CN114735709A - Device and method for producing electronic grade trichlorosilane by combination of rectification, adsorption and membrane separation - Google Patents
Device and method for producing electronic grade trichlorosilane by combination of rectification, adsorption and membrane separation Download PDFInfo
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- CN114735709A CN114735709A CN202210670467.1A CN202210670467A CN114735709A CN 114735709 A CN114735709 A CN 114735709A CN 202210670467 A CN202210670467 A CN 202210670467A CN 114735709 A CN114735709 A CN 114735709A
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- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
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- C01B33/10784—Purification by adsorption
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a device for producing electronic grade trichlorosilane by rectification, adsorption and membrane separation in a combined manner, which comprises an adsorption tower, a first light component removal tower, a first heavy component removal tower, a second light component removal tower, a motorized tower, a second heavy component removal tower and a membrane separation device which are sequentially connected through pipelines. The invention provides a process for producing electronic grade trichlorosilane by a rectification-adsorption-membrane separation combined technology, which realizes that the purity of a product reaches the standard for manufacturing electronic components and meets the high-end requirement of the market of the semiconductor industry; compared with the existing process, the preparation process has the advantages of simple operation, little pollution, high safety factor, great industrial popularization value and market application prospect; the invention adopts trichlorosilane with different sources as raw materials, removes light and heavy components and other trace impurities, and produces the product with high purity and good quality.
Description
Technical Field
The invention belongs to the technical field of electronic chemicals, and particularly relates to a device and a method for producing electronic-grade trichlorosilane by combining rectification, adsorption and membrane separation.
Background
The electronic grade trichlorosilane is an important electronic special gas raw material which is indispensable in the semiconductor industry, and has wide application in the field of silicon epitaxial wafer manufacturing. With the rapid development of the integrated circuit industry in China, the demand for electronic grade trichlorosilane is increasing day by day. However, the key domestic raw materials mainly depend on import, the production and manufacture of the key raw materials have very high technical requirements, only a few countries such as the United states, Japan, Germany and the like in the world can produce the electronic grade trichlorosilane meeting the chip manufacturing requirements in a large scale currently, and the largest producers are Wacher company and Japanese shinning company in Germany. At present, under the background of 'double carbon', the demand of polysilicon manufacturers is vigorous due to the high-speed development of the downstream photovoltaic industry. The yield of the polysilicon in China is 4.20 ten thousand tons in 7 months in 2021, the yield is increased by 47.4 percent on a year-by-year basis, the development speed of the polysilicon industry is increased continuously, and the price of the upstream trichlorosilane is increased violently. The price of trichlorosilane greatly rises in the recent years from less than 6000 yuan/ton to about 15000 yuan/ton and 17000 yuan/ton which are the current market prices, so that the localization of the electronic grade trichlorosilane special gas is realized, and the method has great significance for the development of the integrated circuit industry in China.
The Chinese patent 'a method for simultaneously producing electronic-grade dichlorosilane, electronic-grade trichlorosilane and electronic-grade silicon tetrachloride' describes a method for obtaining a product by using crude trichlorosilane as a raw material and adopting the steps of primary dust removal, gas phase adsorption, primary rectification, disproportionation, complexing agent addition, secondary dust removal, primary separation, secondary rectification, tertiary rectification, quartic rectification and the like. The method is stable in operation and high in product purity, but the production route is complex, the equipment load is large, the method is obtained by adjusting and improving the existing electronic-grade dichlorosilane production line, and the independent production of the electronic-grade trichlorosilane cannot be realized. The prior art has high process cost, large energy consumption and long route.
Therefore, how to develop a device and a method for producing electronic grade trichlorosilane by rectification, adsorption and membrane separation in a combined manner, which have the advantages of low energy consumption, short route, high product purity and good quality, is a technical problem to be solved by technical personnel in the field.
Disclosure of Invention
In view of the above, the invention provides a device and a method for producing electronic-grade trichlorosilane by rectification, adsorption and membrane separation in a combined manner, which are low in energy consumption, short in route, high in product purity and good in quality.
