CN110613955B - Chlorosilane adsorption resin filling device and resin filling method - Google Patents
Chlorosilane adsorption resin filling device and resin filling method Download PDFInfo
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- CN110613955B CN110613955B CN201910937323.6A CN201910937323A CN110613955B CN 110613955 B CN110613955 B CN 110613955B CN 201910937323 A CN201910937323 A CN 201910937323A CN 110613955 B CN110613955 B CN 110613955B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/206—Packing or coating
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
Abstract
The invention discloses a chlorosilane adsorption resin filling device and a resin filling method, wherein the filling device comprises a resin buffer tank, a chlorosilane resin adsorption column, a pump and a Venturi tube, wherein the outlet of the resin buffer tank is connected with the throat part of the Venturi tube, the outlet of the Venturi tube is connected with the inlet of the chlorosilane adsorption column, the outlet of the chlorosilane adsorption column is connected with the inlet of the pump through a cooling system, and the outlet of the pump is connected with the inlet end of the Venturi tube. The invention has the advantages that (1) the energy consumption is low, the nitrogen consumption is low, a small amount of resin is adopted to contact with a large amount of chlorosilane, the heat release is uniform, the resin activity can be ensured, and the filling safety can be ensured; (2) avoiding the abrasion and powdering caused by the high-speed flow of the resin.
Description
Technical Field
The invention relates to a chlorosilane adsorbent resin filling device and a resin filling method, and also relates to chlorosilane adsorbent resin prepared by the method, in particular to application of the chlorosilane resin in impurity removal.
Background
The chlorosilane adsorbent resin is porous weakly alkaline polymer resin with large specific surface area of 35m2The water content of the resin is kept about 1 wt% even if a vacuum drying method is adopted, and the vacuum drying method has the defects of high energy consumption and low drying efficiency. In addition, due to the particularity of physical properties of chlorosilane, chlorosilane is very easy to react with water in micropores of resin to release gas and a large amount of reaction heat, and active load substances in the resin are decomposed and inactivated under severe conditions, even high temperature and high pressure are generated instantly to cause explosion accidents.
In the prior art, three filling methods of chlorosilane adsorbent resin are mainly adopted, but all the methods have some problems. The method comprises the following steps: the resin is firstly loaded into a chlorosilane resin adsorption column, and after the nitrogen replacement is qualified, chlorosilane is introduced into the bottom of the adsorption column. In the process, as the chlorosilane and the water in the resin react to release heat, the chlorosilane introduction speed is low, the reaction heat cannot be taken away in time, the resin is locally overheated, the resin is pulverized, the active groups are lost to inactivate the resin, and even safety accidents occur. The second method comprises the following steps: the resin is directly poured into a chlorosilane resin adsorption column through the inlet hole. In the process, because the partial pressure of the chlorosilane in vaporization is low, the chlorosilane in vaporization is very easy to react with water in air to generate hydrogen chloride to pollute the environment, and meanwhile, the chlorosilane in vaporization damages operators; in addition, the resin density is lower than that of chlorosilane, the resin floats on the surface of the chlorosilane and cannot react fully, and the risk of heat accumulation and release exists; in addition, air can be brought into the system in the direct dumping process, so that the production is damaged. The third method comprises the following steps: and conveying the resin to a chlorosilane resin adsorption column in a pneumatic conveying mode. A certain amount of chlorosilane needs to be filled into a chlorosilane resin adsorption column during pneumatic conveying, in order to enable the resin to be in full contact with the chlorosilane, a submerged pipe inserting mode needs to be adopted, the conveying nitrogen pressure is high, the energy consumption is high, the pneumatic conveying distance is long, the flow speed is high, the resin is greatly abraded, the resin cannot form uniform dispersion flow in a pipeline, and blockage is easily caused during dense-phase conveying.
Therefore, it is desirable to provide a safe and effective resin filling apparatus and method to solve the above problems.
Disclosure of Invention
The purpose of the invention is as follows: the technical problem to be solved by the invention is to provide a chlorosilane adsorption resin filling device and a resin filling method aiming at the defects of the prior art, further provide chlorosilane adsorption resin prepared by the method, and further provide application of the chlorosilane resin in impurity removal.
In order to solve the technical problem, the invention discloses a chlorosilane adsorbent resin filling device.
