upper portion of the filling chamber, and a first pipe opening is provided on the catalyst inlet, and the first pipe opening is connected to the discharge port at the lower portion of the new catalyst storage tank through a first switch valve; a catalyst outlet is provided at the lower portion of the filling chamber, and a second pipe opening is provided on the catalyst outlet, and the second pipe opening is connected to the discharge port of the old catalyst storage tank through a second switch valve; A plurality of filter assemblies are arranged in the catalytic section, and the filter assemblies include an outer sleeve, an inner sleeve, and a filter. The upper end of the outer sleeve is connected to the gas phase separation section, and the outer wall of the upper portion of the outer sleeve is sealed to the bottom plate. The bottom of the outer sleeve is sealed to the bottom plate. The filter is arranged at the lower portion of the outer sleeve. A second hole group is opened at the lower portion of the outer sleeve corresponding to the position of the filter. The second hole group is provided with a second filter screen having a pore size smaller than that of the catalyst particles. The inner sleeve is arranged in the outer sleeve, and the lower part of the inner sleeve passes through the filter and the bottom plate in sequence and is communicated with the liquid phase separation section.

[0007] Preferably, trays or packings are provided in both the gas phase separation section and the liquid phase separation section of the reactive distillation tower.

[0008] Preferably, the catalytic section of the reactive distillation tower is filled with a solid catalyst, which is a molecular sieve, alumina, resin particles or activated carbon.

[0009] Preferably, the size of the filter pores of the filter is smaller than the size of the catalyst particles, the filter is a wire mesh filter, and the lower portion of the filter is fully welded to the bottom plate.

[0010] The outer sleeve serves as a carrier for installing the inner sleeve and the filter. Its specific structure is that the outer sleeve includes a straight cylinder and a top liquid baffle plate arranged thereon. The upper part of the straight cylinder is connected to the cover plate through an upper flange assembly, and the lower part of the straight cylinder is connected to the base plate through a bottom flange assembly.

[0011] In order to facilitate the gas phase generated by the reaction in the outer sleeve to flow out of the outer sleeve to the gas phase separation section for multi-stage separation, the top liquid baffle is connected to the upper end of the straight cylinder through at least one support rod, and the bottom surface of the top liquid baffle is spaced apart from the upper end surface of the straight cylinder.

[0012] A method for replacing catalysts in a silane disproportionation reaction rectifying tower on line, and a device for replacing catalysts in a silane disproportionation reaction rectifying tower on line, steps are as follows, S1, taking out old catalysts Open the second switch valve, close the first switch valve, the catalysts in the catalytic section can be taken into the old catalyst storage tank by liquid materials, after the old catalysts flow out completely, close the second switch valve, do solid-liquid separation in the old catalyst storage tank, and take out the old catalysts; S2, close the second switch valve, close the first switch valve, and fill new catalysts into the new catalyst storage tank; S3, fill new catalysts Open the first switch valve, fill the new catalysts in the new catalyst storage tank into the catalytic section, and close the first switch valve after filling is completed; S4, after the replacement of catalysts on line is completed, sequentially replace the remaining catalytic sections in the whole tower on line.

[0013] The beneficial effects of the present application are that: The catalysts in the catalytic section can be taken into the old catalyst storage tank by liquid materials, after the old catalysts flow out completely, do solid-liquid separation in the old catalyst storage tank, and take out the old catalysts, realize the removal of the catalysts, and realize the installation of new catalysts by injecting new catalysts from the new catalyst tank into the catalytic section, which not only meets the requirements of the reaction rectification process for the contact and mixing of catalysts in the tower with reactants, but also realizes the online removal of failed catalysts and the online installation of new catalysts, and there is no risk of air and water leakage in the whole process; The catalysts in the catalytic section are completely soaked in the reaction materials, the mass transfer and heat transfer effects are optimal, the residence reaction time is prolonged, the energy consumption is reduced, and the raw material utilization rate is improved; The processes of filling new catalysts and dismounting old catalysts are both fully closed processes, and the dangerous materials of silane and chlorosilane are not in contact with air and water, so the process is safer; The processes of filling new catalysts and dismounting old catalysts can be realized on line, without the need for parking replacement and purging, the parking time is shortened, and the production efficiency is improved; The device and method of the present application are not only suitable for the reaction system for preparing silane by reaction rectification method, but also suitable for the reaction system coupled with fixed bed, which reduces the longer interruption of production process caused by the mismatching of the replacement of catalysts in the rectifying tower and the replacement of catalysts in the fixed bed, and improves the production efficiency. BRIEF DESCRIPTION OF DRAWINGS