In order to achieve the purpose, the invention adopts the following technical scheme:
a device for producing electronic grade trichlorosilane jointly through rectification, adsorption and membrane separation comprises an adsorption tower, a first light component removing tower, a first heavy component removing tower, a second light component removing tower, a motorized tower, a second heavy component removing tower and a membrane separation device which are connected in sequence through pipelines.
Further, a discharge hole at the top of the adsorption tower is connected with a feed hole of the first light component removal tower;
the discharge port of the tower kettle of the first light component removal tower is connected with the feed port of the first heavy component removal tower;
a discharge hole at the top of the first heavy component removal tower is connected with a feed hole of the second light component removal tower;
the discharge port of the tower kettle of the second lightness-removing tower is connected with the feed port of the maneuvering tower;
the discharge hole of the tower kettle of the motorized tower is connected with the feed inlet of the second de-heavy tower;
and a discharge port at the top of the second de-heavy tower is connected with a feed port of the membrane separation device.
Further, the device for producing the electronic grade trichlorosilane jointly by rectification, adsorption and membrane separation also comprises a condenser I to a condenser VI, a reboiler I to a reboiler V and a heat pump compressor;
a discharge hole at the top of the adsorption tower, a first condenser and a feed inlet of the first lightness-removing tower are sequentially connected through pipelines;
the outlet at the top of the first lightness-removing tower, the second condenser and the reflux inlet at the top of the first lightness-removing tower are connected in sequence through pipelines;
a tower kettle discharge port of the first light component removal tower, a first reboiler and a feed port of the first heavy component removal tower are sequentially connected through a pipeline;
a first discharge hole at the top of the first heavy component removal tower, a third condenser and a feed hole of the second light component removal tower are sequentially connected through pipelines;
the other discharge port at the top of the first heavy component removal tower and the first reboiler are sequentially connected with the feed port of the first heavy component removal tower through pipelines;
the tower kettle of the first heavy component removal tower is connected with a reboiler through a pipeline;
the tower top outlet of the second light component removal tower, the heat pump compressor, the reboiler III and the condenser IV are sequentially connected with the tower top reflux inlet of the second light component removal tower through pipelines;
a tower kettle discharge port and a reboiler III of the second light component removal tower are sequentially connected with a feed port of the maneuvering tower through pipelines;
the tower top outlet of the motorized tower, the condenser V and the tower top reflux inlet of the motorized tower are sequentially connected through pipelines;
a tower kettle discharge port of the motorized tower and a reboiler IV are sequentially connected with a feed port of the second heavy component removal tower through pipelines;
a discharge port at the top of the second de-heavy tower and a condenser six are sequentially connected with the membrane separation device through pipelines;
and the tower kettle of the second heavy component removal tower is connected with the reboiler V through a pipeline.
The invention also provides a method for producing electronic grade trichlorosilane by the rectification, adsorption and membrane separation combined method of the device, which comprises the following steps:
(1) conveying the byproduct trichlorosilane into an adsorption tower for adsorption separation to remove trace impurities of boron and phosphorus, carbon-hydrogen bonds and hydrogen-oxygen bonds;
(2) conveying the trichlorosilane after the impurities are removed by adsorption into a first lightness-removing tower to remove light impurities such as boron trichloride, hydrogen chloride and hydrogen, and obtaining kettle liquid such as trichlorosilane, silicon tetrachloride and high-boiling-point substances;
(3) feeding the obtained kettle liquid into a first de-heavy tower for separation, and removing high-boiling-point substance impurities containing silicon tetrachloride and phosphorus chloride liquid to obtain an enriched trichlorosilane product;
(4) sending the produced liquid of the first heavy component removal tower into a second light component removal tower to further remove light component impurities;
(5) sending the produced liquid of the second light component removal tower into a motorized tower to randomly remove light and heavy component impurities;
(6) sending the produced liquid of the mobile tower into a second heavy component removal tower for separation, further removing heavy component impurities, and obtaining a trichlorosilane product after secondary enrichment;
(7) and (4) sending the produced liquid of the second de-heavy tower into a membrane separation device, and removing trace solid particles and other metal ion impurities to obtain an electronic grade trichlorosilane product.