The idea of the invention is as follows: (1) resin buffer tank system: increase nitrogen gas formula of relying on oneself governing valve, can ensure to keep nitrogen gas malleation in the resin buffer tank, avoid in the air admission system, resin export control valve can be according to how much control resin of resin water content get into the speed of chlorosilane resin adsorption column. (2) Chlorosilane pump circulation system: chlorosilane is sprayed at the venturi throat to generate negative pressure to suck resin into a pipeline system to be mixed with chlorosilane, a large amount of chlorosilane is in contact with a small amount of moisture in the resin and can completely react in a short time, the chlorosilane and the resin enter the bottom of a chlorosilane resin adsorption column through an insertion pipe, the resin is filtered by a filter cap and stays in the adsorption column, and the chlorosilane exchanges heat with circulating water through a double-pipe heat exchanger and then reacts with the moisture in the resin through the venturi throat again. (3) The venturi tube is arranged: the pump export increases venturi can show the pressure that reduces the resin buffer tank, reduces the design pressure and the manufacturing cost of resin buffer tank, and the resin can be with the quick intensive mixing of chlorosilane in venturi choke department, can accomplish the reaction in the short time.
The invention discloses a chlorosilane adsorption resin filling device, which comprises a resin buffer tank 2, a chlorosilane resin adsorption column 6, a pump 4 and a venturi tube 5, wherein the resin buffer tank is shown in figure 1; wherein, the exit linkage venturi 8's of resin buffer tank 2 throat, venturi 8's exit linkage chlorosilane adsorption column 6's entry, chlorosilane adsorption column 6's export is passed through cooling system 5 and is connected the import of pump 4, and the export of pump 4 links to each other with venturi 8's entry end.
The pump 4 also has a valve 13, which acts to control the flow rate at the outlet of the pump, and the outlet pressure of the pump need not be controlled in the case of a certain type of pump.
Wherein the connection is a pipeline connection; wherein the connection of the pipeline and each part is flange connection.
Wherein the inlet of the resin buffer tank 2 is connected with a nitrogen self-operated regulating valve 1, the outlet is connected with a resin outlet control valve 3, and the top is connected with a pressure gauge 11 and a resin filling port 12; wherein, the outlet control valve 3 of the resin buffer tank is connected with a transparent hose 10 with flanges at two ends of the venturi 8 throat; the pressure gauge is used for observing the pressure in the resin buffer tank, and the situation that nitrogen cannot be supplemented in time when the self-operated regulating valve fails and danger is generated due to the fact that air enters the system due to the fact that negative pressure is generated in the buffer tank is avoided.
The nitrogen self-operated regulating valve can ensure that resin filling is finished in a positive pressure environment of a nitrogen meter, and air is prevented from entering a system; the resin filling port is opened after a tank of resin is filled, and granular resin is poured into the resin buffer tank; wherein the particle size of the resin is 0.7-0.9 mm.
Wherein, the bottom of the chlorosilane resin adsorption column 6 contains a resin filtering cap 7, and an inserting pipe 9 is arranged inside the chlorosilane resin adsorption column 6.
Wherein the resin filtering cap is a resin filtering cap consisting of a metal filament filtering net, and the gap of the filtering cap is 0.3 mm; the filter cap can calculate the flow rate of the adsorption column chlorosilane under the allowable pressure difference according to the sum of the areas of the gaps, and the flow rate of the filter cap in the formal production is basically 2 times of the maximum operation flow rate. Since the resin has a lower true density than chlorosilane, an insert tube is required to prevent the resin from floating on the adsorption column; the pipe diameter of the insertion pipe is small, preferably DN 25; the inserting tube is inserted below the chlorosilane adsorption column to prolong the contact time of the resin and the chlorosilane and improve the heat dissipation effect.
Wherein, the cooling system 5 is a double-pipe heat exchanger with circulating water as cooling medium. Wherein, the circulating water inlet 51 and the circulating water outlet 52 are shown in fig. 1; wherein, the cooling water system mainly takes away the heat released by the reaction of water and chlorosilane in the resin.
Wherein, the pump is a canned motor pump or a magnetic drive pump to ensure the sealing without leakage.
Wherein, the effect of venturi and pump is: (1) spraying chlorosilane at the venturi throat to generate negative pressure to suck resin into the pipeline system and mix the resin with the chlorosilane; (2) the Venturi tube can ensure that the fluid has enough flow velocity at the Venturi throat to fully mix the resin and the chlorosilane; (3) the pump is used for completing self-circulation of chlorosilane, so that reaction heat can be taken out, the heat accumulation of a system can be avoided, and meanwhile, a large amount of liquid is contacted with a small amount of resin, so that a rapid exothermic reaction can be avoided; (3) the reaction can be completed in a short time by contacting a large amount of chlorosilane with a small amount of moisture in the resin.
