CN102259868A - Wet dust removal process for trichlorosilane synthesis gas in production of polycrystalline silicon - Google Patents
Wet dust removal process for trichlorosilane synthesis gas in production of polycrystalline silicon Download PDFInfo
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- CN102259868A CN102259868A CN2011101307225A CN201110130722A CN102259868A CN 102259868 A CN102259868 A CN 102259868A CN 2011101307225 A CN2011101307225 A CN 2011101307225A CN 201110130722 A CN201110130722 A CN 201110130722A CN 102259868 A CN102259868 A CN 102259868A
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- rectifying tower
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- trichlorosilane synthesis
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Abstract
The invention discloses a wet dust removal process for trichlorosilane synthesis gas in the production of polycrystalline silicon, which comprises the following steps of: introducing the trichlorosilane synthesis gas into a dust removal rectifying tower which is a plate tower with the operating pressure of 120 to 150kPa, and ensuring that light components are continuously vaporized, ascended and enriched and are extracted from the top of the dust removal rectifying tower; refluxing reflux consisting of the following components in percentage by mass: 80 to 85 percent of SiHCl3 and 15 to 20 percent of SiCl4 on the top of the dust removal rectifying tower at the temperature of between 10 and 15 DEG C, wherein the feed mass flow rate ratio of the reflux to the trichlorosilane synthesis gas is 0.8 to 2; and ensuring that heavy component impurities in the synthesis gas and the reflux are continuously subjected to heat exchange and condensation, enter a reboiler from the bottom of the dust removal rectifying tower and are partially extracted. The process is simple, has the characteristics of low loss and energy consumption, is easy to implement, and effectively solves the problem of blockage in subsequent production, and continuity and stability in the process of producing trichlorosilane are facilitated.
Description
Technical field
The present invention relates to a kind of purifying method of trichlorosilane synthesis gas, specifically, relate to the dust collecting process of trichlorosilane synthesis gas in a kind of polysilicon production process.
Background technology
Polysilicon is the direct material of manufacture order crystal silicon, is the electronics and information infrastructure material of semiconducter device such as contemporary artificial intelligence, control automatically, information processing, opto-electronic conversion, is called as " foundation stone of Microelectronics Building ".Trichlorosilane claims trichlorosilane or trichlorosilane again, is the important intermediate of making silane coupling agent and other organosilicon product, still makes the main raw material of polysilicon.Silane coupling agent is a kind of organosilicon matrix material of important, high added value, can make non-crosslinked resin realize crosslinking curing or modification by silane coupling agent, has therefore obtained using widely in industries such as glass fibre, casting, rubbers for tire.Constantly soaring along with polysilicon output constantly enlarges the demand of trichlorosilane.
Trichlorosilane be by hydrogenchloride and silica flour in 0.12～0.20MPa (absolute pressure), under 250～350 ℃ the reaction conditions, in fluidized-bed reactor, synthesize.The equation of reaction is: Si+3HCl==HSiCl
3+ H
2, main side reaction is Si+4HCl==SiCl
4+ 2H
2, also have a spot of dichloro-dihydro silicon to generate simultaneously.In addition, in existing trichlorosilane Production Flow Chart since the raw material silica flour with hcl reaction in, can generate AlO
3, FeO
3The contour mixture that boils is very easy to after the condensation stop up pre-cooler and follow-up system pipeline, makes that whole process of production can not be continuous.
At above problem, publication number is that the Chinese patent of CN101766942A has proposed a kind of trichlorosilane dust removal installation and dust collecting process thereof, dust removal installation comprises the tower of giving a dinner of welcome, the give a dinner of welcome bottom of tower is provided with the synthesis gas inlet pipe, top is provided with synthesis gas and goes out pipe, the tower of giving a dinner of welcome is connected with the silicon tetrachloride adding set, the synthetic gas that comes out in the synthetic furnace, entering wet dedusting again through behind the bag-type dust, tower spray technology is adopted in wet dedusting, adopts the silicon tetrachloride as by-product in the trichlorosilane technology to make washing composition.Though this invention selects for use silicon tetrachloride as washing composition, whole complex technical process, equipment is many, investment is big, is unfavorable for automated operation, and rectifying product silicon tetrachloride still need separate, and increases the treatment capacity in the follow-up treating process, increases energy consumption.
Therefore, find a kind of silicon powder particle and higher-boiling compound in the trichlorosilane synthesis gas that effectively separate in polysilicon production process, energy consumption is low simultaneously, and process successive method is very necessary.
