Catalytic system continuous circulation activation system
By combining a continuous cyclic activation system for the catalytic system with silane preparation and high-boiling-point cracking, and utilizing temperature-controlled phase inversion separation technology, the problems of reduced activity and high separation costs caused by the easy polymerization of liquid catalysts were solved. This achieved efficient and rapid separation of silicon tetrachloride and trichlorosilane and sustained catalyst activity, thereby improving production efficiency and economic benefits.
Patent Information
- Application Number
- CN202423242202.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-11-28
- Estimated Expiration
- 2034-12-27
AI Technical Summary
Traditional liquid catalysts are prone to initiating chlorosilane polymerization reactions during silane preparation, leading to reduced catalyst activity. Furthermore, traditional separation methods are costly, affecting silane purity and production efficiency.
A continuous cyclic activation system for the catalytic system is adopted, which combines silane preparation and high-boiling cracking, and utilizes temperature-controlled phase inversion separation technology. Through equipment such as reactive distillation columns, cracking reactors, and temperature-controlled separation tanks, the efficient and rapid separation of silicon tetrachloride and trichlorosilane is achieved.
It effectively solves the problem of increased catalyst viscosity, maintains high catalytic capacity of liquid catalyst, reduces separation costs, and improves product quality and system operating efficiency.
Smart Images
Figure CN223607028U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to a kind of catalytic system continuous circulation activation system, belong to the technical field of silane production. BACKGROUND
[0002] As an important basic raw material for semiconductor and photovoltaic industry, high-purity polysilicon is mainly prepared by modified Siemens method and silane fluidized bed method. Silane fluidized bed method becomes an important process improvement direction for polysilicon preparation due to its low production cost, low comprehensive energy consumption and low carbon emission. Silane, as the core raw material of this method, its preparation process mainly includes Komatsu method, disproportionation method and new silane method, etc. Among them, disproportionation method is the current mainstream process.
[0003] Traditional disproportionation method for preparing silane usually involves two-step reaction, i.e. trichlorosilane is first disproportionated into dichlorosilane, and then further prepared into silane. In order to improve energy utilization rate, reaction rectification technology is introduced in modern process, through multi-stage condensing system and reasonable utilization of cold source, significant reduction of energy consumption for silane preparation is realized.
[0004] However, the organic amine resin catalyst commonly used in industrialized disproportionation for preparing silane has problems of aging and deactivation, etc., which leads to difficulty and high cost for catalyst replacement. In order to solve this problem, researchers have proposed liquid catalyst solutions, such as ionic liquid catalyst and liquid catalyst mixed by aliphatic amine and aromatic amine. These liquid catalysts have advantages of no need for pretreatment, convenient replacement, clean and environmentally friendly, and high catalytic efficiency, etc. However, the high catalytic activity of liquid catalysts also easily leads to polymerization reaction of chlorosilane, forming high-boiling substances, which leads to reduction of catalyst activity and reaction obstruction.
[0005] In order to solve these problems brought by liquid catalysts, researchers have proposed a method combining silane preparation with high-boiling cracking, to realize cracking and separation of chlorosilane polymer into trichlorosilane and silicon tetrachloride. However, traditional separation method not only needs additional equipment and operation, leading to high separation cost, but also may affect the purity and production efficiency of silane to some extent. Therefore, it is urgent to provide a new and effective catalytic system continuous circulation activation system to solve the related technical problems in the prior art. UTILITY MODEL CONTENT
[0006] The utility model aims at providing a kind of catalytic system continuous circulation activation system, by combining silane preparation with high-boiling cracking, and adopting temperature control phase inversion separation technology, to realize efficient and rapid separation of silicon tetrachloride and trichlorosilane, while also reducing separation cost.
[0007] To solve the above technical problems, the utility model is realized by adopting the following technical solutions:
[0008] This utility model provides a continuous circulation activation system for a catalytic system, which includes: a reactive distillation column, a reactive distillation column top condenser, a reboiler, a cracking reactor, a first storage tank, a second storage tank, and a temperature-controlled separation tank;
[0009] The first inlet in the middle of the reactive distillation column is connected to pipe eleven for supplying liquid catalyst and / or trichlorosilane and / or dichlorosilane into the column; the reboiler is located at the bottom of the reactive distillation column; a reactive distillation column top condenser is provided at the top of the reactive distillation column for discharging silane gas and / or dichlorosilane through pipe thirteen.