The method for filling chlorosilane adsorbent resin by using the device comprises the following steps:
(1) placing resin to be filled into a resin buffer tank, placing chlorosilane into a chlorosilane resin adsorption column, and introducing gas into a self-operated regulating valve;
(2) opening a resin outlet control valve to allow resin to flow to the venturi;
(3) pressurizing chlorosilane by a pump, enabling the pressurized chlorosilane to flow through a pipeline system, enabling the pressurized chlorosilane to flow through a cooling system and the pump to reach a venturi tube, converting static pressure energy into kinetic energy, generating negative pressure at the throat of the venturi tube, sucking the resin flowing into the venturi tube in the step (2) into the pipeline system by the negative pressure, mixing the resin with the chlorosilane in the pipeline system to obtain resin adsorbing the chlorosilane and the chlorosilane not adsorbed by the resin, and enabling the resin to enter the bottom of a chlorosilane resin adsorption column through an insertion pipe;
(4) filtering the resin adsorbing the chlorosilane in the step (3) by using a resin filtering cap, staying in an adsorption column, exchanging heat of the chlorosilane not adsorbed by the resin by using a cooling system, pressurizing by using a pump, and simultaneously entering the inserting tube together with the resin through a Venturi throat;
(5) and (5) circulating the steps (2) to (4) until no resin flows through the transparent hose, and finishing resin filling.
In the step (1), the resin is a thermally decomposed resin, preferably a resin with a polystyrene polymer skeleton and polyhydroxy glucosamine as an active component; in the invention, the mass ratio of the resin to the chlorosilane is not specifically required, and preferably 1: 3-5; the resin can be added into the resin buffer tank firstly, and the resin is added into the resin buffer tank through the resin filling port when the resin buffer tank is empty until all the resin is added.
In the step (1), the gas is nitrogen, and the nitrogen flow has no special requirement and is used for ensuring positive pressure in the buffer tank.
In the step (2), the resin outlet control valve is used for manually controlling the flow rate of resin according to the water content of the resin, the water content of the resin is measured by adopting a weighing method before the resin is filled, dense phase conveying is adopted when the water content of the resin is not more than 1%, and the flow rate of the resin is controlled to be 3-5 m/s, so that the resin is uniformly heated in chlorosilane, and the operation can be safely carried out; when the water content of the resin is higher than 1%, reducing the opening of the control valve, detecting the temperature of the pipeline after the resin and the chlorosilane are mixed by using a temperature measuring gun, and controlling the flow rate to enable the temperature of the pipeline to be lower than 40 ℃. Meanwhile, in the whole process, when the water content of the resin is large, the resin outflow speed is reduced, the phenomenon that the chlorosilane and the water in the resin are reacted to release heat excessively is avoided, and the resin is in uniform dense-phase flow through the observation of a transparent hose.
In the step (3), the power of the pump is 2-4 kw; the lift is 35m, the flow is 2.5m3And h, a hand valve is arranged at the outlet of the pump, the flow velocity of chlorosilane and resin at the throat of the Venturi tube is controlled through the opening degree of the hand valve, the flow velocity of the resin is checked at the transparent hose, and the control of the resin at 3-5m/h is more appropriate.
The method can lead out the heat released by the reaction of chlorosilane and water in time in the preparation process, and can effectively avoid the inactivation of resin active groups caused by the temperature rise. Various system risks brought in the resin filling process can be avoided in time, so that the resin filling process can be efficiently and safely completed.
The equipment filled with the chlorosilane adsorbent resin prepared by the method is also within the protection scope of the invention.
The device can be fully applied to chlorosilane adsorption impurity removal.
The active carrier substance in the resin micropores of the chlorosilane adsorption column can generate coordination compounds with trace boron chloride in the chlorosilane to be removed.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1. the invention has low energy consumption and small nitrogen consumption, adopts a small amount of resin to contact with a large amount of chlorosilane, has uniform heat release, and can ensure the activity of the resin and the filling safety.
2. The invention can avoid abrasion and pulverization caused by high-speed flowing of resin.
Drawings
FIG. 1 shows a chlorosilane adsorbent resin filling apparatus.
Detailed Description
The invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the description of the embodiments is only for illustrating the present invention and should not be taken as limiting the invention as detailed in the claims.
