CN116808958A - Device and method for preparing silane through chlorosilane disproportionation reaction - Google Patents
Device and method for preparing silane through chlorosilane disproportionation reaction Download PDFInfo
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- CN116808958A CN116808958A CN202310738295.1A CN202310738295A CN116808958A CN 116808958 A CN116808958 A CN 116808958A CN 202310738295 A CN202310738295 A CN 202310738295A CN 116808958 A CN116808958 A CN 116808958A
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 102
- 238000007323 disproportionation reaction Methods 0.000 title claims abstract description 58
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 46
- 238000000926 separation method Methods 0.000 claims abstract description 326
- 238000006243 chemical reaction Methods 0.000 claims abstract description 207
- 239000007788 liquid Substances 0.000 claims abstract description 65
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 61
- 238000000605 extraction Methods 0.000 claims abstract description 55
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims description 52
- 239000000047 product Substances 0.000 claims description 45
- 239000005052 trichlorosilane Substances 0.000 claims description 34
- 239000007795 chemical reaction product Substances 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 25
- 238000012856 packing Methods 0.000 claims description 24
- 239000003054 catalyst Substances 0.000 claims description 21
- 238000009835 boiling Methods 0.000 claims description 16
- 230000011218 segmentation Effects 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 7
- 239000005977 Ethylene Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000003507 refrigerant Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims 3
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 13
- PPDADIYYMSXQJK-UHFFFAOYSA-N trichlorosilicon Chemical compound Cl[Si](Cl)Cl PPDADIYYMSXQJK-UHFFFAOYSA-N 0.000 description 32
- 238000001816 cooling Methods 0.000 description 15
- BUMGIEFFCMBQDG-UHFFFAOYSA-N dichlorosilicon Chemical compound Cl[Si]Cl BUMGIEFFCMBQDG-UHFFFAOYSA-N 0.000 description 13
- 239000000945 filler Substances 0.000 description 10
- 239000003957 anion exchange resin Substances 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 8
- 238000011049 filling Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000284 extract Substances 0.000 description 4
- 239000012263 liquid product Substances 0.000 description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical class Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- -1 sodium aluminum fluoride Chemical compound 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/04—Hydrides of silicon
- C01B33/043—Monosilane
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0036—Multiple-effect condensation; Fractional condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a device and a method for preparing silane by disproportionation reaction of chlorosilane, wherein the preparation device comprises a reaction separation section, a cold section, a stripping section, a feed inlet and a reboiler; the preparation device adopts a single-tower structure of a reaction separation tower or a double-tower parallel structure of the reaction separation tower and a cold separation tower; when the device adopts a single-tower structure, a high-purity silane extraction pipeline is arranged at the top of the reaction separation tower, and a silicon tetrachloride extraction pipeline is arranged at the bottom of the reaction separation tower; the device adopts a double-tower parallel structure, a high-purity silane extraction pipeline is arranged at the top of a cold separation tower, and a silicon tetrachloride extraction pipeline is arranged at the bottom of a reaction separation tower. Chlorosilane enters a reaction separation tower, flows through a reaction separation section, gas upwards passes through two or more cold sections to separate and purify products, and liquid downwards flows through a stripping section to separate and purify the products; the invention has simple process equipment, can realize multi-step disproportionation reaction by only one reaction separation tower, and can simultaneously carry out reaction and separation, and the conversion rate can reach more than 90 percent.
Description
Technical Field
The invention relates to a device and a method for preparing silane by using chlorosilane as a raw material, and particularly relates to a device and a method for preparing high-purity silane by adding a plurality of (at least two) cold segments, and performing full reaction separation through mass transfer separation and heat exchange parts by using disproportionation reaction.
Background
Polysilicon is a high-quality semiconductor material, and is one of the main materials of solar cells. Currently, polysilicon production methods mainly include an improved siemens method, a silane decomposition method, a zinc reduction method, a silicon dioxide reduction method and the like. The silane decomposition method can prepare polysilicon with higher purity, the purity can reach electronic grade or even higher, and meanwhile, the production process flow is simple, no corrosive gas is generated, the equipment loss is small, and the production cost is low.
There are many current methods for preparing silanes, three of which are the most predominant: silicon magnesium alloy method, sodium aluminum fluoride method and chlorosilane disproportionation method. The three processes are comprehensively evaluated, and the process for preparing the silane by the chlorosilane disproportionation method is more suitable in combination with the current domestic national conditions. The technology for preparing high-purity silane by using chlorosilane disproportionation method is firstly proposed by UCC company, and patent US4340574 proposes a technology for preparing silane by using trichlorosilane as a raw material through fixed bed multi-step disproportionation reaction instead of direct decomposition reaction of trichlorosilane, wherein the disproportionation reaction is followed by a rectification purification procedure to prepare high-purity silane and silicon tetrachloride. In the subsequent decomposition reaction, almost only hydrogen (H 2 ) And metallic silicon, avoiding the direct decomposition of trichlorosilane to produce hydrogen chloride (HCl) class of corrosive compounds. After that, the germany bayer company simplifies the process, and only one reaction rectifying tower is used to obtain high-purity silane product, and in order to reduce the difficulty of process implementation and improve the purity of silane, a process in which one reaction rectifying tower and one rectifying and purifying tower are operated in combination is also provided, and patent US6905576 is filed. There have been many researchers who have improved the above two processes in detail, but there has been no substantial process innovation.
The existing technology for preparing silane by disproportionation of chlorosilane mainly takes trichlorosilane as a reaction raw material, and prepares the silane by multi-step disproportionation reaction, so that the disproportionation reaction conversion rate is low, and in order to fully utilize the raw material, multiple times of circulation are needed, so that disproportionation reaction equipment is huge and complex, and the energy consumption is high. The invention provides a novel process for preparing silane by using chlorosilane disproportionation reaction, which adopts trichlorosilane and dichlorosilane as raw materials, adopts a reaction separation tower, and performs reaction and separation simultaneously.