Summary of the invention
What the present invention will solve is the easy block system of high boiling material, cause the production process of trichlorosilane can not the quantity-produced technical problem, a kind of wet dedusting technology that is applied in the polysilicon production process is provided, by trichlorosilane synthesis gas is carried out wet dedusting, obtain removing the trichlorosilane synthesis gas of high boiling material.Present method technical process is simple, has easy realization, and loss is few, and characteristic of low energy consumption effectively solves the subsequent production blockage problem simultaneously, is convenient to the continous-stable of production process of trichlorosilane.
In order to solve the problems of the technologies described above, device of the present invention is achieved by following technical scheme:
A kind of wet dedusting technology that is used for the production of polysilicon trichlorosilane synthesis gas, this technology comprises the steps:
A. trichlorosilane synthesis gas is fed the dedusting rectifying tower by the opening for feed that is arranged at below the column plate, the dedusting rectifying tower is a tray column, and the trichlorosilane synthesis gas charging is made of following component according to mass percent: H
2: 1%～2%, HCl:8%～10%, SiHCl
3: 80%～82%, SiCl
4: 7%～8%, heavy constituent impurity: 0.3%～0.6%; Dedusting rectifying tower working pressure is 120～150kpa;
B. the rising enrichment of constantly vaporizing of the light constituent in the trichlorosilane synthesis gas is finally by the extraction of dedusting rectifying tower cat head;
C. dedusting rectifying tower cat head adopts phegma to reflux, and phegma is made of following component according to mass percent: SiHCl
3: 80%～85%, SiCl
4: 15%～20%; The temperature of phegma is 10～15 ℃, and phegma is 0.8～2 with the mass flow rate ratio of trichlorosilane synthesis gas charging;
D. the continuous heat exchange condensation of phegma that descends in heavy constituent impurity in the trichlorosilane synthesis gas and the dedusting rectifying tower finally enters reboiler, the part extraction by dedusting rectifying tower tower bottom branch.
The column plate of described dedusting rectifying tower is preferably the block-resisting type column plate.
The invention has the beneficial effects as follows:
(1) the present invention adopts rectifying and dedusting combinatorial principle to remove silicon powder particle and higher-boiling compound in the trichlorosilane synthesis gas, does not introduce novel substance, is convenient to following process, has easy realization, and loss is few, simultaneously characteristic of low energy consumption.
(2) the present invention includes only a rectifying tower, and technical process is simple, and the phegma wide material sources adopt the thick product reflux of subsequent technique, and are easy to operate, are beneficial to the continuity operation, pollutes for a short time, and cost is low.
(3) the dedusting rectifying tower of the present invention's employing can be tray column, and is simple in structure, is convenient to the processing design.
(4) the resulting trichlorosilane synthesis gas heavy constituent of the present invention high boiling material decreasing ratio can reach 99.99%, avoids the subsequent technique line clogging, helps full-range serialization production.
Description of drawings
Accompanying drawing is the schematic flow sheet of wet dedusting technology of the present invention.
Embodiment
The material that the present invention handles is a trichlorosilane synthesis gas, is particularly suitable for the trichlorosilane synthesis gas through whirlwind, bag-type dusting processing, adopts rectifying and dedusting combinatorial principle and wet dedusting mode, obtains removing the trichlorosilane synthesis gas of high boiling material.
As shown in drawings, the present invention discloses a kind of wet dedusting technology that is used for the production of polysilicon trichlorosilane synthesis gas, form with relevant pipeline by a dedusting rectifying tower, the dedusting rectifying tower adopts tray column, its column plate can adopt bubble cap plate, sieve tray, valve tray, ejection-type column plate etc., preferred block-resisting type column plate.
Earlier trichlorosilane synthesis gas is fed the dedusting rectifying tower by the opening for feed that is arranged at below the column plate, the trichlorosilane synthesis gas charging is made of following component according to mass percent: H
2: 1%～2%, HCl:8%～10%, SiHCl
3: 80%～82%, SiCl
4: 7%～8%, heavy constituent impurity: 0.3%～0.6%, H wherein
2, HCl, SiHCl
3, SiCl
4Be light constituent, and heavy constituent impurity is aluminum chloride, boron trichloride, other metallic compounds and unreacted silica flour.The feeding temperature of trichlorosilane synthesis gas is general 130～150 ℃, and feed pressure is generally 150～170kpa, and the working pressure of dedusting rectifying tower is 120-150kpa.Dedusting rectifying tower cat head adopts the thick product reflux of trichlorosilane, and phegma is made of following component according to mass percent: SiHCl
3: 80%～85%, SiCl
4: 15%～20%; The temperature of phegma is 10～15 ℃, and phegma is 0.8～2 with the mass flow rate ratio of trichlorosilane synthesis gas charging.