[0014] In the drawings: Figure 1 It is a structural schematic diagram; Figure 2 It is a sleeve structure schematic diagram; Figure 3 Figure 1 is a top view of the outer sleeve; The components represented by the reference numerals in the drawings are as follows: T01, reaction rectification tower; V01, new catalyst storage tank; V02, old catalyst storage tank; V-1, first switch valve; V-2, second switch valve; 1, separation section; 2, catalytic section; 3, cover plate; 4, outer sleeve; 401, bottom flange; 402, straight cylinder; 403, upper flange; 404, top liquid baffle; 5, inner sleeve; 6, filter; 7, bottom plate. DETAILED DESCRIPTION

[0015] Example 1 Referring to Figure 1 , Figure 2 and Figure 3 , a silane disassociation reaction rectification tower T01 can replace catalysts on-line, which comprises a reaction rectification tower T01, a new catalyst storage tank V01 and an old catalyst storage tank V02.

[0016] The reaction rectification tower T01 internally comprises a separation section 1 and a catalytic section 2, the separation section 1 comprises a gas phase separation section and a liquid phase separation section, and the reaction rectification tower T01 internally has the gas phase separation section, the catalytic section 2 and the liquid phase separation section arranged in sequence from top to bottom. The reaction rectification tower T01 is provided with a tower tray or a packing in the gas phase separation section and the liquid phase separation section. The catalytic section 2 of the reaction rectification tower T01 is filled with solid catalysts, and the solid catalysts are molecular sieves, alumina, resin particles or activated carbon.

[0017] The new catalyst storage tank V01 is used to fill new catalysts. The old catalyst storage tank V02 is used to fill failed catalysts.

[0018] The catalytic section 2 comprises a cover plate 3 and a bottom plate 7 arranged below the cover plate 3, the outer edges of the cover plate 3 and the bottom plate 7 are sealingly connected with the inner wall of the reaction rectification tower T01, a filling chamber for filling solid catalysts is formed between the cover plate 3 and the bottom plate 7, a first hole group is formed on the cover plate 3, the first hole group comprises a plurality of first through holes, a first filter screen with a hole diameter smaller than that of the catalyst particles is arranged on the first hole group to prevent the catalyst particles from moving to the gas phase separation section through the cover plate 3; The upper part of the filling chamber is provided with a catalyst inlet, the catalyst inlet is provided with a first pipe opening A, the first pipe opening A is connected with the discharge port of the lower part of the new catalyst storage tank V01 through a first switch valve V-1 and a pipeline; the lower part of the filling chamber is provided with a catalyst outlet, the catalyst outlet is provided with a second pipe opening B, the second pipe opening B is connected with the discharge port of the old catalyst storage tank V02 through a second switch valve V-2 and a pipeline.

[0019] A plurality of filter assemblies are arranged in the catalytic section 2, each filter assembly comprising an outer sleeve 4, an inner sleeve 5 and a filter 6, the upper end of the outer sleeve 4 being in communication with the gas phase separation section, the outer sleeve 4 being in sealing connection with the bottom plate 7 at the upper portion of the outer sleeve 4, the bottom of the outer sleeve 4 being in sealing connection with the bottom plate 7, the filter 6 being arranged at the lower portion of the outer sleeve 4, a second hole group being formed at the lower portion of the outer sleeve 4 corresponding to the position of the filter 6, and a second filter screen with a smaller hole diameter than the catalyst particles being arranged on the second hole group. The inner sleeve 5 is arranged in the outer sleeve 4, and the lower portion of the inner sleeve 5 is in communication with the liquid phase separation section by sequentially penetrating the filter 6 and the bottom plate 7.

[0020] The filter hole of the filter 6 is smaller than the size of the catalyst particles, and the filter 6 is a wire mesh filter, a Johnson filter or a metal wire filter, etc. The lower portion of the filter 6 is in full welding connection with the bottom plate 7.