Disclosure of Invention
The invention provides a process for preparing silane by using chlorosilane disproportionation reaction, which uses trichlorosilane and dichlorosilane as raw materials, and prepares high-purity silane by mass transfer separation and heat exchange partial full reaction separation through disproportionation reaction.
The disproportionation reaction involved in the invention is as follows:
wherein SiH is 3 Cl is unstable and the presence of this species is barely detectable in the presence of the catalyst. Thus, the latter two reactions can be combined in engineering into one-step reactions, namely:
the technical scheme of the invention is as follows:
the invention provides a device for preparing silane by a chlorosilane disproportionation reaction; the preparation device comprises a reaction separation section (1), a cold section (2) and a stripping section (3), a feed inlet (5) and a reboiler (4); the preparation device adopts a single-tower structure of a reaction separation tower or a double-tower parallel structure of the reaction separation tower and a cold separation tower; when the device adopts a single-tower structure, a high-purity silane extraction pipeline is arranged at the top of the reaction separation tower, and a silicon tetrachloride extraction pipeline is arranged at the bottom of the reaction separation tower; the device adopts a double-tower parallel structure, a high-purity silane extraction pipeline is arranged at the top of a cold separation tower, and a silicon tetrachloride extraction pipeline is arranged at the bottom of a reaction separation tower.
The device for preparing silane by the disproportionation reaction of the chlorosilane; when a single-tower structure of the reaction separation tower is adopted, a silicon tetrachloride extraction pipeline of the tower kettle is connected with a tower kettle reboiler (4); the stripping section (3), the raw material feed inlet (5), the reaction separation section (1), at least more than two cold sections (2) and a tower top high-purity silane extraction pipeline are sequentially arranged from the tower bottom to the tower top.
The device for preparing silane by the disproportionation reaction of the chlorosilane; when the reaction separation tower and the cold separation tower are in a parallel structure, a silicon tetrachloride extraction pipeline at the tower bottom of the reaction separation tower is connected with a tower bottom reboiler (4), and the reaction separation tower is sequentially provided with a stripping section (3), a raw material feed inlet (5), a reaction separation section (1) and a tower top gas product conveying pipeline from the tower bottom to the tower top, wherein the pipeline is connected with the cold separation tower bottom; at least two cold sections (2) are arranged in the cold separation tower, and the cold sections in the cold separation tower are connected with a tower top high-purity silane extraction pipeline; the cold separation tower kettle is provided with a liquid conveying pipeline which is connected with a conveying pump and then connected with the top of the reaction separation tower.
The device for preparing silane by the disproportionation reaction of the chlorosilane; when the reaction separation tower and cold separation tower double-tower parallel structure is adopted, a silicon tetrachloride extraction pipeline at the bottom of the reaction separation tower is connected with a tower kettle reboiler (4), and the reaction separation tower is sequentially provided with a stripping section (3), a raw material feed inlet (5), a reaction separation section (1) and a connection section cold subsection (2) from the bottom of the tower to the top of the tower; the first section of cold section (2) is connected with a gas product conveying pipeline at the top of the tower, and the pipeline is connected with the tower bottom of the cold separation tower; at least one cold section (2) is connected in the cold separation tower, the cold section (2) in the cold separation tower is connected with a high-purity silane extraction pipeline at the top of the tower, a liquid conveying pipeline is arranged at the bottom of the cold separation tower and is connected with a conveying pump, and then the liquid conveying pipeline is connected with the top of the reaction separation tower.
The device for preparing silane by the disproportionation reaction of the chlorosilane; the cold section (2) comprises a mass transfer separation part (2 a) and a heat exchange part (2 b), wherein the mass transfer separation part (2 a) is filled with one or more of structured packing, random packing and separation trays; the heat exchange part (2 b) adopts one or a plurality of combinations of a shell and tube type, a coil type and a U-shaped tube type.
According to the method for preparing the silane by the device for preparing the silane by the chlorosilane disproportionation reaction, the chlorosilane enters a reaction separation tower, flows through a reaction separation section, gas upwards passes through two or more cold sections to separate and purify products, and liquid downwards flows through a stripping section to separate and purify the products; the reaction separation section is filled with a catalyst.
In the method, chlorosilane enters a reaction separation tower, first, disproportionation reaction is fully carried out in the reaction separation section, the pressure in the reaction separation tower is 0.1-1.0 MPa, the reaction temperature is 50-100 ℃, the obtained reaction product gas and liquid are initially separated in the reaction separation section, the product gas contains silane, silicon monochloride, silicon dichloride and low-boiling-point trichlorosilane, and the gas goes upward to be further separated by cold segmentation; the product liquid contains trichlorosilane and silicon tetrachloride, and the liquid flows downwards to flow through the stripping section for separation.
In the method, the cold source introduced into the heat exchange part in the cold section (2) is circulating water, water at 7 ℃, frozen salt, freon and CO 2 One or more of refrigerant, ethylene and liquid nitrogen; the gas product is firstly adsorbed and separated in the cold sectional mass transfer separation process, then fully transfers heat with the cold source at two sides of the heat exchange structure, exchanges heat, further condenses impurities and non-target products into liquid, flows downwards, further adsorbs and separates the liquid through the mass transfer separation part, and the gas continues to upwards; mass transfer separation and heat exchange separation are carried out through multiple times of cold segmentation, the temperature of the top of the reaction separation tower is between 170 ℃ below zero and 10 ℃, and finally high-purity silane is extracted through a high-purity silane extraction pipeline.