[0010] The outlet of the reboiler of the reactive distillation column is connected to the first inlet of the cracking reactor via pipe 15, and pump 1 is installed on pipe 15; the second inlet of the cracking reactor is connected to pipe 43, which is used to supply HCl into the cracking reactor to carry out a cracking reaction with the material output from the reboiler, and pump 2 is installed on pipe 43.
[0011] The first outlet of the pyrolysis reactor is connected to the inlet of the first storage tank via pipe 42; the inlet of the temperature-controlled separator is connected to the second outlet of the first storage tank via pipe 104, for separating the liquid catalyst, trichlorosilane, and silicon tetrachloride; the outlet of the temperature-controlled separator is connected to the inlet of the second storage tank via pipe 106, and the outlet of the second storage tank is connected to the second inlet of the reactive distillation column via pipe 14, for conveying the liquid catalyst and trichlorosilane into the column, and a pump 3 is installed on pipe 14; the outlet of the temperature-controlled separator is also connected to a corresponding separation system or distillation system via pipe 105.
[0012] Optionally, corresponding valves are provided on pipes eleven, thirteen, fifteen, forty-two, forty-three, 104, 105 and 106.
[0013] Optionally, the continuous circulation activation system of the catalytic system further includes: a pyrolysis reactor condenser and a pipeline forty-one; the second outlet of the pyrolysis reactor is connected to the inlet of the pyrolysis reactor condenser through the pipeline forty-one, for conveying excess HCl and chlorosilane gas in the pyrolysis reactor to the pyrolysis reactor condenser for condensation through the pipeline forty-one.
[0014] Optionally, the pipe forty-one is equipped with a corresponding valve.
[0015] Optionally, the silane preparation cycle activation system further includes: pipe twelve, which is connected to the top of the reactive distillation column for discharging non-condensable gases from the column.
[0016] Optionally, one end of the pipeline twelve is communicated with the top outlet of the reaction rectifying tower, and the other end is communicated with the reaction rectifying tower overhead condenser, which is used for cryogenic separation and recovery of silane gas.
[0017] Optionally, the catalytic system continuous circulation activation system further comprises a pipeline fifty-one; the first outlet of the first storage tank is communicated with the inlet of the cracking reactor condenser through the pipeline fifty-one, which is used for conveying the residual HCl in the first storage tank to the cracking reactor condenser for condensation.
[0018] Optionally, the pipeline fifty-one is provided with a corresponding valve.
[0019] Optionally, the first outlet of the cracking reactor condenser is communicated with a pipeline sixty-four, which is used for conveying the condensed silicon tetrachloride, trichlorosilane and liquid catalyst in the cracking reactor condenser to the corresponding separation system for separation.
[0020] Optionally, the pipeline sixty-four is provided with a corresponding valve.
[0021] Optionally, the second outlet of the cracking reactor condenser is communicated with the second inlet of the cracking reactor in sequence through a pipeline sixty-one, a pipeline sixty-three and a pipeline forty-three, which is used for conveying the non-condensable gas HCl in the cracking reactor condenser back to the cracking reactor.
[0022] Optionally, the pipeline sixty-one, the pipeline sixty-three and the pipeline forty-three are provided with corresponding valves.
[0023] Optionally, the second outlet of the cracking reactor condenser is communicated with the pipeline sixty-two through the pipeline sixty-one, which is used for recycling or treating the non-condensable gas HCl in the cracking reactor condenser through the pipeline sixty-two.
[0024] Optionally, the pipeline sixty-two is provided with a corresponding valve.
[0025] Optionally, the pipeline forty-three is further communicated with a pipeline seventy-one, which is used for supplementing HCl required for cracking reaction through the pipeline seventy-one.
[0026] Optionally, the pipeline seventy-one is provided with a corresponding valve.
[0027] Optionally, the catalytic system continuous circulation activation system further comprises a pipeline fifty-two, which is communicated with the second outlet of the first storage tank, which is used for conveying the liquid catalyst-containing chlorosilane after removing HCl to the corresponding separation system through the pipeline fifty-two for separation of liquid catalyst and chlorosilane.