[0021] The outer sleeve 4 serves as a carrier for mounting the inner sleeve 5 and the filter 6. The specific structure of the outer sleeve 4 is that the outer sleeve 4 comprises a straight cylinder 402 and a top liquid blocking plate 404 arranged thereon, the upper portion of the straight cylinder 402 is connected with the cover plate 3 through an upper flange assembly, and the lower portion of the straight cylinder 402 is connected with the bottom plate 7 through a bottom flange assembly. The upper flange assembly comprises an upper flange 403 and connecting bolts, the upper flange 403 is in full welding connection with the upper portion of the straight cylinder 402, and the upper flange 403 is detachably connected with the cover plate 3 through the connecting bolts. The bottom flange assembly comprises a bottom plate flange 401 and connecting bolts, the bottom plate flange 401 is in full welding connection with the lower portion of the straight cylinder 402, and the bottom plate flange 401 is detachably connected with the bottom plate 7 through the connecting bolts.

[0022] In order to facilitate the gas phase generated in the outer sleeve 4 to flow out of the outer sleeve 4 to the gas phase separation section for multi-stage separation, the top liquid blocking plate 404 is connected with the upper end of the straight cylinder 402 through at least one supporting rod, and the bottom surface of the top liquid blocking plate 404 is arranged in a spaced manner with the upper end surface of the straight cylinder 402.

[0023] Embodiment 2 A method for replacing catalysts in a silane disproportionation rectifying column T01 online, using a device for replacing catalysts in a silane disproportionation rectifying column T01 online, the steps are as follows, S1, removing old catalysts The second switch valve V-2 is opened, and the first switch valve V-1 is closed, so that the catalysts in the catalytic section 2 can be carried by the liquid material into the old catalyst storage tank V02, after the old catalysts flow out completely, the second switch valve V-2 is closed, and the old catalysts are removed after solid-liquid separation in the old catalyst storage tank V02; S2, closing the second switch valve V-2 and the first switch valve V-1, and filling the new catalysts into the new catalyst storage tank V01; S3, filling new catalysts Open the first switch valve V-1, and fill the new catalyst in the new catalyst storage tank V01 into the catalytic section 2. After the filling is completed, the first switch valve V-1 is closed. S4, after the online replacement of the catalyst is completed, sequentially replace the remaining catalytic sections 2 in the whole tower.

[0024] The online catalyst replacement device and method provided in the above embodiments can realize the new catalyst filling and old catalyst dismounting processes on-line without stopping and replacing and purging, shorten the stopping time, improve the production efficiency, and can be controlled by the control system based on real-time gas phase detection and process parameter monitoring for catalyst replacement early warning and instruction triggering, or can be manually operated.

[0025] Moreover, the device and method are not only suitable for the reaction system for preparing silane by reaction rectification, but also suitable for a reaction system coupled with a fixed bed, thereby reducing the longer interruption of the production process caused by the mismatch between the catalyst replacement periods of the rectification tower and the fixed bed, and ensuring the production efficiency. The reaction system coupled with a fixed bed refers to a reaction system in which a fixed bed reactor is additionally arranged for a reaction rectification tower, and the gas phase of a water cooler of the reaction rectification tower at the top of the reaction rectification tower is connected with the fixed bed reactor. In the system, the reaction processes can be realized in the reaction rectification tower and the fixed bed reactor. The bottom of the reaction rectification tower is connected with a reaction rectification tower reboiler. The liquid phase at the bottom of the reaction rectification tower returns to the bottom of the reaction rectification tower after being gasified in the reaction rectification tower reboiler. The gas phase at the top of the reaction rectification tower enters the water cooler of the reaction rectification tower. The condensed liquid returns to the top of the reaction rectification tower. The non-condensed gas enters the fixed bed reactor to react to achieve component balance. The reaction product enters the rear-end component separation. Different from the reaction system for preparing silane by reaction rectification, the reaction process and component balance of the fixed bed reactor are also considered during the replacement process. For example, the pressure fluctuation of the control system does not exceed the design pressure range (±0.1 barg) of the fixed bed reactor. The reboiler steam amount can be adjusted, and a fixed bed bypass valve (part of the non-condensed gas is shunted) can be additionally arranged. In addition, the selection of the catalyst replacement time comprehensively considers the difference (≤10%) between the activity parameters (such as the specific surface area and the pore size distribution) of the new catalyst and the fixed bed catalyst, and strictly controls the replacement time to be not too long.