In the method, silicon tetrachloride and high-boiling-point trichlorosilane flowing through a stripping section are continuously heated and evaporated through a tower kettle reboiler, are separated in the stripping section, the temperature of the tower kettle of a reaction separation tower is 80-160 ℃, and finally high-purity silicon tetrachloride is extracted from the tower kettle.
The invention relates to a device for preparing silane by a chlorosilane disproportionation reaction, which is characterized by comprising a reaction separation section (1), a cold section (2) and a stripping section (3), a feed inlet (5) and a reboiler (4); the preparation device adopts a single-tower structure of a reaction separation tower or a double-tower parallel structure of the reaction separation tower and a cold separation tower. When the device adopts a single-tower structure, a high-purity silane extraction pipeline is arranged at the top of the reaction separation tower, and a silicon tetrachloride extraction pipeline is arranged at the bottom of the reaction separation tower; the device adopts the cold separation tower top to set up high-purity silane extraction pipeline when two tower parallel structure, and reaction separation tower cauldron sets up silicon tetrachloride extraction pipeline preparation device adopt the single tower structure of reaction separation tower time connected mode, from the cauldron to the top of the tower, cauldron silicon tetrachloride extraction pipeline connection tower cauldron reboiler (4), stripping section (3), raw materials feed inlet (5), reaction separation section (1) connect at least more than two cold segmentation (2), cold segmentation reconnection tower top high-purity silane extraction pipeline, as shown in fig. 1.
When the preparation device adopts a double-tower parallel structure of a reaction separation tower and a cold separation tower, various setting modes exist in each section of working procedure in the tower:
as shown in the figure 2, the reaction separation tower is arranged from a tower kettle to the tower top, a silicon tetrachloride extraction pipeline at the tower kettle is connected with a tower kettle reboiler (4), a stripping section (3) and a raw material feeding port (5), the reaction separation section (1) is connected with a tower top gas product conveying pipeline to a connected cold separation tower kettle, at least more than two cold sections (2) are connected in the cold separation tower, a high-purity silane extraction pipeline at the top of the tower is connected in the cold separation tower in a cold section mode, a liquid conveying pipeline is arranged at the tower kettle of the cold separation tower and is connected with a conveying pump, and the tower top of the reaction separation tower is connected.
As shown in the arrangement of figure 3, the reaction separation tower is from tower kettle to the top of the tower, tower kettle silicon tetrachloride extraction pipeline is connected with a tower kettle reboiler (4), stripping section (3), raw material feed inlet (5), reaction separation section (1) is connected with a section of cold segmentation (2), cold segmentation (2) is connected with a tower top gas product conveying pipeline to the connected cold separation tower kettle, at least more than one cold segmentation (2) is connected in the cold separation tower, the cold segmentation (2) is connected with a tower top high-purity silane extraction pipeline in the cold separation tower, the cold separation tower kettle is provided with a liquid conveying pipeline and is connected with a conveying pump, and the cold separation tower is connected with the top of the reaction separation tower.
The reaction separation section (1) is filled with a catalyst.
The tower comprises at least two cold sections (2) for separating gas products, wherein each cold section (2) comprises a mass transfer separation part (2 a) and a heat exchange part (2 b), the reaction separation section (1) is connected with the mass transfer separation part, and the mass transfer separation part is connected with the heat exchange part. The mass transfer separation section (2 a) in the cold section (2) is filled with one or more combinations of structured packing, random packing, and separation trays. The heat exchange part (2 b) in the cold section (2) adopts one or a plurality of combinations of a shell and tube type, a coil type and a U-shaped tube type.
The method for preparing the silane by the disproportionation reaction of the chlorosilane is characterized in that the method takes the chlorosilane as a reaction raw material and prepares high-purity silane parallel product silicon tetrachloride through a disproportionation reaction device. Chlorosilane enters a reaction separation tower through a feed inlet (5), flows through a reaction separation section, gas upwards passes through two or more cold sections to separate and purify products, and liquid downwards flows through a stripping section to separate and purify products.
The chlorosilane enters a reaction separation tower, first, disproportionation reaction is fully carried out in the reaction separation section, the pressure in the tower is controlled to be 0.1-1.0 MPa, the reaction temperature is 50-100 ℃, the obtained reaction product gas and liquid are subjected to preliminary separation in the reaction separation section, the product gas contains silane, monochloro-hydrosilicon, dichlorosilane and low-boiling-point trichlorosilane, and the gas upwards goes through a cold section for further separation; the product liquid contains trichlorosilane and silicon tetrachloride, and the liquid flows downwards to flow through the stripping section for separation.
The cold source introduced by the heat exchange part in the cold section (2) is circulating water, 7 ℃ water, frozen salt, freon and CO 2 One or more of refrigerant, ethylene and liquid nitrogen. The gas product is firstly subjected to simple adsorption separation in the cold sectional mass transfer separation procedure, and then fully transfers heat with the cold source at the two sides of the heat exchange structure, exchanges heat and entersThe impurities and non-target products are condensed into liquid in one step and flow downwards, the liquid is further adsorbed and separated by the mass transfer separation part, and the gas continues to flow upwards. Mass transfer separation and heat exchange separation are carried out through multiple times of cold segmentation, the temperature of the tower top of all towers is controlled to be between 170 ℃ below zero and 10 ℃, and finally high-purity silane is extracted through a high-purity silane extraction pipeline.
The silicon tetrachloride and the high-boiling-point trichlorosilane flowing through the stripping section are continuously heated and evaporated through a tower kettle reboiler, are separated in the stripping section, the temperature of the tower kettle is controlled to be 80-160 ℃, and finally the high-purity silicon tetrachloride is extracted from the tower kettle.