In rectifying, high boiling material such as the silica flour in the trichlorosilane synthesis gas are because boiling point higher (generally more than 150 ℃), with the continuous heat exchange condensation of the phegma that descends in the dedusting rectifying tower, finally enrichment at the bottom of tower, the output section enters reboiler at the bottom of the tower, rectifying tower is returned in vaporization through reboiler, as the vapour phase of rectifying tower rising; Part extraction, extraction are the raffinate that is rich in high boiling material; And trichlorosilane and other light constituent boiling points (31.85 ℃) are lower, the rising enrichment of constantly vaporizing, and by dedusting rectifying tower cat head extraction trichlorosilane monomer mixture, the raffinate of high boiling material is rich in the extraction of tower still like this.
Below by specific embodiment technical process of the present invention is described in further detail:
Following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1
Trichlorosilane synthesis gas is fed the dedusting rectifying tower by the opening for feed that is arranged at below the column plate, and the dedusting rectifying tower is a tray column, and the trichlorosilane synthesis gas charging is made of following component according to mass percent: H
2: 1%, HCl:10%, SiHCl
3: 81.4%, SiCl
4: 7%, heavy constituent impurity: 0.6%, dedusting rectifying tower 1 working pressure is 120kpa; The rising enrichment of constantly vaporizing of light constituent in the trichlorosilane synthesis gas is finally by the extraction of dedusting rectifying tower cat head; Dedusting rectifying tower cat head adopts phegma to reflux, and phegma is made of following component according to mass percent: SiHCl
3: 80%, SiCl
4: 20%; The temperature of phegma is 10 ℃, and phegma is 0.8 with the mass flow rate ratio of trichlorosilane synthesis gas charging; The continuous heat exchange condensation of phegma that descends in heavy constituent impurity in the trichlorosilane synthesis gas and the dedusting rectifying tower finally enters reboiler, the part extraction by dedusting rectifying tower tower bottom branch.After above-mentioned art breading, the content of high boiling material is 0.0009% in the monomer mixture of extraction, and the rate of recovery of trichlorosilane is 98.4%, and the content of trichlorosilane and silicon tetrachloride is 30.5% in the high boiling material.
Embodiment 2
Trichlorosilane synthesis gas is fed the dedusting rectifying tower by the opening for feed that is arranged at below the column plate, and the dedusting rectifying tower is a tray column, and the trichlorosilane synthesis gas charging is made of following component according to mass percent: H
2: 1.3%, HCl:8.5%, SiHCl
3: 81.9%, SiCl
4: 7.8%, heavy constituent impurity: 0.5%, dedusting rectifying tower 1 working pressure is 125kpa; The rising enrichment of constantly vaporizing of light constituent in the trichlorosilane synthesis gas is finally by the extraction of dedusting rectifying tower cat head; Dedusting rectifying tower cat head adopts phegma to reflux, and phegma is made of following component according to mass percent: SiHCl
3: 82.1%, SiCl
4: 17.9%; The temperature of phegma is 12 ℃, and phegma is 1.0 with the mass flow rate ratio of trichlorosilane synthesis gas charging; The continuous heat exchange condensation of phegma that descends in heavy constituent impurity in the trichlorosilane synthesis gas and the dedusting rectifying tower finally enters reboiler, the part extraction by dedusting rectifying tower tower bottom branch.After above-mentioned art breading, the content of high boiling material is 0.0008% in the monomer mixture of extraction, and the rate of recovery of trichlorosilane is 99.1%, and the content of trichlorosilane and silicon tetrachloride is 29.8% in the high boiling material.