[0026] Example 3 On the basis of example 1 and example 2, in this embodiment, the silane reaction rectification tower T01 with a capacity of 200 tons / year is used. The tower diameter is 0.6 m. A total of 6 separation sections 1 and 6 catalytic sections 2 are arranged at intervals. The gas phase separation section and the liquid phase separation section both use mesh wave corrugated structured packing to realize component separation. The catalytic section 2 uses modified activated carbon catalyst for catalytic reaction.

[0027] The distance between the bottom of the cover plate 3 of each catalytic section 2 and the top of the bottom plate 7 is 1.2 m, and the total amount of catalyst used is 0.24 m3. The cover plate 3 is used to block the overflow of the catalyst in the catalytic section 2 by covering the holes with a wire mesh. The outer sleeve 4 is made of 7 seamless pipes with a diameter of 89x4 mm, each pipe is 1 m long, and the top is a circular liquid baffle. The inner sleeve 5 is made of 7 seamless pipes with a diameter of 57x4 mm, each pipe is 1 m long, and the lower part is fully welded to the bottom plate 7 to prevent liquid leakage. The filter 6 is a filter screen structure wrapped with a wire mesh, with the same size as the outer sleeve 4, i.e., 89x4 mm. The large-hole filter pipe has an opening rate of 85%, the wire mesh has a wire diameter of 0.15 mm, the wire mesh has a mesh size of 20, and the total height of the filter 6 is 300 mm. The upper part of the filter 6 is fully welded to the outer sleeve 4 to prevent liquid leakage, and the bottom is fully welded to the bottom plate 7 to prevent liquid leakage. The bottom plate 7 is fully welded to the tower wall around the opening to prevent liquid leakage, and the filter assembly is installed in the opening and connected to the inner sleeve 5 and the filter 6.

[0028] After the device is put into operation, the average monthly production of silane is about 19.3 tons initially, and after one and a half years, the average monthly production of silane decreases to about 17.1 tons, which cannot meet the production requirements, and the catalyst is replaced online.

[0029] The second valve is opened, the catalyst in the catalytic section 2 is brought into the old catalyst storage tank V02 by the liquid material, after the catalyst flows out completely, the second valve is closed, and the solid-liquid separation is performed in the old catalyst storage tank V02, and the old catalyst is taken out.

[0030] The first switch valve V-1 is opened, the catalyst in the new catalyst storage tank V01 flows into the catalytic section 2, after the catalyst flows in completely, the first switch valve V-1 is closed, the online replacement of the catalyst is completed, and the online replacement of the six catalytic sections 2 of the whole tower is sequentially performed.

[0031] After the catalyst is replaced and the device is put into operation, the average monthly production of silane is restored to about 19.2 tons initially.

[0032] Example 4 Based on examples 1 and 2, this example is according to a 5000 tons / year capacity silane reaction rectification tower T01, the tower diameter is 2 m, and a total of 8 separation sections 1 and 8 catalytic sections 2 are arranged at intervals, both the gas phase separation section and the liquid phase separation section use plate corrugated structured packing to realize component separation, and the catalytic section 2 uses resin catalyst for catalytic reaction.

[0033] The distance between the bottom of the cover plate 3 and the top of the bottom plate 7 of each catalytic section 2 is 1.8 m, and the total amount of catalyst used is 3.3 m3. The cover plate 3 uses a whole plate with holes covered with a wire mesh to block the overflow of the catalyst in the catalytic section 2. The outer sleeve 4 uses 19 seamless pipes with a diameter of 273x5 mm, each pipe is 1.5 m long, and the top is a circular liquid baffle; the inner sleeve 5 uses 19 seamless pipes with a diameter of 219x4 mm, each pipe is 1.6 m long, and the lower part is full-welded to the bottom plate 7 to prevent liquid leakage; the filter 6 uses 19 Johnson filter screen structures, with the same size as the outer sleeve 4, i.e., 273x5 mm, the filter screen wire diameter is 1.5 mm, the gap width is 0.25 mm, and the total height of the filter 6 is 400 mm, the upper part of which is full-welded to the outer sleeve 4 to prevent liquid leakage, and the bottom is full-welded to the bottom plate 7 to prevent liquid leakage. The bottom plate 7 is a whole plate with holes, the periphery is full-welded to the tower wall to prevent liquid leakage, and the installation position of the filter assembly is holed and connected with the inner sleeve 5 and the filter 6.