The invention sends chlorosilane into a reaction separation tower through a raw material feed inlet, and the chlorosilane flows through a reaction section, under the action of a catalyst, the pressure is controlled to be 0.1-1.0 MPa, the reaction temperature is 50-100 ℃, and the chlorosilane undergoes disproportionation reaction: continuously heating the liquid product through a tower kettle reboiler, adsorbing and separating the liquid product through a stripping section, and extracting high-purity silicon tetrachloride from the tower kettle of a reaction separation tower; the gas product flows through a multi-stage cold section, is subjected to repeated condensation, adsorption and separation, and is extracted through a high-purity silane extraction pipeline. The product is continuously extracted from a silane extraction pipeline and a silicon tetrachloride extraction pipeline, so that the disproportionation reaction is promoted to be continuously carried out towards the direction of product generation, the reaction is promoted to be more thorough, and the conversion rate can reach more than 90%.
The invention has the following advantages:
[1] compared with the traditional multi-step disproportionation process, the process equipment is simple, the multi-step disproportionation reaction can be realized by only one reaction separation tower, the reaction and the separation are simultaneously carried out, the unique cold segmentation process is designed, the product separation is carried out in a single tower or multi-tower mode, the high-purity silane is continuously extracted from the silane extraction pipeline, the disproportionation reaction is continuously carried out towards the direction of generating the silane, and the disproportionation reaction is promoted to be more thorough.
[2] The cold segmentation process is fully utilized in the tower, and the cold segmentation process comprises a mass transfer separation part and a heat exchange part, so that products are fully separated, a silane product is in a gas phase state all the time, and the silane product is subjected to impurity removal treatment through a plurality of cold segments, so that the purity of the obtained silane product is higher.
[3] The liquid product separated by the reaction separation section contains trichlorosilane and silicon tetrachloride, the liquid downwards flows through the stripping section, the liquid is continuously heated and evaporated by a tower kettle reboiler, the product is separated, and the silicon tetrachloride is extracted from the tower kettle of the reaction separation tower.
Drawings
FIG. 1 shows a single tower structure of a device for preparing silane by disproportionation reaction of chlorosilane;
FIG. 2 shows a double-tower structure of a device for preparing silane through disproportionation reaction of chlorosilane, namely a structure without cold segmentation in a reaction separation tower;
FIG. 3 shows a double-tower structure of a device for preparing silane through chlorosilane disproportionation reaction, wherein a reaction separation tower comprises a cold sectional structure;
FIG. 4 is a longitudinal section of the reaction separation section (1);
fig. 5 is a schematic diagram of a cold source pipeline structure of a cold sectional heat exchange part, a is a tube array structure, b is a U-shaped tube structure, and c is a coil structure.
Wherein: 1-a reaction separation section; 2-cold section, mass transfer separation part in 2 a-cold section, heat exchange part in 2 b-cold section; 3-stripping section; 4-reboiler; 5-chlorosilane feed inlet.
Detailed Description
The process and apparatus provided by the present invention are further described below with reference to the accompanying drawings.
As shown in figure 1, the device for preparing silane by the chlorosilane disproportionation reaction comprises a chlorosilane preliminary disproportionation reaction separation section (1), a gas product separation and purification cold section (2), a trichlorosilane and silicon tetrachloride separation and purification stripping section (3), a tower kettle reboiler (4) and a feed inlet (5), and the direction from the tower kettle to the tower top is specified to be from bottom to top.
The method for preparing silane by utilizing the device of the invention for carrying out the chlorosilane disproportionation reaction comprises the steps of adding chlorosilane into a reaction separation tower through a feed inlet (5), carrying out disproportionation reaction on the chlorosilane in a reaction separation section (1), carrying out primary separation on the chlorosilane in the reaction separation section, and carrying out cold sectional separation on the gas which contains silane, monochloro-hydrosilicon, dichlorosilane and low-boiling trichlorosilane and going upwards to obtain high-purity silane which is extracted from a silane extraction pipeline; the product liquid contains high-boiling trichlorosilane and silicon tetrachloride, the liquid flows downwards to flow through the stripping section, the liquid is continuously heated and evaporated through a tower kettle reboiler, the product is separated, and the silicon tetrachloride is extracted from the tower kettle.
Specific application examples are as follows:
example 1:
the TCS raw material is pumped into a disproportionation reaction separation tower, and the preparation device adopts a single-tower structure of the reaction separation tower, as shown in figure 1. The TCS feed inlet (5) enters the device and is connected with the reaction separation section (1), the reaction separation section is filled with catalyst, the catalyst is filled in a corrosion-resistant permeable pocket by alkaline anion exchange resin, and the catalyst is coiled with silk screen corrugated filler at intervals to play a role in reaction separation. The operating pressure of the reaction separation tower in the section is controlled at 1MPaG, the temperature of the reaction section is controlled between 105 ℃ and 120 ℃, the temperature of the reaction separation section in the middle part is gradually increased from top to bottom, and the reaction products are separated from liquid and gas in the section as shown in figure 4. The reaction product liquid contains high-boiling trichlorosilane and silicon tetrachloride, flows to a tower kettle, flows through a stripping section, has the theoretical plate number of the stripping section of 50, is continuously heated and evaporated by a tower kettle reboiler, has the temperature of 150-160 ℃, is continuously adsorbed and separated from the silicon tetrachloride, and has the purity of 99.2 percent. The reaction product gas contains silane, silicon monochloride, dichlorosilane and low boiling point trichlorosilane, and flows away to the top of the tower, and flows through two sections of cooling sections, the mass transfer separation part of the first section of cooling sections is filled with structured packing from bottom to top, the heat exchange part of cooling source adopts 7 ℃ water, a cooling source pipeline adopts a coil pipe structure as shown in figure 5c, and the temperature of the section of cooling source pipeline is controlled to be 10 ℃; the second stage cold sectional mass transfer separation part is filled with structured packing, and the heat exchange part cold source adopts CO 2 The cold source, the cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the top of the tower is controlled to be-50 ℃. Under the operating condition, the high-purity silane with the purity of 99.2% is extracted from the high-purity silane extraction pipeline at the top of the reaction separation tower.