Embodiment 3
Trichlorosilane synthesis gas is fed the dedusting rectifying tower by the opening for feed that is arranged at below the column plate, and the dedusting rectifying tower is a tray column, and the trichlorosilane synthesis gas charging is made of following component according to mass percent: H
2: 1.5%, HCl:9%, SiHCl
3: 81.55%, SiCl4:7.5%, heavy constituent impurity: 0.45%, dedusting rectifying tower 1 working pressure is 130kpa; The rising enrichment of constantly vaporizing of light constituent in the trichlorosilane synthesis gas is finally by the extraction of dedusting rectifying tower cat head; Dedusting rectifying tower cat head adopts phegma to reflux, and phegma is made of following component according to mass percent: SiHCl
3: 83.6%, SiCl
4: 16.4%; The temperature of phegma is 15 ℃, and phegma is 1.3 with the mass flow rate ratio of trichlorosilane synthesis gas charging; The continuous heat exchange condensation of phegma that descends in heavy constituent impurity in the trichlorosilane synthesis gas and the dedusting rectifying tower finally enters reboiler, the part extraction by dedusting rectifying tower tower bottom branch.After above-mentioned art breading, the content of high boiling material is 0.0006% in the monomer mixture of extraction, and the rate of recovery of trichlorosilane is 99.4%, and the content of trichlorosilane and silicon tetrachloride is 29.6% in the high boiling material.
Embodiment 4
Trichlorosilane synthesis gas is fed the dedusting rectifying tower by the opening for feed that is arranged at below the column plate, and the dedusting rectifying tower is a tray column, and the trichlorosilane synthesis gas charging is made of following component according to mass percent: H
2: 1.7%, HCl:9.4%, SiHCl
3: 80.9%, SiCl
4: 7.6%, heavy constituent impurity: 0.4%, dedusting rectifying tower 1 working pressure is 140kpa; The rising enrichment of constantly vaporizing of light constituent in the trichlorosilane synthesis gas is finally by the extraction of dedusting rectifying tower cat head; Dedusting rectifying tower cat head adopts phegma to reflux, and phegma is made of following component according to mass percent: SiHCl
3: 84.3%, SiCl
4: 15.7%; The temperature of phegma is 17 ℃, and phegma is 1.7 with the mass flow rate ratio of trichlorosilane synthesis gas charging; The continuous heat exchange condensation of phegma that descends in heavy constituent impurity in the trichlorosilane synthesis gas and the dedusting rectifying tower finally enters reboiler, the part extraction by dedusting rectifying tower tower bottom branch.After above-mentioned art breading, the content of high boiling material is 0.0006% in the monomer mixture of extraction, and the rate of recovery of trichlorosilane is 99.3%, and the content of trichlorosilane and silicon tetrachloride is 29.4% in the high boiling material.
Embodiment 5
Trichlorosilane synthesis gas is fed the dedusting rectifying tower by the opening for feed that is arranged at below the column plate, and the dedusting rectifying tower is a tray column, and the trichlorosilane synthesis gas charging is made of following component according to mass percent: H
2: 2%, HCl:8%, SiHCl
3: 81.7%, SiCl
4: 8%, heavy constituent impurity: 0.3%, dedusting rectifying tower 1 working pressure is 150kpa; The rising enrichment of constantly vaporizing of light constituent in the trichlorosilane synthesis gas is finally by the extraction of dedusting rectifying tower cat head; Dedusting rectifying tower cat head adopts phegma to reflux, and phegma is made of following component according to mass percent: SiHCl
3: 85%, SiCl
4: 15%; The temperature of phegma is 20 ℃, and phegma is 2 with the mass flow rate ratio of trichlorosilane synthesis gas charging; The continuous heat exchange condensation of phegma that descends in heavy constituent impurity in the trichlorosilane synthesis gas and the dedusting rectifying tower finally enters reboiler, the part extraction by dedusting rectifying tower tower bottom branch.After above-mentioned art breading, the content of high boiling material is 0.0005% in the monomer mixture of extraction, and the rate of recovery of trichlorosilane is 99.5%, and the content of trichlorosilane and silicon tetrachloride is 29.3% in the high boiling material.
Embodiment 6
Trichlorosilane synthesis gas is fed the dedusting rectifying tower by the opening for feed that is arranged at below the column plate, and the dedusting rectifying tower is a tray column, and the trichlorosilane synthesis gas charging is made of following component according to mass percent: H
2: 1.3%, HCl:8.5%, SiHCl
3: 81.9%, SiCl
4: 7.8%, heavy constituent impurity: 0.5%, dedusting rectifying tower 1 working pressure is 130kpa; The rising enrichment of constantly vaporizing of light constituent in the trichlorosilane synthesis gas is finally by the extraction of dedusting rectifying tower cat head; Dedusting rectifying tower cat head adopts phegma to reflux, and phegma is made of following component according to mass percent: SiHCl
3: 82.2%, SiCl
4: 17.8%; The temperature of phegma is 15 ℃, and phegma is 1.5 with the mass flow rate ratio of trichlorosilane synthesis gas charging; The continuous heat exchange condensation of phegma that descends in heavy constituent impurity in the trichlorosilane synthesis gas and the dedusting rectifying tower finally enters reboiler, the part extraction by dedusting rectifying tower tower bottom branch.After above-mentioned art breading, the content of high boiling material is 0.0004% in the monomer mixture of extraction, and the rate of recovery of trichlorosilane is 99.6%, and the content of trichlorosilane and silicon tetrachloride is 29.0% in the high boiling material.