Furthermore, the first light component removing tower, the first heavy component removing tower, the second light component removing tower, the maneuvering tower and the second heavy component removing tower are all provided with sampling ports.
Further, in the step (1), the adsorption medium in the adsorption tower is activated alumina, silica gel or activated carbon.
Further, the adsorption and separation process in the step (1) is a process of performing adsorption and desorption by using two adsorption tower streams, and nitrogen is blown into the adsorption towers to desorb impurities after adsorption is completed.
The technical effect of adopting the further technical scheme is as follows: since SiHCl3The optical fiber is not symmetrical molecules, trace impurities such as boron, phosphorus, carbon-hydrogen bonds and hydrogen-oxygen bonds have high absorption intensity to light, the optical fiber loss can be increased, and the impurities are easy to generate association reaction in the rectification process, so that the impurities are removed as far as possible, and nitrogen or other gases used for desorption can be recycled.
Further, the first light component removal tower, the first heavy component removal tower, the second light component removal tower, the motorized tower and the second heavy component removal tower adopt a plate tower, a packed tower or a plate-packed composite tower.
The technical effect of adopting the further technical scheme is as follows: the rectifying tower adopts a plate tower, a packed tower or a plate-packed composite tower, the equipment technology is mature and reliable, the operation is stable, and continuous production can be realized.
Further, the processes of the steps (2) to (6) adopt a multi-effect rectification mode and a heat pump rectification mode.
The technical effect of adopting the further technical scheme is as follows: the rectification process adopts a multi-effect rectification mode, a certain tower is pressurized, and tower top steam is used as a heating medium of a reboiler of another atmospheric tower in the process, so that an additional heat source is not required to be introduced; meanwhile, a heat pump rectification mode is adopted, so that the steam at the top of a certain tower is heated and pressurized by a compressor and is used as a heating medium of a reboiler of the tower, the latent heat of condensation of the steam at the top of the tower is effectively recovered, the consumption of public works is reduced, and energy conservation and consumption reduction are realized.
Further, the membrane separation device in the step (7) adopts a nanofiltration, microfiltration, ultrafiltration or pervaporation membrane separation mode.
The invention has the beneficial effects that: 1. the invention provides a process for producing electronic grade trichlorosilane by a rectification-adsorption-membrane separation combined technology, which realizes that the purity of a product reaches the standard for manufacturing electronic components and meets the high-end requirement of the market of the semiconductor industry;
2. compared with the existing process, the preparation process has the advantages of simple operation, little pollution, high safety coefficient, great industrial popularization value and market application prospect;
3. the invention adopts trichlorosilane with different sources as raw materials, removes light and heavy components and other trace impurities, and produces products with high purity and good quality.
Drawings
FIG. 1 is a diagram of a device for producing electronic grade trichlorosilane by combining rectification, adsorption and membrane separation.
Wherein: 1-an adsorption column; 2-a first condenser; 3-a first lightness-removing tower; 4-a second condenser; 5-a reboiler I; 6-a first de-weighting tower; 7-condenser III; 8-reboiler II; 9-a second lightness-removing tower; 10-a heat pump compressor; 11-reboiler III; 12-condenser four; 13-a motorized tower; 14-condenser five; 15-reboiler four; 16-a second de-weighting column; 17-condenser six; 18-reboiler five; 19-membrane separation unit.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the device for producing electronic grade trichlorosilane by rectification, adsorption and membrane separation jointly comprises an adsorption tower 1, a first light component removal tower 3, a first heavy component removal tower 6, a second light component removal tower 9, a mobile tower 13, a second heavy component removal tower 16 and a membrane separation device 19 which are connected in sequence through pipelines.
