CN115196638A - Method for removing impurities from silicon tetrachloride - Google Patents
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Abstract
The invention discloses a method for removing impurities from silicon tetrachloride, which comprises the following steps: introducing the crude silicon tetrachloride into a dedusting tower to remove high-boiling-point substances and silicon powder to obtain a liquid-phase product; pressurizing the liquid-phase product, and then sending the liquid-phase product into a membrane separator to remove other chlorides in the chlorosilane to obtain a high-pressure chlorosilane mixture; and (3) decompressing and removing trichlorosilane from the high-pressure chlorosilane mixture to obtain a high-purity silicon tetrachloride product with the mass fraction of more than 99.9999%. The method effectively removes other chlorides in the chlorosilane by using a membrane separation technology, combines membrane separation and rectification to achieve the aim of saving energy, has the membrane replacement time far shorter than the time of adsorbent regeneration or plasma drying, and effectively inhibits the extension of the production period and the increase of the impurity removal cost of silicon tetrachloride.
Description
Technical Field
The invention belongs to the technical field of polycrystalline silicon production, and particularly relates to a method for removing impurities from silicon tetrachloride.
Background
Silicon tetrachloride, also known as tetrachlorosilane, is an inorganic compound of the formula SiCl 4 At normal temperature and pressure, the melting point is-70 deg.C and the boiling point is 57.6 deg.C, which is heated or decomposed with water to release heat, generate silicic acid or ortho silicic acid, and release hydrogen chloride. SiCl 4 Mainly used for producing optical fibers, which requires SiCl in the raw material 4 The purity of the optical fiber reaches 6N (mass fraction) so as to ensure that the optical fiber product has good performance. Currently, siCl is produced 4 Most of the by-product method of polysilicon, namely, the method for producing SiHCl by improving the Siemens process 3 In the process of (2), by-product SiCl is collected 4 SiCl obtained by this process 4 Contains high polymer, silicon powder and SiHCl 3 、PCl 3 、BCl 3 And metal chlorides (TiCl) 4 、AlCl 3 、FeCl 3 ) And the like. In order to prepare high-purity SiCl 4 Many schemes are provided, and the schemes are divided into 3 types of absorption method, rectification method and plasma method from the idea of impurity removal, and each method has different purification effects and selectivity to impurities according to SiCl 4 And (4) the components of the intermediate impurities can be used singly or in combination.
A method for purifying optical fiber grade silicon tetrachloride by total reflux rectification (CN 201510884606.0) comprises the steps of enabling silicon tetrachloride waste liquid to enter a light component removal rectification tower, discharging tower bottoms consisting of silicon tetrachloride and phosphorus trichloride from the bottom of the tower to enter a silicon tetrachloride purification tower, condensing a tower top condenser, then enabling one part of the condensed tower bottoms to reflux, and enabling the other part of the condensed tower bottoms to be extracted to obtain an optical fiber grade silicon tetrachloride product.
In a method (CN 201811075032.2) for purifying silicon tetrachloride serving as a byproduct of polycrystalline silicon, crude silicon tetrachloride is adsorbed by amphoteric ion exchange resin to obtain purified silicon tetrachloride, and after purification is finished, the amphoteric ion exchange resin can be regenerated by rinsing with water.
In the method and the device (CN 201911112197.7), crude silicon tetrachloride is added into dry anhydrous ionic liquid for electrolysis and then is heated in a water bath, and steam obtained by heating is condensed to obtain high-purity silicon tetrachloride.
In order to solve the problems, the development of an energy-saving and economical method for removing impurities from silicon tetrachloride is particularly important.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for removing impurities from silicon tetrachloride aiming at the defects of the prior art. The method comprises the steps of introducing crude silicon tetrachloride into the bottom of a dedusting tower provided with a condenser at the top, obtaining high-boiling-point substances and silicon powder at the bottom of the dedusting tower to prevent subsequent equipment from being blocked, and obtaining a liquid-phase product at the top of the dedusting tower while refluxing and washing gas by part of condensed liquid; pressurizing the liquid-phase product by a shielding pump to obtain a high-pressure liquid-phase product and sending the high-pressure liquid-phase product into a membrane separator; the membrane in the membrane separator adopts an organic polymer reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride which are dissolved in silicon tetrachloride and trichlorosilane can be effectively removed, high-pressure chlorosilane mixed liquor processed by the membrane separator is introduced into a buffer tank, liquid chlorosilane mixed liquor is prevented from being gasified from the high-pressure membrane separator to a normal-pressure lightness-removing tower, the decompressed chlorosilane mixed liquor is sent to the lightness-removing tower for separation, trichlorosilane is obtained at the top of the lightness-removing tower, and a high-purity silicon tetrachloride product with the mass fraction of more than 99.9999% is obtained at the bottom of the tower.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method for removing impurities from silicon tetrachloride is characterized by comprising the following steps:
s1, introducing a crude silicon tetrachloride into a dedusting tower, and dedusting under the conditions that the operation pressure at the top of the dedusting tower is 1bar and the operation temperature at the top of the dedusting tower is 65-85 ℃, wherein high-boiling-point substances and silicon powder are obtained at the bottom of the dedusting tower, and a liquid-phase product is obtained at the top of the dedusting tower;
s2, pressurizing the liquid-phase product obtained in the S1 through a shielding pump, and introducing the pressurized liquid-phase product into a membrane separator for impurity removal to obtain high-pressure chlorosilane mixed liquid; introducing the high-pressure chlorosilane mixed solution into a buffer tank which is depressurized to 1bar to obtain a chlorosilane mixed solution;
s3, introducing the chlorosilane mixed liquid obtained in the S2 into a light component removal tower for rectification, wherein the operation pressure at the top of the light component removal tower is 1bar, and the operation temperature at the top of the light component removal tower is 35-55 ℃; trichlorosilane is discharged from the top of the light component removing tower, and high-purity silicon tetrachloride with the mass fraction of more than 99.9999 percent is obtained from the tower bottom.