Although in conjunction with the accompanying drawings the preferred embodiments of the present invention are described above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment only is schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not breaking away under the scope situation that aim of the present invention and claim protect, can also make the concrete conversion of a lot of forms, these all belong within protection scope of the present invention.
Claims (2)
1. a wet dedusting technology that is used for the production of polysilicon trichlorosilane synthesis gas is characterized in that this technology comprises the steps:
A. trichlorosilane synthesis gas is fed the dedusting rectifying tower by the opening for feed that is arranged at below the column plate, the dedusting rectifying tower is a tray column, and the trichlorosilane synthesis gas charging is made of following component according to mass percent: H
2: 1%～2%, HCl:8%～10%, SiHCl
3: 80%～82%, SiCl
4: 7%～8%, heavy constituent impurity: 0.3%～0.6%; Dedusting rectifying tower working pressure is 120～150kpa;
B. the rising enrichment of constantly vaporizing of the light constituent in the trichlorosilane synthesis gas is finally by the extraction of dedusting rectifying tower cat head;
C. dedusting rectifying tower cat head adopts phegma to reflux, and phegma is made of following component according to mass percent: SiHCl
3: 80%～85%, SiCl
4: 15%～20%; The temperature of phegma is 10～15 ℃, and phegma is 0.8～2 with the mass flow rate ratio of trichlorosilane synthesis gas charging;
D. the continuous heat exchange condensation of phegma that descends in heavy constituent impurity in the trichlorosilane synthesis gas and the dedusting rectifying tower finally enters reboiler, the part extraction by dedusting rectifying tower tower bottom branch.
2. a kind of wet dedusting technology that is used for the production of polysilicon trichlorosilane synthesis gas according to claim 1 is characterized in that the column plate of described dedusting rectifying tower is the block-resisting type column plate.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102794070A (en) * | 2012-07-25 | 2012-11-28 | 新疆大全新能源有限公司 | Processing method for trichlorosilane gas |
| CN103693649A (en) * | 2013-11-25 | 2014-04-02 | 新特能源股份有限公司 | Impurity-removal and waste chlorosilane liquid-recovery method of synthetic gas production technology |
| CN108434910A (en) * | 2018-04-02 | 2018-08-24 | 江苏金牛环保工程设备有限公司 | One kind being used for organosilicon, production of polysilicon dust removal method and its production system |
| CN115557503A (en) * | 2022-10-11 | 2023-01-03 | 内蒙古鄂尔多斯多晶硅业有限公司 | Method for producing polycrystalline silicon and silane coupling agent in multiple-supplement and multiple-row mode |
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| CN201704078U (en) * | 2010-06-23 | 2011-01-12 | 天津市华瑞奕博化工科技有限公司 | Trichlorosilane raw monomer purifying device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102794070A (en) * | 2012-07-25 | 2012-11-28 | 新疆大全新能源有限公司 | Processing method for trichlorosilane gas |
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| CN103693649A (en) * | 2013-11-25 | 2014-04-02 | 新特能源股份有限公司 | Impurity-removal and waste chlorosilane liquid-recovery method of synthetic gas production technology |
| CN108434910A (en) * | 2018-04-02 | 2018-08-24 | 江苏金牛环保工程设备有限公司 | One kind being used for organosilicon, production of polysilicon dust removal method and its production system |
| CN108434910B (en) * | 2018-04-02 | 2021-05-11 | 江苏金牛环保工程设备有限公司 | Dust removal method and production system for production of organic silicon and polycrystalline silicon |
| CN115557503A (en) * | 2022-10-11 | 2023-01-03 | 内蒙古鄂尔多斯多晶硅业有限公司 | Method for producing polycrystalline silicon and silane coupling agent in multiple-supplement and multiple-row mode |
| CN115557503B (en) * | 2022-10-11 | 2023-12-05 | 内蒙古鄂尔多斯多晶硅业有限公司 | Method for producing polycrystalline silicon and silane coupling agent in multiple-compensation multiple rows |
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