Example 2:
the DCS raw material is pumped into a disproportionation reaction separation tower, and the preparation device adopts a single-tower structure of the reaction separation tower, as shown in figure 1. DCS feed inlet (5) gets into the device, connects reaction separation section (1), and reaction section fills the catalyst, fills in corrosion-resistant penetrating pocket by alkaline anion exchange resin, and with silk screen ripple packing interval lapping preparation, plays the effect of reaction separation. The operating pressure of the reaction separation tower in the section is controlled at 0.8MPaG, the temperature of the reaction section is controlled between 65 ℃ and 80 ℃, the temperature of the middle reaction separation section gradually rises from top to bottom, and the reaction products are separated from liquid and gas in the section as shown in figure 4. The reaction product liquid contains high-boiling trichlorosilane and silicon tetrachloride, flows to a tower kettle, flows through a stripping section, has the theoretical plate number of the stripping section of 100, is continuously heated and evaporated by a tower kettle reboiler, has the temperature of about 145-150 ℃, is continuously adsorbed and separated from the silicon tetrachloride, and has the purity of 99.2 percent. The reaction product gas contains silane, silicon monochloride, dichlorosilane and low boiling point trichlorosilane, and flows away to the top of the tower, and flows through two sections of cold sections, wherein the mass transfer separation part of the first section of cold section is filled with random packing from bottom to top, the heat exchange part of the cold source adopts 7 ℃ water, a cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the section of cold source pipeline is controlled to be 10 ℃; the second stage of cold sectional mass transfer separation part is filled with random packing, the heat exchange part is made of Freon, the cold source pipeline adopts a tube structure as shown in figure 5a, and the temperature of the tower top is controlled to be-65 ℃. Under the operating condition, the high-purity silane with the purity of 99.0% is extracted from the high-purity silane extraction pipeline at the top of the reaction separation tower.
Example 3:
the TCS raw material is pumped into a disproportionation reaction separation tower, and the preparation device is arranged in a parallel structure of a reaction separation tower and a cold separation tower, as shown in figure 2. The TCS feed inlet (5) enters the device and is connected with the reaction separation section (1), the reaction section in the reaction separation tower is filled with catalyst, the catalyst is filled in a corrosion-resistant permeable pocket by alkaline anion exchange resin, the catalyst and the silk screen corrugated filler are coiled at intervals to play a role in reaction separation, the operation pressure of the reaction separation tower in the section is controlled at 0.3MPaG, the temperature of the reaction section is controlled between 70 and 80 ℃, the temperature of the middle reaction separation section is gradually increased from top to bottom, and the reaction product is separated from liquid and gas in the section as shown in figure 4. The reaction product liquid contains high-boiling trichlorosilane and silicon tetrachloride, flows to a tower kettle, flows through a stripping section, has the theoretical plate number of the stripping section of 100, is continuously heated and evaporated by a tower kettle reboiler, has the temperature of about 100-110 ℃, is continuously adsorbed and separated from the silicon tetrachloride, and is extracted from a silicon tetrachloride extraction pipeline of the reaction separation tower kettle, wherein the purity of the silicon tetrachloride is 99.0%. The reaction product gas contains silane, silicon monochloride, silicon dichloride and low-boiling-point trichlorosilane and flows away to the top of the reaction separation tower, and flows to a connected cold separation tower kettle through a gas product conveying pipeline at the top of the reaction separation tower, the cold separation tower adopts three sections of cold sections, a mass transfer separation part of the first section of cold sections is filled with a separation tray filler from bottom to top, a heat exchange part of cold source adopts circulating water, a cold source pipeline adopts a coil pipe structure as shown in figure 5c, and the temperature of the section of cold source pipeline is controlled to be 30 ℃; the second section of cold sectional mass transfer separation part is filled with separation tray filler, the heat exchange part adopts frozen brine as a cold source, a cold source pipeline adopts a U-shaped pipe structure as shown in figure 5b, and the temperature of the second section is controlled to be-10 ℃; the third section of cold sectional mass transfer separation part is filled with separation tray filler, the heat exchange part is made of ethylene, the cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the top of the cold separation tower is controlled to be-85 ℃. The liquid separated by the cold separation tower is returned to the reaction separation tower through a liquid conveying pipeline of the tower kettle by a conveying pump. Under the operating condition, the high-purity silane with the purity of 99.8% is extracted from the high-purity silane extraction pipeline at the top of the cold separation tower.