[0034] After the device is put into operation, the average value of the initial silane monthly output is about 462 tons, and after two years, the average value of the silane monthly output decreases to about 413 tons, which cannot meet the production requirements, and the catalyst is replaced online.

[0035] The second valve is opened, the catalyst in the catalytic section 2 is brought into the old catalyst storage tank V02 by the liquid material, after the catalyst flows out completely, the second valve is closed, and the solid-liquid separation is performed in the old catalyst storage tank V02, and the old catalyst is taken out.

[0036] The first switch valve V-1 is opened, the catalyst in the new catalyst storage tank V01 flows into the catalytic section 2, after the catalyst flows in completely, the first switch valve V-1 is closed, the online replacement of the catalyst is completed, and the online replacement of the 8 catalytic sections 2 of the whole tower is sequentially performed.

[0037] After the catalyst is replaced and the device is put into operation, the average value of the initial silane monthly output is restored to about 463 tons.

[0038] Example 5 On the basis of Example 1 and Example 2, in this example, the silane reaction rectifying tower T01 with a capacity of 20000 tons / year is used, the tower diameter is 3.8 m, there are 7 separation sections 1 and 7 catalytic sections 2 in the whole tower, which are distributed at intervals, the gas phase separation section and the liquid phase separation section both use trays to realize component separation, and the catalytic section 2 uses modified molecular sieve catalyst for catalytic reaction.

[0039] The distance between the bottom of the cover plate 3 and the top of the bottom plate 7 of each catalytic section 2 is 2 m, and the total amount of catalyst used is 14.6 m3. The cover plate 3 is used to block the overflow of the catalyst in the catalytic section 2 by covering the large-pore screen with a combination plate. The outer sleeve 4 is made of 37 seamless pipes with a diameter of 325x5 mm, each pipe is 1.6 m long, and the top is a circular liquid baffle; the inner sleeve 5 is made of 37 seamless pipes with a diameter of 273x5 mm, each pipe is 1.5 m long, and the lower part is fully welded to the bottom plate 7 to prevent liquid leakage; the filter 6 is a filter net structure wrapped with a large-pore filter pipe, with the same size as the outer sleeve 4, i.e., 325x5 mm, the opening rate of the large-pore filter pipe is 90%, the pore size of the large-pore screen is 0.3 mm, and the total height of the filter 6 is 500 mm. The upper part of the filter 6 is fully welded to the outer sleeve 4 to prevent liquid leakage, and the bottom is fully welded to the bottom plate 7 to prevent liquid leakage. The bottom plate 7 is made of a whole plate with holes, and the periphery is fully welded to the tower wall to prevent liquid leakage. The installation position of the filter assembly is opened and connected with the inner sleeve 5 and the filter 6.

[0040] After the device is put into operation, the average monthly output of silane is about 1893 tons initially, and after two and a half years, the average monthly output of silane decreases to about 1711 tons, which cannot meet the production requirements, and the catalyst is replaced online.

[0041] The second valve is opened, the catalyst in the catalytic section 2 is carried into the old catalyst storage tank V02 by the liquid material, after the catalyst flows out completely, the second valve is closed, and the solid-liquid separation is carried out in the old catalyst storage tank V02, and the old catalyst is taken out.

[0042] The first switch valve V-1 is opened, the catalyst in the new catalyst storage tank V01 flows into the catalytic section 2, after the catalyst flows in completely, the first switch valve V-1 is closed, the online replacement of the catalyst is completed, and the online replacement of the seven catalytic sections 2 in the whole tower is sequentially carried out.

[0043] After the catalyst is replaced and the device is put into operation, the average monthly output of silane is restored to about 1883 tons initially.