In one embodiment, the top discharge port of the adsorption tower 1 is connected with the feed port of the first lightness-removing tower 3;
a discharge port of a tower kettle of the first light component removal tower 3 is connected with a feed port of the first heavy component removal tower 6;
a discharge port at the top of the first heavy component removal tower 6 is connected with a feed port of a second light component removal tower 9;
a tower kettle discharge port of the second lightness-removing tower 9 is connected with a feed port of the maneuvering tower 13;
a discharge port of a tower kettle of the motorized tower 13 is connected with a feed port of a second de-weighting tower 16;
the outlet of the second heavy component removing tower 16 is connected with the inlet of the membrane separation device 19.
In one embodiment, further comprising condenser one 2 to condenser six 17, reboiler one 5 to reboiler five 18, and heat pump compressor 10;
a discharge hole at the top of the adsorption tower 1, a first condenser 2 and a feed inlet of a first lightness-removing tower 3 are sequentially connected through pipelines;
the outlet at the top of the first lightness-removing column 3, the second condenser 4 and the reflux inlet at the top of the first lightness-removing column 3 are connected in turn through pipelines;
a tower kettle discharge port of the first light component removal tower 3, a first reboiler 5 and a feed port of the first heavy component removal tower 6 are sequentially connected through pipelines;
a first discharge hole at the top of the first heavy component removal tower 6, a third condenser 7 and a second light component removal tower 9 are sequentially connected through pipelines;
the other discharge port at the top of the first heavy component removal tower 6, the first reboiler 5 and the feed port of the first heavy component removal tower 6 are sequentially connected through a pipeline;
the tower kettle of the first heavy component removal tower 6 is connected with a reboiler II 8 through a pipeline;
the top outlet of the second lightness-removing tower 9, the heat pump compressor 10, the reboiler III 11, the condenser IV 12 and the top reflux inlet of the second lightness-removing tower 9 are connected in sequence through pipelines;
a tower kettle discharge port of the second lightness-removing tower 9, a reboiler III 11 and a feed port of a maneuvering tower 13 are sequentially connected through pipelines;
the tower top outlet of the mobile tower 13, the condenser five 14 and the tower top reflux inlet of the mobile tower 13 are sequentially connected through pipelines;
a tower kettle discharge port of the motorized tower 13, a reboiler IV 15 and a feed port of the second de-heavy tower 16 are sequentially connected through pipelines;
a discharge port at the top of the second de-weighting tower 16, a condenser VI 17 and a membrane separation device 19 are connected in sequence through pipelines;
the bottom of the second de-heavy column 16 is connected with a reboiler five 18 through a pipeline.
Example 1
The method for producing the electronic grade trichlorosilane by combining rectification, adsorption and membrane separation comprises the following steps:
(1) the byproduct trichlorosilane in the production of polysilicon is sent into an adsorption tower 1 for adsorption separation to remove trace impurities such as boron, phosphorus, carbon hydrogen bond and hydrogen-oxygen bond, because the absorption intensity of the trichlorosilane to light is high, the loss of optical fiber can be increased, and the impurities are easy to generate association reaction in the rectification process, so the trichlorosilane is firstly removed as much as possible by using an adsorption device, and the SiHCl is removed as the SiHCl3The adsorption tower 1 adopts two tower streams to complete the adsorption and desorption processes, nitrogen is blown into the adsorption tower 1 to desorb impurities after the adsorption is completed, wherein the nitrogen can be recycled, and the adsorption time is controlled;
(2) conveying the trichlorosilane after the impurities are removed by adsorption into a first lightness-removing tower 3 to remove light impurities such as boron trichloride, hydrogen chloride and hydrogen, wherein the first lightness-removing tower 3 adopts a packed tower, and equipment materials adopt 316L ultra-clean electropolishing materials to ensure the high purity of products, so as to obtain kettle liquid such as trichlorosilane, silicon tetrachloride and high-boiling-point substances;
(3) feeding the obtained kettle liquid into a first de-weighting tower 6 for separation, wherein the first de-weighting tower 6 adopts a plate-filled composite tower, 40 layers of tower plates are arranged at the top of the tower, fillers are arranged at the lower section of the tower, electronic-grade trichlorosilane is obtained through the tower plates, impurities in the fillers are prevented from polluting products, 316L ultra-clean electropolishing materials are adopted as equipment materials to ensure the high purity of the products, a multi-effect rectification mode is adopted between the two towers in the process, steam at the top of the first de-weighting tower 6 is used as a first light-component removal tower 3, a heat source of a reboiler at the tower bottom is used for reducing public works to remove high-boiling-point impurities containing silicon tetrachloride and phosphorus chloride liquid, and the enriched trichlorosilane product is obtained;