Preferably, the theoretical plate number of the dust removing tower in the S1 is 45-65, and the reflux ratio is 1-5.
Preferably, the liquid phase product in S1 comprises silicon tetrachloride, trichlorosilane, boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride.
Preferably, the outlet pressure of the shielding pump in S2 is 1 MPa-6 MPa.
Preferably, the membrane in the membrane separator in S2 is an organic polymer reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic polymer reverse osmosis membrane is a trimesoyl chloride-polyether sulfone membrane.
Preferably, the high-pressure chlorosilane mixed solution in S2 comprises silicon tetrachloride and trichlorosilane.
Preferably, the theoretical plate number of the light component removal tower in the S3 is 60 to 80, and the reflux ratio is 3 to 5.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the membrane separator is arranged, other chlorides and chlorosilane are separated by using the organic polymer reverse osmosis membrane, other chlorides in the chlorosilane are effectively removed, and the mass fraction of high-purity silicon tetrachloride reaches 99.9999% after subsequent light removal and purification.
2. The invention combines membrane separation and rectification, only adopts two rectifying towers, saves two rectifying towers compared with the traditional method for removing impurities from silicon tetrachloride by singly adopting rectification, and realizes the purpose of energy conservation.
3. The time for replacing the film is far shorter than the time for regenerating the adsorbent or drying the plasma, so that the extension of the production period and the increase of the impurity removal cost of silicon tetrachloride are effectively inhibited.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic flow diagram of a method for removing silicon tetrachloride according to the invention.
Description of reference numerals:
1-crude silicon tetrafluoride; 2-high boiling residue and silicon powder; 3-liquid phase product; 4-high pressure liquid phase product; 5-high pressure chlorosilane mixed liquor; 6-chlorosilane mixed liquor; 7-trichlorosilane; 8-high purity silicon tetrafluoride; t101, a dust removal tower; p101 — canned pump; m101-membrane separator; h101, a buffer tank; t102-lightness-removing tower.
Detailed Description
The crude silicon tetrachloride used in examples 1-3 had the following composition: the mass fraction of the silicon tetrachloride is 85%, the mass fraction of the trichlorosilane is 13%, the total mass fraction of the high-boiling-point substance and the silicon powder is 1%, and the total mass fraction of the boron trichloride, the phosphorus trichloride, the titanium tetrachloride, the aluminum trichloride and the ferric trichloride is 1%.