[0028] Optionally, the pipeline fifty-two is provided with a corresponding valve.
[0029] Optionally, the outlet of the pipeline 105 is communicated with the corresponding rectifying system for separating the silicon tetrachloride and the liquid catalyst; wherein the liquid catalyst is transported to the cracking reactor condenser or the reaction rectifying tower through the corresponding pipeline.
[0030] Optionally, the continuous circulation activation system of the catalytic system further comprises a third storage tank, a membrane separator, a fourth pump, a pipeline 113 and a pipeline 114 as a separation system for separating the liquid catalyst and the silicon tetrachloride.
[0031] The inlet of the third storage tank is communicated with the pipeline 105, the outlet of the third storage tank is communicated with the inlet of the membrane separator through the pipeline 107, and the fourth pump is arranged on the pipeline 107.
[0032] The first outlet of the membrane separator is communicated with the third inlet of the cracking reactor through the pipeline 113 for transporting the liquid catalyst and part of the silicon tetrachloride intercepted by the membrane into the cracking reactor, and the pipeline 114 is communicated with the second outlet of the membrane separator for transporting the silicon tetrachloride.
[0033] Compared with the prior art, the catalytic system continuous circulation activation system has the following beneficial effects:
[0034] The embodiment effectively solves the problem of viscosity increase of the catalyst system caused by chlorosilane polymerization by combining silane preparation and high-boiling cracking and using the ionic liquid catalyst, so that the liquid catalyst can continuously maintain high catalytic capacity, and the consumption of the catalyst is reduced. On this basis, the efficient and rapid separation of silicon tetrachloride and trichlorosilane is realized by using the temperature control separation tank and the membrane separator and other equipment through the temperature control separation technology, and the liquid catalyst, trichlorosilane and silicon tetrachloride can be effectively recovered, realizing energy recycling. This not only improves the product quality, but also reduces the separation cost, and the operation efficiency and economic benefit of the overall system are also significantly improved. BRIEF DESCRIPTION OF DRAWINGS
[0035] Figure 1 Fig. 1 is a structural schematic diagram of one embodiment of the continuous circulation activation system of the catalytic system of the utility model;
[0036] Figure 2 Fig. 2 is a structural schematic diagram of another embodiment of the continuous circulation activation system of the catalytic system of the utility model;
[0037] In the figure: 1-reaction rectifying column; 11-pipe eleven; 12-pipe twelve; 13-pipe thirteen; 14-pipe fourteen; 15-pipe fifteen; 2-reboiler; 3-pump one; 4-cracking reactor; 41-pipe forty-one; 42-pipe forty-two; 43-pipe forty-three; 5-first storage tank; 51-pipe fifty-one; 52-pipe fifty-two; 6-cracking reactor condenser; 61-pipe sixty-one; 62-pipe sixty-two; 63-pipe sixty-three; 64-pipe sixty-four; 7-pump two; 71-pipe seventy-one; 8-reaction rectifying column overhead condenser; 101-temperature control separation tank; 102-second storage tank; 103-pump three; 104-pipe one zero four; 105-pipe one zero five; 106-pipe one zero six; 107-pipe one zero seven; 110-third storage tank; 111-pump four; 112-membrane separator; 113-pipe one hundred and thirteen; 114-pipe one hundred and fourteen. DETAILED DESCRIPTION
[0038] The utility model will be described further below in conjunction with the drawings. The following examples are only used to explain the technical scheme of the utility model more clearly, and cannot limit the protection scope of the utility model.