Example 4:
the DCS raw material is pumped into a disproportionation reaction separation tower, and the preparation device is arranged in a parallel structure of a reaction separation tower and a cold separation tower, as shown in figure 2. DCS feed inlet (5) enters the device, connecting reaction separation section (1), filling catalyst in reaction section of reaction separation tower, filling alkaline anion exchange resin in corrosion-resistant transparent pocket, rolling with silk screen ripple filler to obtain reaction separation, controlling operation pressure of reaction separation tower at 0.4MPaG, controlling temperature of reaction section at 60-80deg.C, raising temperature of middle reaction separation section gradually from top to bottom, separating reaction product with liquid and gas in the section as shown in figure 4. The reaction product liquid contains high-boiling trichlorosilane and silicon tetrachloride, flows to a tower kettle, flows through a stripping section, has the theoretical plate number of the stripping section of 100, is continuously heated and evaporated by a tower kettle reboiler, has the temperature of about 110-120 ℃, is continuously adsorbed and separated from the silicon tetrachloride, and the silicon tetrachloride extraction pipeline of the reaction separation tower kettle extracts high-purity silicon tetrachloride with the purity of 99.2 percent. The reaction product gas contains silane, silicon monochloride, silicon dichloride and low-boiling-point trichlorosilane and flows away to the top of the reaction separation tower, and flows to a connected cold separation tower kettle through a gas product conveying pipeline at the top of the reaction separation tower, the cold separation tower adopts three sections of cold sections, the mass transfer separation part of the first section of cold sections is filled with structured packing from bottom to top, the heat exchange part of cold source adopts circulating water, a cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the section of cold source pipeline is controlled to be 30 ℃; the second stage of cold sectional mass transfer separation part is filled with structured packing, the heat exchange part adopts frozen brine as a cold source, a cold source pipeline adopts a coil pipe structure as shown in fig. 5c, and the temperature of the second stage is controlled to be-10 ℃; the third stage of cold sectional mass transfer separation part is filled with structured packing, the heat exchange part is made of ethylene, the cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the top of the cold separation tower is controlled to be-80 ℃. The liquid separated by the cold separation tower is returned to the reaction separation tower through a liquid conveying pipeline of the tower kettle by a conveying pump. Under the operating condition, the high-purity silane with the purity of 99.6% is extracted from the high-purity silane extraction pipeline at the top of the cold separation tower.
Example 5:
the TCS raw material is pumped into a disproportionation reaction separation tower, and the preparation device is arranged in a parallel structure of a reaction separation tower and a cold separation tower, as shown in figure 3. The TCS feed inlet (5) enters the device and is connected with the reaction separation section (1), the reaction section in the reaction separation tower is filled with catalyst, the catalyst is filled in a corrosion-resistant permeable pocket by alkaline anion exchange resin, the catalyst and the silk screen corrugated filler are coiled at intervals to play a role in reaction separation, the operation pressure of the reaction separation tower in the section is controlled at 0.4MPaG, the temperature of the reaction section is controlled between 70 and 90 ℃, the temperature of the middle reaction separation section is gradually increased from top to bottom, and the reaction product is separated from liquid and gas in the section as shown in figure 4. The reaction product liquid contains high-boiling trichlorosilane and silicon tetrachloride, flows to a tower kettle, flows through a stripping section, has theoretical plate number of 40, is continuously heated and evaporated by a tower kettle reboiler, has the temperature of about 110-115 ℃, is continuously adsorbed and separated from the silicon tetrachloride, and the silicon tetrachloride extraction pipeline of the reaction separation tower kettle extracts high-purity silicon tetrachloride with the purity of 99.0%. The reaction product gas contains silane, silicon monochloride, silicon dichloride and low-boiling-point silicon trichloride which flow away to the top of a reaction separation tower, and pass through a cooling section of the reaction separation tower, a mass transfer separation part of the cooling section is filled with random packing, a heat exchange part cold source is water with the temperature of 7 ℃, a cold source pipeline adopts a U-shaped pipe structure as shown in figure 5b, and the temperature of the section is controlled to be 10 ℃; the cold section of the reaction separation tower is connected with a tower top gas product conveying pipeline to a tower bottom of the connected cold separation tower, the cold separation tower adopts a section of cold section, a mass transfer separation part of the cold section is filled with random packing, a heat exchange part of the cold source adopts ethylene, a cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the tower top of the cold separation tower is controlled to be-80 ℃. The liquid separated by the cold separation tower is returned to the reaction separation tower through a liquid conveying pipeline of the tower kettle by a conveying pump. Under the operating condition, the high-purity silane with the purity of 99.2% is extracted from the high-purity silane extraction pipeline at the top of the cold separation tower.
Example 6:
the DCS raw material is pumped into a disproportionation reaction separation tower, and the preparation device is arranged in a parallel structure of a reaction separation tower and a cold separation tower, as shown in figure 3. DCS feed inlet (5) enters the device, connecting reaction separation section (1), filling catalyst in reaction section of reaction separation tower, filling alkaline anion exchange resin in corrosion-resistant transparent pocket, rolling with silk screen ripple filler to obtain reaction separation, controlling operation pressure of reaction separation tower at 0.4MPaG, controlling temperature of reaction section at 75-90 deg.C, raising temperature of middle reaction separation section gradually from top to bottom, separating reaction product with liquid and gas in the section as shown in figure 4. The reaction product liquid contains high-boiling trichlorosilane and silicon tetrachloride, flows to a tower kettle, flows through a stripping section, has a theoretical plate number of 30, is continuously heated and evaporated by a tower kettle reboiler, has the temperature of about 110-120 ℃, is continuously adsorbed and separated from the silicon tetrachloride, and the silicon tetrachloride extraction pipeline of the reaction separation tower kettle extracts high-purity silicon tetrachloride with the purity of 99.0%. The reaction product gas contains silane, monochloro-silicon, dichloro-silicon and low boiling point trichlorosilane, and flows away to the top of the reaction separation tower, and passes through the cooling section of the reaction separation tower, the mass transfer separation part of the cooling section is filled with structured packing, the heat exchange part of the cooling source adopts 7 ℃ water, the pipeline of the cooling source adopts a tube array structure as shown in figure 5a, and the temperature of the section is controlled to be 10 ℃; the cold section of the reaction separation tower is connected with a tower top gas product conveying pipeline to a connected cold separation tower kettle, the cold separation tower adopts a section of cold section, a mass transfer separation part of the cold section is filled with structured packing, a heat exchange part of the cold source adopts ethylene, a cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the tower top of the cold separation tower is controlled to be-80 ℃. The liquid separated by the cold separation tower is returned to the reaction separation tower through a liquid conveying pipeline of the tower kettle by a conveying pump. Under the operating condition, the high-purity silane with the purity of 99.0% is extracted from the high-purity silane extraction pipeline at the top of the cold separation tower.