Example 1: chlorosilane adsorbent resin is filled in the device
(1) A resin (1.8 m) with a polystyrene polymer as a skeleton and polyhydroxy glucosamine as an active component3) Placing the resin buffer tank with water content of 0.5% for 2m3In the column, 30000kg of chlorosilane was placed on a chlorosilane resin adsorption column (bottom area: 2 m)2Height of 18m), and nitrogen is introduced into a self-operated regulating valve at a flow rate of 30Nm3About/h, the self-operated regulating valve can be automatically opened according to the nitrogen pressure in the nitrogen buffer tank so as to ensure positive pressure in the buffer tank;
(2) opening a resin outlet control valve, controlling the flow speed of the resin to be 3-5 m/s, enabling the resin to flow to a Venturi tube, and observing through a transparent hose to enable the resin to be in dense-phase flow;
(3) pressurizing chlorosilane by a shielding pump (the power is 2.5kw, the pressure is 0.4MPa, the lift is about 0.4MPa), enabling the chlorosilane to flow through a pipeline system, passing through a cooling system and a pump, reaching a Venturi tube, converting static pressure energy into kinetic energy, generating negative pressure (the negative pressure is obtained by converting the static pressure energy of liquid at the outlet of the pump into the kinetic energy and is micro negative pressure during normal operation) at a throat (the flow speed is 25m/s) of the Venturi tube, sucking the resin flowing into the Venturi tube in the step (2) into the pipeline system by the negative pressure, mixing the resin with the chlorosilane in the pipeline system to obtain resin adsorbed with the chlorosilane and the chlorosilane not adsorbed by the resin, and enabling the resin to enter the bottom of a chlorosilane resin adsorption column through an insertion tube;
(4) filtering the resin adsorbing the chlorosilane in the step (3) by using resin filtering caps (72 resin filtering caps with the diameter of 45mm and the height of 50mm) to stay in an adsorption column, and performing heat exchange on the chlorosilane not adsorbed by the resin and circulating water by using a double-pipe heat exchanger and then passing through a pump (the outlet circulation is 2.5 m)3H) pressurizing, then passing through the Venturi throat again and entering the inserting pipe together with the resin;
(5) adding 1.8m again when no material is in the transparent hose in the step (2)3And (5) resin, and circulating the steps (2) to (4) until the resin filling is finished, thus obtaining the resin.
Example 2: application of impurity removal
Using the apparatus packed with chlorosilane-based adsorbent resin prepared in example 1 (wherein the volume of the chlorosilane-based adsorbent column was 30 m)3) Removing trace of chlorosilaneBoron, the specific process is as follows:
(1) 40t/h of chlorosilane containing trace boron impurities produced by an upstream device is conveyed into a boron removal adsorption column 6 through a pipe orifice at the top of the adsorption column by a pump;
(2) the active carrier substance in the resin micropores can generate coordination compounds with trace boron chloride in the chlorosilane to be removed in the process that the chlorosilane flows downwards from the top of the adsorption column;
(3) a single boron removal adsorption column can process 40t of chlorosilane with the boron content of 500ppb per hour, the boron content at an outlet is 1-2 ppb, and the removal rate of boron impurities is over 99%.
(4) And (3) separating the chlorosilane and the resin at the filter cap after the resin is adsorbed and purified, and conveying the chlorosilane to a downstream device through a pipe orifice at the bottom of the adsorption column.
The invention provides a device and a method for filling chlorosilane adsorbent resin, and a method and a device for filling chlorosilane adsorbent resin, and a plurality of methods and ways for implementing the technical scheme, the above description is only a preferred embodiment of the invention, and it should be noted that, for those skilled in the art, a plurality of improvements and decorations can be made without departing from the principle of the invention, and the improvements and decorations should also be regarded as the protection scope of the invention. All the components not specified in the present embodiment can be realized by the prior art.