Example 1
The method for removing the silicon tetrachloride comprises the following steps:
s1, introducing crude silicon tetrachloride 1 with the total mass flow of 100.00kg/h into the bottom of a dedusting tower T101, dedusting under the conditions that the operation pressure at the top of the dedusting tower T101 is 1bar, the operation temperature at the top of the dedusting tower is 65 ℃, the number of theoretical plates is 45, and the reflux ratio is 1, obtaining high-boiling-point substances and silicon powder 2 with the mass flow of 1.2kg/h at the bottom of the dedusting tower T101, and obtaining a liquid-phase product 3 with the mass flow of 98.80kg/h at the top of the dedusting tower;
the liquid phase product 3 comprises silicon tetrachloride, trichlorosilane, boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride; the content of silicon tetrachloride in the liquid-phase product 3 is 85.83%, the content of trichlorosilane is 13.15%, the total content of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is 1.01%, and the total content of high-boiling-point substances and silicon powder is less than 1ppm;
s2, introducing the liquid-phase product 3 obtained in the S1 into a shielding pump P101 for pressurization to obtain a high-pressure liquid-phase product 4; introducing a high-pressure liquid-phase product 4 with the mass flow of 98.80kg/h into a membrane separator M101 for impurity removal under the condition that the outlet pressure of the shielding pump P101 is 6MPa to obtain a high-pressure chlorosilane mixed liquid 5 with the mass flow of 97.65 kg/h; introducing the high-pressure chlorosilane mixed solution 5 into a buffer tank H101 decompressed to 1bar to obtain a chlorosilane mixed solution 6 with the mass flow of 97.65 kg/H;
the membrane in the membrane separator M101 adopts an organic polymer reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic polymer reverse osmosis membrane is a trimesoyl chloride-polyether sulfone membrane; the content of silicon tetrachloride in the high-pressure chlorosilane mixed solution 5 is 86.74 percent, the content of trichlorosilane is 13.25 percent, the total content of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is less than 1ppm, and the total content of high-boiling-point substances and silicon powder is less than 1ppm;
s3, introducing the chlorosilane mixed liquor 6 obtained in the S2 into a light component removal tower T102 for rectification, wherein the operation pressure at the top of the light component removal tower T102 is 1bar, the operation temperature at the top of the light component removal tower is 35 ℃, the number of theoretical plates is 60, and the reflux ratio is 3; trichlorosilane 7 with the mass flow of 12.97kg/h is discharged from the top of the lightness-removing tower T102, and high-purity silicon tetrachloride 8 with the mass flow of 84.68kg/h is obtained from the bottom of the tower;
through detection, the content of the silicon tetrachloride in the high-purity silicon tetrachloride 8 is 99.99996%, the content of the trichlorosilane is 38ppm, the total content of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is less than 1ppm, and the content of high-boiling-point substances and silicon powder is less than 1ppm.
Example 2
The method for removing the silicon tetrachloride comprises the following steps:
s1, introducing crude silicon tetrachloride 1 with the total mass flow of 100.00kg/h into the bottom of a dedusting tower T101, dedusting under the conditions that the operation pressure at the top of the dedusting tower T101 is 1bar, the operation temperature at the top of the dedusting tower is 85 ℃, the number of theoretical plates is 65, and the reflux ratio is 5, obtaining high-boiling-point substances and silicon powder 2 with the mass flow of 1.05kg/h at the bottom of the dedusting tower T101, and obtaining a liquid-phase product 3 with the mass flow of 98.95kg/h at the top of the dedusting tower;
the liquid-phase product 3 comprises silicon tetrachloride, trichlorosilane, boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride; the content of silicon tetrachloride in the liquid-phase product 3 is 85.85%, the content of trichlorosilane is 13.13%, the total content of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is 1.01%, and the total content of high-boiling-point substances and silicon powder is less than 1ppm;
s2, introducing the liquid-phase product 3 obtained in the S1 into a shielding pump P101 for pressurization to obtain a high-pressure liquid-phase product 4; introducing a high-pressure liquid-phase product 4 with the mass flow of 98.95kg/h into a membrane separator M101 for impurity removal under the condition that the outlet pressure of the shielding pump P101 is 1MPa to obtain a high-pressure chlorosilane mixed solution 5 with the mass flow of 97.60 kg/h; introducing the high-pressure chlorosilane mixed solution 5 into a buffer tank H101 decompressed to 1bar to obtain a chlorosilane mixed solution 6 with the mass flow of 97.60 kg/H;
the membrane in the membrane separator M101 is an organic polymer reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic polymer reverse osmosis membrane is a trimesoyl chloride-polyether sulfone membrane; the content of silicon tetrachloride in the high-pressure chlorosilane mixed solution 5 is 86.78 percent, the content of trichlorosilane is 13.21 percent, the total content of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is less than 1ppm, and the total content of high-boiling-point substances and silicon powder is less than 1ppm;
s3, introducing the chlorosilane mixed solution 6 obtained in the S2 into a light component removal tower T102 for rectification, wherein the operation pressure at the top of the light component removal tower T102 is 1bar, the operation temperature at the top of the light component removal tower is 55 ℃, the number of theoretical plates is 80, and the reflux ratio is 5; trichlorosilane 7 with the mass flow of 13.32kg/h is discharged from the top of the lightness-removing column T102, and high-purity silicon tetrachloride 8 with the mass flow of 84.28kg/h is obtained from the bottom of the column;
through detection, the content of the silicon tetrachloride in the high-purity silicon tetrachloride 8 is 99.99999 percent, the content of the trichlorosilane is 8ppm, the total content of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is less than 1ppm, and the total content of high-boiling-point substances and silicon powder is less than 1ppm.