Example 7:
the TCS raw material is pumped into a disproportionation reaction separation tower, and the preparation device is arranged in a parallel structure of a reaction separation tower and a cold separation tower, as shown in figure 3. The TCS feed inlet (5) enters the device and is connected with the reaction separation section (1), the reaction section in the reaction separation tower is filled with catalyst, the catalyst is filled in a corrosion-resistant permeable pocket by alkaline anion exchange resin, the catalyst and the silk screen corrugated filler are coiled at intervals to play a role in reaction separation, the operation pressure of the reaction separation tower at the section adopts 0.1MPaG, the temperature of the reaction section is controlled between 40 and 60 ℃, the temperature of the middle reaction separation section is gradually increased from top to bottom, and the reaction product is separated from the liquid and the gas at the section, as shown in figure 4. The reaction product liquid contains high-boiling trichlorosilane and silicon tetrachloride, flows to a tower kettle, flows through a stripping section, has the theoretical plate number of the stripping section of 100, is continuously heated and evaporated by a tower kettle reboiler, has the temperature of about 70-80 ℃, is continuously adsorbed and separated from the silicon tetrachloride, and has the purity of 99.3 percent. The reaction product gas contains silane, monochloro-silicon, dichloro-silicon and low boiling point trichlorosilane, and flows away to the top of the reaction separation tower, and passes through the cooling section of the reaction separation tower, the mass transfer separation part of the cooling section is filled with random packing, the heat exchange part of the cooling source adopts 7 ℃ water, the pipeline of the cooling source adopts a coil pipe structure as shown in figure 5c, and the temperature of the section is controlled to be 10 ℃; the reaction separation tower is internally cooled and sectionally connected with a tower top gas product conveying pipeline to a connected cold separation tower kettle, and the cold separation tower adopts two sections of coldSectioning, namely filling random packing into a mass transfer separation part of a first section of cold sectioning from bottom to top, and selecting CO as a heat exchange part cold source 2 The cold source, the cold source pipeline adopts a coil pipe structure as shown in figure 5c, and the temperature of the section is controlled to be-40 ℃; the second stage of cold sectional mass transfer separation part is filled with random packing, the heat exchange part adopts liquid nitrogen as a cold source, a cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the top of the cold separation tower is controlled to be-160 ℃. The liquid separated by the cold separation tower is returned to the reaction separation tower through a liquid conveying pipeline of the tower kettle by a conveying pump. Under the operating condition, the high-purity silane with the purity of 99.5% is extracted from the high-purity silane extraction pipeline at the top of the cold separation tower.
Example 8:
the DCS raw material is pumped into a disproportionation reaction separation tower, and the preparation device adopts a double-tower parallel structure of the reaction separation tower and the cold separation tower, and the arrangement is shown in figure 3. DCS feed inlet (5) enters the device, connecting reaction separation section (1), filling catalyst in reaction section of reaction separation tower, filling alkaline anion exchange resin in corrosion-resistant transparent pocket, rolling with silk screen ripple filler to obtain reaction separation, adopting 0.1MPaG for operation pressure of reaction separation tower, controlling reaction section temperature between 40-60 deg.C, raising middle reaction separation section temperature from top to bottom, separating reaction product with liquid and gas in the section as shown in figure 4. The reaction product liquid contains high-boiling trichlorosilane and silicon tetrachloride, flows to a tower kettle, flows through a stripping section, has the theoretical plate number of the stripping section of 100, is continuously heated and evaporated by a tower kettle reboiler, has the temperature of about 70-80 ℃, is continuously adsorbed and separated from the silicon tetrachloride, and the silicon tetrachloride extraction pipeline of the reaction separation tower kettle extracts high-purity silicon tetrachloride with the purity of 99.0%. The reaction product gas contains silane, monochloro-silicon, dichloro-silicon and low boiling point trichlorosilane, and flows away to the top of the reaction separation tower, and is cooled and segmented through the reaction separation tower, the cold segmented mass transfer separation part is filled with random packing, the heat exchange part is a heat exchange part with 7 ℃ water, a cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the segment is controlled to be 10 ℃; the reaction separation tower is internally cooled and sectionally connected with a tower top gas product conveying pipeline to a connected cold separation tower kettle, the cold separation tower adopts two sections of cold sections, and the first section of cold section is transmitted from bottom to topThe mass separation part is filled with random packing, and the heat exchange part cold source adopts CO 2 The cold source, the cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the section is controlled to be-40 ℃; the second stage of cold sectional mass transfer separation part is filled with random packing, the heat exchange part adopts liquid nitrogen as a cold source, a cold source pipeline adopts a tube array structure as shown in figure 5a, and the temperature of the top of the cold separation tower is controlled to be-160 ℃. The liquid separated by the cold separation tower is returned to the reaction separation tower through a liquid conveying pipeline of the tower kettle by a conveying pump. Under the operating condition, the high-purity silane with the purity of 99.6% is extracted from the high-purity silane extraction pipeline at the top of the cold separation tower.
The invention provides a device and a method for preparing silane through chlorosilane disproportionation reaction, and the device and the method have been described through examples. The technical scheme disclosed and proposed by the invention can be realized by a relevant technical person through the links of properly changing the condition route and the like by referring to the content of the text, although the method and the preparation technology of the invention have been described by the preferred embodiment examples, the relevant technical person can obviously change or recombine the method and the technical route described herein to realize the final preparation technology without departing from the content, the spirit and the scope of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be included within the spirit, scope and content of the invention.