[0039] Example 1
[0040] This example introduces a kind of continuous circulation activation system of catalytic system, it includes: reaction rectifying column 1, reaction rectifying column overhead condenser 8, reboiler 2, cracking reactor 4, first storage tank 5, second storage tank 102 and temperature control separation tank 101;
[0041] The first inlet of the middle part of the reaction rectifying column 1 is communicated with pipe eleven 11 for liquid catalyst and / or trichlorosilane and / or dichlorodisilane to enter the tower;The reboiler 2 is arranged at the bottom of the reaction rectifying column 1;The reaction rectifying column 1 top is equipped with reaction rectifying column overhead condenser 8, for silane gas or / and dichlorodisilane is discharged by pipe thirteen 13;
[0042] The outlet of the column of the reaction rectifying column 1 is communicated with the first inlet of the cracking reactor 4 by pipe fifteen 15, and pump one 3 is arranged on the pipe fifteen 15;The second inlet of the cracking reactor 4 is communicated with pipe forty-three 43, for HCl enters into cracking reactor 4 and carries out cracking reaction with the material output from column, and pump two 7 is arranged on the pipe forty-three 43;
[0043] The first outlet of the cracking reactor 4 is communicated with the inlet of the first storage tank 5 through pipeline forty-two 42; the inlet of the temperature control separation tank 101 is communicated with the second outlet of the first storage tank 5 through pipeline one-zero-four 104, for separating the liquid catalyst, trichlorosilane and silicon tetrachloride; the outlet of the temperature control separation tank 101 is communicated with the inlet of the second storage tank 102 through pipeline one-zero-six 106, and the outlet of the second storage tank 102 is communicated with the second inlet of the reaction rectifying tower 1 through pipeline fourteen 14, for transporting the liquid catalyst and trichlorosilane into the tower to realize recycling; a pump three 103 is arranged on the pipeline fourteen 14; the outlet of the temperature control separation tank 101 is also communicated with the corresponding separation system or rectification system through pipeline one-zero-five 105.
[0044] In the actual application process of the embodiment, the liquid catalyst and / or trichlorosilane and / or dichlorodisilane and other raw materials enter the reaction rectifying tower 1 through pipeline eleven 11. In the reaction rectifying tower 1, the relevant raw materials and catalysts react at a set temperature and pressure. The silane gas and / or dichlorodisilane generated in the reaction process is condensed by the reaction rectifying tower overhead condenser 8 and then discharged through pipeline thirteen 13.
[0045] Further, the material in the tower kettle of the reaction rectifying tower 1 enters the cracking reactor 4 through pipeline fifteen 15. In the cracking reactor 4, HCl enters through pipeline forty-three 43 and reacts with the material output from the tower kettle. Then, the product after the cracking reaction is stored in the first storage tank 5.
[0046] Further, the material in the first storage tank 5 enters the temperature control separation tank 101 through pipeline one-zero-four 104 for separation. In the temperature control separation tank 101, the liquid catalyst, trichlorosilane and silicon tetrachloride are separated. Among them, the liquid catalyst and trichlorosilane separated in the upper layer of the temperature control separation tank 101 enter the second storage tank 102 through pipeline one-zero-six 106, and then are transported back to the second inlet of the reaction rectifying tower 1 through pipeline fourteen 14 under the action of the pump three 103, forming continuous circulation. The liquid catalyst and silicon tetrachloride separated in the lower layer of the temperature control separation tank 101 enter the corresponding separation system or rectification system through pipeline one-zero-five 105 for next step processing.
[0047] In general, the embodiment can realize the continuous circulation activation process of the catalyst system through the steps of accurate raw material and catalyst addition, reaction rectifying tower operation, cracking reaction, product storage and separation, and catalyst and raw material recycling.
[0048] Embodiment 2
[0049] Reference Figure 1The embodiment will introduce the related structure composition and function realization process of the continuous circulation activation system of the catalytic system, as follows.
[0050] In the actual application process of the embodiment, the liquid catalyst and / or trichlorosilane and / or dichlorodisilane enters the reaction rectification tower 1 from the pipeline eleven 11, and the dismutation reaction is carried out in the reaction rectification tower 1 to prepare silane or / and dichlorodisilane. The bottom of the reaction rectification tower 1 is equipped with a reboiler 2 for providing a heat source.
[0051] In the dismutation reaction process, silane gas or / and dichlorodisilane is extracted from the pipeline thirteen 13, and non-condensable gas is discharged from the pipeline twelve 12 for recovery or treatment. It is worth mentioning that in addition to being directly treated as non-condensable gas, the pipeline twelve 12 can be in communication with the top outlet of the reaction rectification tower 1 at one end and in communication with the reaction rectification tower overhead condenser 8 at the other end, for further cryogenic separation and recovery of silane or a small amount of chlorosilane (such as monochlorotrihydrogen silane, etc.). The pipeline twelve 12 and the pipeline thirteen 13 are both provided with corresponding valves. The material in the tower kettle of the reaction rectification tower 1 enters the cracking reaction kettle 4 through the pump one 3 and the pipeline fifteen 15 for further cracking treatment. The pipeline fifteen 15 is also provided with a corresponding valve.