(4) sending the produced liquid of the first heavy component removal tower 6 into a second light component removal tower 9 to further remove light component impurities;
(5) sending the produced liquid of the second light component removal tower 9 into a motorized tower 13 to randomly remove light and heavy component impurities;
(6) the produced liquid of the mobile tower 13 is sent to a second heavy component removal tower 16 for separation, the second heavy component removal tower 16 adopts a plate-packed composite tower, the upper section is provided with 40 layers of tower plates, the lower section is provided with filler for further removing heavy component impurities to obtain a re-enriched trichlorosilane product, and the first light component removal tower 3, the first heavy component removal tower 6, the second light component removal tower 9, the mobile tower 13 and the second heavy component removal tower 16 are respectively provided with a sampling port from which the analysis product can be obtained to form;
(7) and (3) sending the produced liquid of the second de-weighting tower 16 into a membrane separation device 19, removing trace solid particles and other metal ion impurities to obtain an electronic grade trichlorosilane product, wherein the purity reaches 99.9999999%, the electronic grade trichlorosilane product can be used for manufacturing electronic components, the scale of the product is 200 tons/year, and the production time is 330 days.
The membrane separation device adopts nanofiltration.
The description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A device for producing electronic grade trichlorosilane jointly through rectification, adsorption and membrane separation is characterized by comprising an adsorption tower, a first light component removing tower, a first heavy component removing tower, a second light component removing tower, a motorized tower, a second heavy component removing tower and a membrane separation device which are connected in sequence through pipelines.
2. The device for producing the electronic-grade trichlorosilane jointly by rectification, adsorption and membrane separation according to claim 1 is characterized in that a discharge port at the top of the adsorption tower is connected with a feed port of the first lightness-removing tower;
a discharge port of a tower kettle of the first light component removal tower is connected with a feed port of the first heavy component removal tower;
a discharge hole at the top of the first heavy component removal tower is connected with a feed hole of the second light component removal tower;
a tower kettle discharge port of the second light component removal tower is connected with a feed port of the mobile tower;
a tower kettle discharge port of the motorized tower is connected with a feed port of the second de-weighting tower;
and a discharge port at the top of the second de-weighting tower is connected with a feed port of the membrane separation device.
3. The device for producing the electronic-grade trichlorosilane by combining rectification, adsorption and membrane separation according to claim 1, further comprising a condenser I to a condenser VI, a reboiler I to a reboiler V and a heat pump compressor;
a discharge hole at the top of the adsorption tower, a first condenser and a feed inlet of the first lightness-removing tower are sequentially connected through pipelines;
the outlet at the top of the first lightness-removing tower, the second condenser and the reflux inlet at the top of the first lightness-removing tower are connected in sequence through pipelines;
a tower kettle discharge port of the first light component removal tower, a first reboiler and a feed port of the first heavy component removal tower are sequentially connected through a pipeline;
a first discharge hole at the top of the first heavy component removal tower, a third condenser and a feed hole of the second light component removal tower are sequentially connected through pipelines;
the other discharge port at the top of the first heavy component removal tower, the first reboiler and the feed port of the first heavy component removal tower are sequentially connected through a pipeline;
the tower kettle of the first de-heavy tower is connected with a reboiler through a pipeline;
the tower top outlet of the second light component removal tower, the heat pump compressor, the reboiler III and the condenser IV are sequentially connected with the tower top reflux inlet of the second light component removal tower through pipelines;
a tower kettle discharge hole and a reboiler III of the second light component removal tower are sequentially connected with a feed inlet of the maneuvering tower through pipelines;
the tower top outlet of the motorized tower, the condenser V and the tower top reflux inlet of the motorized tower are sequentially connected through pipelines;
a tower kettle discharge hole and a reboiler IV of the motorized tower are sequentially connected with a feed hole of the second de-heavy tower through pipelines;
a discharge port at the top of the second de-heavy tower, a condenser VI and the membrane separation device are sequentially connected through pipelines;
and the tower kettle of the second heavy component removal tower is connected with the reboiler V through a pipeline.