Claims (9)
1. A device for preparing silane by disproportionation reaction of chlorosilane; the preparation device is characterized by comprising a reaction separation section (1), a cold section (2) and a stripping section (3), a feed inlet (5) and a reboiler (4); the preparation device adopts a single-tower structure of a reaction separation tower or a double-tower parallel structure of the reaction separation tower and a cold separation tower; when the device adopts a single-tower structure, a high-purity silane extraction pipeline is arranged at the top of the reaction separation tower, and a silicon tetrachloride extraction pipeline is arranged at the bottom of the reaction separation tower; the device adopts a double-tower parallel structure, a high-purity silane extraction pipeline is arranged at the top of a cold separation tower, and a silicon tetrachloride extraction pipeline is arranged at the bottom of a reaction separation tower.
2. The apparatus for preparing silane by disproportionation reaction of chlorosilane as in claim 1; the method is characterized in that when a single-tower structure of the reaction separation tower is adopted, a silicon tetrachloride extraction pipeline of the tower kettle is connected with a tower kettle reboiler (4); the stripping section (3), the raw material feed inlet (5), the reaction separation section (1), at least more than two cold sections (2) and a tower top high-purity silane extraction pipeline are sequentially arranged from the tower bottom to the tower top.
3. The apparatus for preparing silane by disproportionation reaction of chlorosilane as in claim 1; the method is characterized in that when the reaction separation tower and the cold separation tower are in a double-tower parallel structure, a silicon tetrachloride extraction pipeline at the bottom of the reaction separation tower is connected with a tower kettle reboiler (4), and the reaction separation tower is sequentially provided with a stripping section (3), a raw material feed inlet (5), a reaction separation section (1) and a tower top gas product conveying pipeline from the tower kettle to the tower top, wherein the pipelines are connected to the bottom of the cold separation tower; at least two cold sections (2) are arranged in the cold separation tower, and the cold sections in the cold separation tower are connected with a tower top high-purity silane extraction pipeline; the cold separation tower kettle is provided with a liquid conveying pipeline which is connected with a conveying pump and then connected with the top of the reaction separation tower.
4. The apparatus for preparing silane by disproportionation reaction of chlorosilane as in claim 1; the method is characterized in that when the reaction separation tower and the cold separation tower are in a double-tower parallel structure, a silicon tetrachloride extraction pipeline at the bottom of the reaction separation tower is connected with a tower kettle reboiler (4), and the reaction separation tower is sequentially provided with a stripping section (3), a raw material feed inlet (5), a reaction separation section (1) and a connection section cold subsection (2) from the bottom of the tower to the top of the tower; the first section of cold section (2) is connected with a gas product conveying pipeline at the top of the tower, and the pipeline is connected with the tower bottom of the cold separation tower; at least one cold section (2) is connected in the cold separation tower, the cold section (2) in the cold separation tower is connected with a high-purity silane extraction pipeline at the top of the tower, a liquid conveying pipeline is arranged at the bottom of the cold separation tower and is connected with a conveying pump, and then the liquid conveying pipeline is connected with the top of the reaction separation tower.
5. The apparatus for preparing silane by disproportionation reaction of chlorosilane as in claim 1; the cold section (2) comprises a mass transfer separation part (2 a) and a heat exchange part (2 b), wherein the mass transfer separation part (2 a) is filled with one or more of structured packing, random packing and separation trays; the heat exchange part (2 b) adopts one or a plurality of combinations of a shell and tube type, a coil type and a U-shaped tube type.
6. The method for preparing the silane by the device for preparing the silane by the disproportionation reaction of the chlorosilane, which is characterized in that the chlorosilane enters a reaction separation tower, flows through a reaction separation section, gas upwards passes through two or more cold sections for product separation and purification, and liquid downwards flows through a stripping section for product separation and purification; the reaction separation section is filled with a catalyst.
7. The method of claim 6, wherein chlorosilane enters a reaction separation tower, first, disproportionation reaction is fully carried out in the reaction separation section, the pressure in the reaction separation tower is 0.1-1.0 MPa, the reaction temperature is 50-100 ℃, the obtained reaction product gas and liquid are initially separated in the reaction separation section, the product gas contains silane, monochloro-silicon, dichlorosilane and low-boiling-point trichlorosilane, and the gas goes upward to be further separated by cold segmentation; the product liquid contains trichlorosilane and silicon tetrachloride, and the liquid flows downwards to flow through the stripping section for separation.
8. The method as set forth in claim 6, wherein the cold source introduced into the heat exchange part of the cold stage (2) is circulating water, 7 ℃ water, frozen salt, freon, CO 2 One or more of refrigerant, ethylene and liquid nitrogen; the gas product is firstly adsorbed and separated in the cold sectional mass transfer separation process, then fully transfers heat with the cold source at two sides of the heat exchange structure, exchanges heat, further condenses impurities and non-target products into liquid, flows downwards, further adsorbs and separates the liquid through the mass transfer separation part, and the gas continues to upwards; mass transfer separation and heat exchange separation are carried out through multiple times of cold segmentation, the temperature of the top of the reaction separation tower is between 170 ℃ below zero and 10 ℃, and finally high-purity silane is extracted through a high-purity silane extraction pipeline.
9. The method according to claim 6, wherein the silicon tetrachloride and the high-boiling trichlorosilane flowing through the stripping section are continuously heated and evaporated by a tower kettle reboiler and separated in the stripping section, the temperature of the tower kettle of the reaction separation tower is 80-160 ℃, and finally the high-purity silicon tetrachloride is extracted from the tower kettle.
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