[0052] HCl enters the cracking reaction kettle 4 through the pipeline forty-three 43 to carry out a cracking reaction with the material in the tower kettle of the reaction rectification tower 1. The pipeline forty-three 43 is provided with a corresponding valve.
[0053] The excess HCl and chlorosilane gas in the cracking reaction kettle 4 enter the cracking reaction kettle condenser 6 through the pipeline forty-one 41 for condensation. The condensed silicon tetrachloride, trichlorosilane and a small amount of catalyst pass through the pipeline sixty-five 65 to the trichlorosilane and silicon tetrachloride separation system for separation. The pipeline forty-one 41 and the pipeline sixty-five 65 are both provided with corresponding valves.
[0054] In the cracking reaction kettle condenser 6, the non-condensable gas is mainly HCl, which can pass through the pipeline sixty-one 61 and the pipeline sixty-three 63 in turn, be pressurized by the pump two 7 and then return to the cracking reaction kettle 4 through the pipeline forty-three 43, or be directly treated through the pipeline sixty-two 62. The pipeline sixty-one 61 and the pipeline sixty-three 63 are provided with corresponding valves. In addition, the required HCl for cracking can also be supplemented through the pipeline seventy-one 71 and the corresponding valve.
[0055] After the polysilane in the cracking reactor 4 is cracked, the chlorosilane containing catalyst is introduced into the first storage tank 5 through pipeline forty-two 42. In the first storage tank 5, the residual HCl is further removed, and the residual HCl is further condensed and separated through pipeline fifty-one 51 into the cracking reactor condenser 6. Among them, the pipeline forty-two 42 and the pipeline fifty-one 51 are also provided with corresponding valves.
[0056] Further, the chlorosilane containing catalyst after removing HCl is introduced into the temperature-controlled separation tank 101 through pipeline one hundred and four 104 for separation. A coil is arranged inside the temperature-controlled separation tank 101. In actual application, the operator can control the temperature of the water entering the coil to control the temperature of the temperature-controlled separation tank 101, thereby realizing the effective separation of the liquid catalyst, trichlorosilane and silicon tetrachloride. Among them, the silicon tetrachloride and the liquid catalyst separated in the lower layer of the temperature-controlled separation tank 101 are introduced into the corresponding separation system or rectification system through pipeline one hundred and five 105 to realize the separation of the liquid catalyst and the silicon tetrachloride, and the liquid catalyst and trichlorosilane separated in the upper layer of the temperature-controlled separation tank 101 are introduced into the second storage tank 102 through pipeline one hundred and six 106, and then returned to the reaction rectification column 1 through pipeline fourteen 14 by pump three 103 for recycling.
[0057] In addition, the chlorosilane containing liquid catalyst after removing HCl can also be directly separated into liquid catalyst and chlorosilane through pipeline fifty-two 52, which communicates with the second outlet of the first storage tank. Among them, the pipeline fourteen 14, the pipeline fifty-two 52, the pipeline one hundred and four 104, the pipeline one hundred and five 105 and the pipeline one hundred and six 106 are all provided with corresponding valves. In addition, it is worth mentioning that the liquid catalyst used in this embodiment is an ionic liquid catalyst.
[0058] Embodiment 3
[0059] Reference Figure 2 This embodiment will introduce another related structure composition and function realization process of the continuous circulation activation system of the catalyst system, as follows.
[0060] In the actual application process of this embodiment, the liquid catalyst and / or trichlorosilane and / or dichlorodihydrogen silicon are introduced into the reaction rectification column 1 from pipeline eleven 11 to carry out disproportionation reaction to prepare silane or / and dichlorodihydrogen silicon. Among them, the pipeline eleven 11 is provided with a corresponding valve; the bottom of the reaction rectification column 1 is provided with a reboiler 2 for providing heat source.