4. A method for producing electronic grade trichlorosilane by performing rectification, adsorption and membrane separation jointly according to the device of any one of claims 1 to 3, is characterized by comprising the following steps:
(1) conveying the byproduct trichlorosilane into an adsorption tower for adsorption separation to remove trace impurities of boron and phosphorus, carbon-hydrogen bonds and hydrogen-oxygen bonds;
(2) conveying the trichlorosilane after the impurities are removed by adsorption into a first lightness-removing tower to remove light impurities such as boron trichloride, hydrogen chloride and hydrogen, and obtaining kettle liquid such as trichlorosilane, silicon tetrachloride and high-boiling-point substances;
(3) feeding the obtained kettle liquid into a first de-heavy tower for separation, and removing high-boiling-point substance impurities containing silicon tetrachloride and phosphorus chloride liquid to obtain an enriched trichlorosilane product;
(4) sending the produced liquid of the first heavy component removal tower into a second light component removal tower to further remove light component impurities;
(5) sending the produced liquid of the second light component removal tower into a motorized tower to randomly remove light and heavy component impurities;
(6) sending the produced liquid of the mobile tower into a second heavy component removal tower for separation, further removing heavy component impurities, and obtaining a trichlorosilane product after secondary enrichment;
(7) and (4) sending the produced liquid of the second de-heavy tower into a membrane separation device, and removing trace solid particles and other metal ion impurities to obtain an electronic grade trichlorosilane product.
5. The method for producing electronic-grade trichlorosilane through rectification, adsorption and membrane separation in a combined mode according to claim 4, wherein the first light component removal tower, the first heavy component removal tower, the second light component removal tower, the motorized tower and the second heavy component removal tower are provided with sampling ports.
6. The method for producing electronic-grade trichlorosilane through rectification, adsorption and membrane separation in a combined manner according to claim 4, wherein the adsorption medium in the adsorption tower in the step (1) is activated alumina, silica gel or activated carbon.
7. The method for producing electronic grade trichlorosilane by combining rectification, adsorption and membrane separation according to claim 4, wherein the adsorption separation process in the step (1) is a process of alternately completing adsorption and desorption by adopting two adsorption towers, and nitrogen is blown into the adsorption towers after adsorption is completed to desorb impurities.
8. The method for producing the electronic-grade trichlorosilane through the combination of rectification, adsorption and membrane separation according to claim 4, wherein the first lightness-removing tower, the first heaving tower, the second lightness-removing tower, the motorized tower and the second heaving tower adopt a plate tower, a packed tower or a plate-packed composite tower.
9. The method for producing electronic grade trichlorosilane by combining rectification, adsorption and membrane separation according to claim 4, wherein the processes in the steps (2) - (6) adopt a multi-effect rectification mode and a heat pump rectification mode.
10. The method for producing electronic-grade trichlorosilane by combining rectification, adsorption and membrane separation according to claim 4, wherein the membrane separation device in the step (7) adopts a nanofiltration, microfiltration, ultrafiltration or pervaporation membrane separation mode.
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| CN115006883A (en) * | 2022-08-04 | 2022-09-06 | 北京化工大学 | Production system, production method and application of general high-purity chemicals |
| CN115196638A (en) * | 2022-07-23 | 2022-10-18 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for removing impurities from silicon tetrachloride |
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