Claims (7)
1. A chlorosilane adsorption resin filling device is characterized by comprising a resin buffer tank (2), a chlorosilane resin adsorption column (6), a pump (4) and a Venturi tube (8); wherein, the outlet of the resin buffer tank (2) is connected with the throat part of the Venturi tube (8), the outlet of the Venturi tube (8) is connected with the inlet of the chlorosilane resin adsorption column (6), the outlet of the chlorosilane resin adsorption column (6) is connected with the inlet of the pump (4) through the cooling system (5), and the outlet of the pump (4) is connected with the inlet end of the Venturi tube (8);
wherein the inlet of the resin buffer tank (2) is connected with a nitrogen self-operated regulating valve (1), the outlet of the resin buffer tank is connected with a resin outlet control valve (3), and the top of the resin buffer tank is connected with a pressure gauge (11) and a resin filling port (12); wherein, the outlet control valve (3) of the resin buffer tank is connected with the throat of the Venturi tube (8) by a transparent hose (10) with flanges at two ends;
wherein the bottom of the chlorosilane resin adsorption column (6) contains a resin filter cap (7), and an insertion pipe (9) is arranged in the chlorosilane resin adsorption column (6); the resin filtering cap is a resin filtering cap consisting of a metal filament filtering net;
wherein, the pump (4) is a canned motor pump or a magnetic pump.
2. The filling device of chlorosilane adsorbent resin as claimed in claim 1, wherein the cooling system (5) is a double pipe heat exchanger with circulating water as cooling medium.
3. The method for filling chlorosilane adsorbent resin in the device of claim 1 or 2, comprising the steps of:
(1) placing resin to be filled into a resin buffer tank, placing chlorosilane into a chlorosilane resin adsorption column, and introducing gas into a self-operated regulating valve;
(2) opening a resin outlet control valve to allow resin to flow to the venturi;
(3) pressurizing chlorosilane by a pump, enabling the pressurized chlorosilane to flow through a pipeline system, enabling the pressurized chlorosilane to flow through a cooling system and the pump to reach a venturi tube, generating negative pressure at the throat of the venturi tube, sucking the chlorosilane and the resin flowing into the venturi tube in the step (2) into the pipeline system by the negative pressure, mixing to obtain resin adsorbing the chlorosilane and chlorosilane not adsorbed by the resin, and enabling the resin to enter a chlorosilane resin adsorption column through an insertion pipe;
(4) filtering the resin adsorbing the chlorosilane in the step (3) by using a resin filtering cap, staying in an adsorption column, exchanging heat of the chlorosilane not adsorbed by the resin by using a cooling system, pressurizing by using a pump, and simultaneously entering the inserting tube together with the resin through a Venturi throat;
(5) and (4) circulating the steps (2) to (4) until no resin flows through the transparent hose.
4. The method for filling chlorosilane adsorbent resin according to claim 3, wherein in the step (1), the resin is a thermally decomposed resin, the resin skeleton is polystyrene polymer, and the active component is polyhydroxy glucosamine; the gas is nitrogen.
5. The method for filling chlorosilane adsorbent resin as claimed in claim 3, wherein in the step (2), the resin outlet control valve is used for manually controlling the flow rate of the resin according to the water content of the resin, and when the water content of the resin is not more than 1%, the flow rate of the resin is controlled to be 3-5 m/s; when the water content of the resin is higher than 1%, controlling the flow rate to enable the temperature of the pipeline to be lower than 40 ℃.
6. The method for filling chlorosilane adsorbent resin as claimed in claim 3, wherein in the step (3), the power of the pump is 2-4 kW.
7. An apparatus filled with chlorosilane adsorbent resin prepared by the process of claim 3.
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| CN111243081A (en) * | 2020-01-08 | 2020-06-05 | 广西医科大学附属口腔医院 | Manufacturing method of resin filling guide plate beside digital chair and guide plate |
| CN111228856A (en) * | 2020-02-26 | 2020-06-05 | 苏州费斯特工业设备有限公司 | Safety monitoring system and control method of chemical purification device |
| CN111514497A (en) * | 2020-05-29 | 2020-08-11 | 应急管理部四川消防研究所 | Through-wall fire extinguishing device |
| EP4081480A1 (en) * | 2020-11-05 | 2022-11-02 | Wacker Chemie AG | Process for removing an impurity from a chlorosilane mixture |
| CN113086936B (en) * | 2021-03-22 | 2022-08-02 | 浙江嘉松科技有限公司 | Double-oil-tank oil supply system with oil-submersible pump |
| CN117105322A (en) * | 2023-10-10 | 2023-11-24 | 上海利顺环保工程有限公司 | Water treatment purifier |
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| US20150030520A1 (en) * | 2012-03-14 | 2015-01-29 | Centrotherm Photovoltaics Usa, Inc. | Trichlorosilane production |
| CN205471634U (en) * | 2016-02-24 | 2016-08-17 | 福建宁德核电有限公司 | Conveying device |
| CN208809520U (en) * | 2018-08-30 | 2019-05-03 | 新疆大全新能源股份有限公司 | Resin adsorption impurity device |
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