[0061] During the disproportionation reaction, silane gas or / and dichlorodisilane is taken out from pipeline thirteen 13, and non-condensed gas is discharged from pipeline twelve 12 for recovery or treatment. Similarly, in addition to being directly treated as non-condensed gas, pipeline twelve 12 can be in communication with the top outlet of the reaction rectification tower 1 at one end and the reaction rectification tower overhead condenser 8 at the other end, for further cryogenic separation to recover silane or a small amount of chlorosilane (such as chlorotrihydrogen silane, etc.) therein. The pipeline twelve 12 and the pipeline thirteen 13 are each provided with a corresponding valve. The material in the bottom of the reaction rectification tower 1 is pumped by pump one 3 and pipeline fifteen 15 into the cracking reaction kettle 4 for further cracking treatment. The pipeline fifteen 15 is also provided with a corresponding valve.
[0062] HCl is introduced into the cracking reaction kettle 4 through pipeline forty-three 43 to react with the material in the bottom of the reaction rectification tower 1. The pipeline forty-three 43 is provided with a corresponding valve.
[0063] The excess HCl and chlorosilane gas in the cracking reaction kettle 4 are introduced into the cracking reaction kettle condenser 6 through pipeline forty-one 41 for condensation. The condensed silicon tetrachloride, trichlorosilane and a small amount of catalyst are separated through pipeline sixty-five 65 to a trichlorosilane and silicon tetrachloride separation system. The pipeline forty-one 41 and the pipeline sixty-five 65 are each provided with a corresponding valve.
[0064] In the cracking reaction kettle condenser 6, the non-condensed gas is mainly HCl, which can be returned to the cracking reaction kettle 4 through pipeline sixty-one 61 and pipeline sixty-three 63 in sequence, pressurized by pump two 7, and then passed through pipeline forty-three 43, or directly treated through pipeline sixty-two 62. The pipeline sixty-one 61 and the pipeline sixty-three 63 are each provided with a corresponding valve. In addition, the required HCl can also be supplemented through pipeline seventy-one 71 and the corresponding valve.
[0065] After the polysilane in the cracking reaction kettle 4 is cracked, it is introduced into the first storage tank 5 through pipeline forty-two 42. In the first storage tank 5, the residual HCl is further removed, and the residual HCl is introduced into the cracking reaction kettle condenser 6 through pipeline fifty-one 51 for further condensation and separation. The pipeline forty-two 42 and the pipeline fifty-one 51 are each provided with a corresponding valve.
[0066] Further, the chlorosilane containing catalyst after removal of HCl is introduced into the temperature-controlled separation tank 101 through pipeline one zero four 104 for separation. A coil is arranged inside the temperature-controlled separation tank 101. In actual application, the operator can control the water temperature entering the coil to control the temperature of the temperature-controlled separation tank 101, thereby realizing effective separation of the liquid catalyst, trichlorosilane and silicon tetrachloride.
[0067] The silicon tetrachloride and liquid catalyst separated from the lower layer of the temperature control separation tank 101 are communicated with the third storage tank 110 through the pipeline one zero five 105. The third storage tank 110 is communicated with the membrane separator 112 through the pipeline one zero seven 107, and the liquid catalyst and silicon tetrachloride are separated in the membrane separator 112 under the action of the pump four 111. The catalyst and part of the silicon tetrachloride intercepted by the membrane are returned to the cracking reaction kettle 4 through the pipeline one one three 113 from the first outlet of the membrane separator 112, so as to realize recycling. The second outlet of the membrane separator 112 is communicated with the pipeline one one four 114, and the silicon tetrachloride is transported through the pipeline one one four 114, so as to realize recycling.
[0068] In addition, the outlet of the pipeline one zero five 105 can also be communicated with the corresponding rectification system, and the silicon tetrachloride and the liquid catalyst can also be separated. The liquid catalyst is returned to the cracking reaction kettle condenser 6 or the reaction rectification tower 1 through the corresponding pipeline.
[0069] The liquid catalyst and trichlorosilane separated from the upper layer of the temperature control separation tank 101 are communicated with the second storage tank 102 through the pipeline one zero six 106, and then returned to the reaction rectification tower 1 through the pipeline fourteen 14 by the pump three 103, so as to realize recycling.