Claims

1. A device for online catalyst replacement in a silane disproportionation reaction distillation tower, characterized in that: include, A reactive distillation tower (T01) is provided with a gas phase separation section, a catalytic section (2) and a liquid phase separation section in order from top to bottom; New catalyst storage tank (V01), which is used to load new catalyst; Old catalyst storage tank (V02), which is used to store spent catalyst; The catalytic section (2) includes a cover plate (3) and a bottom plate (7) disposed thereunder. The outer edges of the cover plate (3) and the bottom plate (7) are sealedly connected to the inner wall of the reaction distillation tower (T01). A filling chamber for filling the solid catalyst is formed between the cover plate (3) and the bottom plate (7). The cover plate (3) is provided with a first hole group, and the first hole group is provided with a first filter screen having a hole diameter smaller than that of the catalyst particles. The upper portion of the filling chamber is provided with a catalyst inlet, which is provided with a first pipe opening, and the first pipe opening is connected to the discharge port at the lower portion of the new catalyst storage tank (V01) through a first switch valve (V-1); the lower portion of the filling chamber is provided with a catalyst outlet, which is provided with a second pipe opening, and the second pipe opening is connected to the discharge port of the old catalyst storage tank (V02) through a second switch valve (V-2); A plurality of filter assemblies are arranged in the catalytic section (2), and the filter assemblies include an outer sleeve (4), an inner sleeve (5) and a filter (6). The upper end of the outer sleeve (4) is communicated with the gas phase separation section, and the upper outer wall of the outer sleeve (4) is sealedly connected to the bottom plate (7). The bottom of the outer sleeve (4) is sealedly connected to the bottom plate (7). The filter (6) is arranged at the lower part of the outer sleeve (4). A second hole group is opened at the lower part of the outer sleeve (4) corresponding to the position of the filter (6). The second hole group is provided with a second filter screen having a pore size smaller than that of the catalyst particles. The inner sleeve (5) is arranged inside the outer sleeve (4), and the lower portion of the inner sleeve (5) passes through the filter (6) and the bottom plate (7) in sequence to communicate with the liquid phase separation section.

2. The device for online catalyst replacement in a silane disproportionation reaction distillation tower according to claim 1, characterized in that: The gas phase separation section and the liquid phase separation section of the reactive distillation tower (T01) are both provided with tower trays or fillers.

3. The device for online catalyst replacement in a silane disproportionation reaction distillation tower according to claim 1, characterized in that: The catalytic section (2) of the reactive distillation tower (T01) is filled with a solid catalyst, which is a molecular sieve, alumina, resin particles or activated carbon.

4. The device for online catalyst replacement in a silane disproportionation reaction distillation tower according to claim 1, characterized in that: The size of the filter holes of the filter (6) is smaller than the size of the catalyst particles. The filter (6) is a wire mesh filter. The lower part of the filter (6) is fully welded to the bottom plate (7).

5. The device for online catalyst replacement in a silane disproportionation reaction distillation tower according to claim 1, characterized in that: The outer sleeve (4) comprises a straight cylinder (402) and a top liquid baffle (404) arranged thereon; the upper portion of the straight cylinder (402) is connected to the cover plate (3) via an upper flange assembly, and the lower portion of the straight cylinder (402) is connected to the bottom plate (7) via a bottom flange assembly.

6. The device for online catalyst replacement in a silane disproportionation reaction distillation tower according to claim 5, characterized in that: The top liquid baffle plate (404) is connected to the upper end of the straight cylinder (402) via at least one supporting rod, and the bottom surface of the top liquid baffle plate (404) is spaced apart from the upper end surface of the straight cylinder (402).

7. A method for online catalyst replacement in a silane disproportionation reaction distillation tower, characterized in that: The device for online catalyst replacement in a silane disproportionation reaction distillation tower according to any one of claims 1 to 6 is used, and the steps are as follows: S1. Remove the old catalyst The second on-off valve (V-2) is opened, and the first on-off valve (V-1) is closed. The catalyst in the catalytic section (2) can be carried into the old catalyst storage tank (V02) by the liquid material. After all the old catalyst flows out, the second on-off valve (V-2) is closed, and solid-liquid separation is performed in the old catalyst storage tank (V02) to remove the old catalyst; S2, close the second on-off valve (V-2), close the first on-off valve (V-1), and fill the new catalyst into the new catalyst storage tank (V01); S3. Loading new catalyst Open the first switch valve (V-1), the new catalyst storage tank (V01) in the new catalyst is filled into the catalytic section (2), after the filling is completed, close the first switch valve (V-1); S4. After the catalyst is replaced online, the remaining catalytic sections (2) of the entire tower are replaced online in sequence.

Citation Information

Patent Citations

  • Device and method for preparing high-purity silane through disproportionation reactive distillation of trichlorosilane

    CN103172071A

  • Reactive distillation method and equipment for preparing silane through direct disproportionation of trichlorosilane

    CN103241743A