[0070] The pipeline fourteen 14, the pipeline one zero four 104, the pipeline one zero five 105 and the pipeline one zero six 106 are all provided with corresponding valves. In addition, it should be pointed out that the liquid catalyst used in the embodiment is also an ionic liquid catalyst.
[0071] In the description of the utility model disclosure / the present application, it should be understood that the terms "center", "upper", "lower", "front", "rear", "left", "right", "inner", "outer" and the like indicate the orientation or positional relationship shown in the drawings, and are only used to explain the relative position relationship, movement condition and the like between the components in a certain specific posture. If the specific posture changes, the directional indication also changes accordingly. It is only for the convenience of describing the utility model disclosure / the present application and simplifying the description, and does not indicate or imply that the indicated device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the utility model disclosure / the present application.
[0072] In the description of the utility model discloses / the application, it is necessary to explain, unless another explicit provision and limitation, the term " install " " be connected " " connection " should do broad sense understanding, for example, can be fixed connection, also can be detachable connection, or integrally connected, can be mechanical connection, also can be electrical connection, can be directly connected, also can indirectly be connected through the intermediate medium, can be the intercommunication of two elements internally. For ordinary skilled person in the art, the specific meaning of the above-mentioned term in the utility model discloses / the application can be understood by specific circumstances. In addition, in the description of the embodiment, unless otherwise stated, the meaning of " multiple " is two or more than two.
[0073] The above only is the preferred embodiment of the utility model, it should be pointed out, for ordinary skilled person in the art, on the premise of not departing from the technical principle of the utility model, can also make a number of improvements and deformation, these improvements and deformation also should be considered the protection scope of the utility model.
Claims
1. A continuous cycle activation system of a catalytic system, characterized in that, The application relates to a reaction rectification tower (1), a reaction rectification tower overhead condenser (8), a reboiler (2), a cracking reactor (4), a first storage tank (5), a second storage tank (102) and a temperature-controlled separation tank (101). A first inlet in the middle of the reaction rectification tower (1) is communicated with a pipeline XI (11) for feeding liquid catalyst and / or trichlorosilane and / or dichlorodisilane into the tower; the reboiler (2) is arranged at the bottom of the reaction rectification tower (1); and a reaction rectification tower overhead condenser (8) is arranged at the top of the reaction rectification tower (1) and used for discharging silane gas or / and dichlorodisilane through a pipeline XIII (13). An outlet of a tower kettle of the reaction rectification tower (1) is communicated with a first inlet of the cracking reactor (4) through a pipeline XV (15), a pump I (3) is arranged on the pipeline XV (15); a second inlet of the cracking reactor (4) is communicated with a pipeline XLIII (43) and used for feeding HCl into the cracking reactor (4) to carry out cracking reaction with materials output from the tower kettle, and a pump II (7) is arranged on the pipeline XLIII (43); A first outlet of the cracking reactor (4) is communicated with an inlet of the first storage tank (5) through a pipeline XLII (42); an inlet of the temperature-controlled separation tank (101) is communicated with a second outlet of the first storage tank (5) through a pipeline 104 (104) and used for separating liquid catalyst, trichlorosilane and silicon tetrachloride; an outlet of the temperature-controlled separation tank (101) is communicated with an inlet of the second storage tank (102) through a pipeline 106 (106), an outlet of the second storage tank (102) is communicated with a second inlet of the reaction rectification tower (1) through a pipeline XIV (14) and used for feeding liquid catalyst and trichlorosilane into the tower, and a pump III (103) is arranged on the pipeline XIV (14); and the outlet of the temperature-controlled separation tank (101) is also communicated with a corresponding separation system or rectification system through a pipeline 105 (105). Valves are arranged on the pipeline XI (11), the pipeline XIII (13), the pipeline XV (15), the pipeline XLII (42), the pipeline XLIII (43), the pipeline 104 (104), the pipeline 105 (105) and the pipeline 106 (106).
2. Catalytic system continuous cycle activation system according to claim 1, characterized in that, The application further comprises a cracking reactor condenser (6) and a pipeline XLI (41).
3. Catalytic system continuous cycle activation system according to claim 1 or 2, characterized in that, A second outlet of the cracking reactor (4) is communicated with an inlet of the cracking reactor condenser (6) through the pipeline XLI (41) and used for feeding excessive HCl and chlorosilane gas in the cracking reactor (4) into the cracking reactor condenser (6) to carry out condensation; and a valve is arranged on the pipeline XLI (41). The application further comprises a pipeline XII (12) and a pipeline LI (51).
4. The continuous cyclic activation system of a catalytic system according to claim 3, characterized in that, The pipeline twelve (12) is communicated with the top of the reaction rectification tower for discharging non-condensable gas in the tower; or one end of the pipeline twelve (12) is communicated with the top outlet of the reaction rectification tower, and the other end is communicated with the reaction rectification tower overhead condenser (8) for cryogenic separation and recovery of silane gas; The first outlet of the storage tank (5) is communicated with the inlet of the cracking reactor condenser (6) through the pipeline fifty-one (51) for conveying the residual HCl in the storage tank (5) to the cracking reactor condenser (6) for condensation through the pipeline fifty-one (51); Wherein, the pipeline twelve (12) and the pipeline fifty-one (51) are provided with corresponding valves.
5. The continuous cyclic activation system of a catalytic system according to claim 4, characterized in that, The first outlet of the cracking reactor condenser (6) is communicated with the pipeline sixty-four (64) for conveying the condensed silicon tetrachloride, trichlorosilane and liquid catalyst in the cracking reactor condenser (6) to the corresponding separation system for separation; wherein, the pipeline sixty-four (64) is provided with a corresponding valve.
6. The continuous cyclic activation system of a catalytic system according to claim 5, characterized in that, The second outlet of the cracking reactor condenser (6) is communicated with the second inlet of the cracking reactor (4) through the pipeline sixty-one (61), the pipeline sixty-three (63) and the pipeline forty-three (43) in sequence for conveying the non-condensable gas HCl in the cracking reactor condenser (6) back to the cracking reactor (4); The pipeline forty-three (43) is also communicated with the pipeline seventy-one (71) for supplementing HCl required for cracking reaction through the pipeline seventy-one (71); Wherein, the pipeline sixty-one (61), the pipeline sixty-three (63), the pipeline forty-three (43) and the pipeline seventy-one (71) are provided with corresponding valves.
7. The continuous cyclic activation system of a catalytic system according to claim 5, characterized in that, The second outlet of the cracking reactor condenser (6) is communicated with the pipeline sixty-two (62) through the pipeline sixty-one (61) for recycling or processing the non-condensable gas HCl in the cracking reactor condenser (6) through the pipeline sixty-two (62); wherein, the pipeline sixty-two (62) is provided with a corresponding valve.
8. Catalytic system continuous cycle activation system according to claim 6 or 7, characterized in that, Further comprising a pipeline fifty-two (52); The pipeline fifty-two (52) is communicated with the second outlet of the first storage tank (5) for conveying the chlorosilane containing liquid catalyst after removing HCl to the corresponding separation system through the pipeline fifty-two (52) for separation of liquid catalyst and chlorosilane; wherein, the pipeline fifty-two (52) is provided with a corresponding valve.
9. The continuous cyclic activation system of a catalytic system according to claim 8, characterized in that, The outlet of the pipeline one zero five (105) is communicated with the corresponding rectification system for separating silicon tetrachloride and liquid catalyst; Wherein, the liquid catalyst is conveyed to the cracking reactor condenser (6) or the reaction rectification tower (1) through the corresponding pipeline.
10. The continuous cyclic activation system of a catalytic system according to claim 8, characterized in that, Further comprising a third storage tank (110), a membrane separator (112), a pump four (111), a pipeline one hundred and thirteen (113) and a pipeline one hundred and fourteen (114) as a separation system for separating liquid catalyst and silicon tetrachloride; The inlet of the third storage tank (110) is communicated with pipeline 105 (105), the outlet of the third storage tank (110) is communicated with the inlet of the membrane separator (112) through pipeline 107 (107), and the pump four (111) is arranged on the pipeline 107 (107); The first outlet of the membrane separator (112) is communicated with the third inlet of the cracking reaction kettle (4) through pipeline 113 (113), which is used for conveying the liquid catalyst and part of the silicon tetrachloride intercepted by the membrane into the cracking reaction kettle (4); and the pipeline 114 is communicated with the second outlet of the membrane separator (112), which is used for conveying the silicon tetrachloride.