Example 3
The method for removing the silicon tetrachloride comprises the following steps:
s1, introducing crude silicon tetrachloride 1 with the total mass flow of 100.00kg/h into the bottom of a dedusting tower T101, dedusting under the conditions that the operation pressure at the top of the dedusting tower T101 is 1bar, the operation temperature at the top of the dedusting tower is 75 ℃, the number of theoretical plates is 55, and the reflux ratio is 3, obtaining high-boiling-point substances and silicon powder 2 with the mass flow of 1.13kg/h at the bottom of the dedusting tower T101, and obtaining a liquid-phase product 3 with the mass flow of 98.87kg/h at the top of the dedusting tower;
the liquid phase product 3 comprises silicon tetrachloride, trichlorosilane, boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride; the content of silicon tetrachloride in the liquid-phase product 3 is 85.83%, the content of trichlorosilane is 13.15%, the total content of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is 1.01%, and the total content of high-boiling-point substances and silicon powder is less than 1ppm;
s2, introducing the liquid-phase product 3 obtained in the S1 into a shielding pump P101 for pressurization to obtain a high-pressure liquid-phase product 4; introducing a high-pressure liquid-phase product 4 with the mass flow of 98.87kg/h into a membrane separator M101 for impurity removal under the condition that the outlet pressure of the shielding pump P101 is 3MPa to obtain a high-pressure chlorosilane mixed solution 5 with the mass flow of 97.62 kg/h; introducing the high-pressure chlorosilane mixed solution 5 into a buffer tank H101 decompressed to 1bar to obtain a chlorosilane mixed solution 6 with the mass flow of 97.62 kg/H;
the membrane in the membrane separator M101 is an organic polymer reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic polymer reverse osmosis membrane is a trimesoyl chloride-polyether sulfone membrane; the content of silicon tetrachloride in the high-pressure chlorosilane mixed liquid 5 is 86.77 percent, the content of trichlorosilane is 13.22 percent, the total content of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is less than 1ppm, and the total content of high-boiling-point substances and silicon powder is less than 1ppm;
s3, introducing the chlorosilane mixed solution 6 obtained in the S2 into a light component removal tower T102 for rectification, wherein the operation pressure at the top of the light component removal tower T102 is 1bar, the operation temperature at the top of the tower is 45 ℃, the number of theoretical plates is 70, and the reflux ratio is 4; trichlorosilane 7 with the mass flow of 13.07kg/h is discharged from the top of the lightness-removing column T102, and high-purity silicon tetrachloride 8 with the mass flow of 84.55kg/h is obtained from the bottom of the column;
through detection, the content of the silicon tetrachloride in the high-purity silicon tetrachloride 8 is 99.99998%, the content of the trichlorosilane is 18ppm, the total content of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is less than 1ppm, and the total content of high-boiling-point substances and silicon powder is less than 1ppm.
In examples 1 to 3, the contents of the respective components are represented by mass fractions; in the embodiment 1-3, the device used in the method for removing the silicon tetrachloride impurities comprises a dust removal tower T101, a shielding pump P101, a membrane separator M101, a buffer tank H101 and a light component removal tower T102 which are sequentially connected in series; and a condenser is arranged at the top of the dust removing tower T101.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (7)
1. A method for removing impurities from silicon tetrachloride is characterized by comprising the following steps:
s1, introducing a crude silicon tetrachloride into a dedusting tower, and dedusting under the conditions that the operation pressure at the top of the dedusting tower is 1bar and the operation temperature at the top of the dedusting tower is 65-85 ℃, wherein high-boiling-point substances and silicon powder are obtained at the bottom of the dedusting tower, and a liquid-phase product is obtained at the top of the dedusting tower;
s2, pressurizing the liquid-phase product obtained in the S1 through a shielding pump, and introducing the pressurized liquid-phase product into a membrane separator for impurity removal to obtain high-pressure chlorosilane mixed liquid; introducing the high-pressure chlorosilane mixed solution into a buffer tank which is depressurized to 1bar to obtain a chlorosilane mixed solution;
s3, introducing the chlorosilane mixed liquor obtained in the S2 into a light component removal tower for rectification, wherein the operation pressure at the top of the light component removal tower is 1bar, and the operation temperature at the top of the light component removal tower is 35-55 ℃; trichlorosilane is discharged from the top of the light component removing tower, and high-purity silicon tetrachloride with the mass fraction of more than 99.9999 percent is obtained from the tower bottom.
2. An impurity removal method for silicon tetrachloride according to claim 1, wherein the number of theoretical plates of the dust removal tower in the S1 is 45-65, and the reflux ratio is 1-5.
3. A method for removing impurities from silicon tetrachloride according to claim 1, wherein the liquid-phase product in S1 comprises silicon tetrachloride, trichlorosilane, boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride.
4. An impurity removal method for silicon tetrachloride according to claim 1, wherein the outlet pressure of the shielding pump in S2 is 1MPa to 6MPa.
5. An impurity removal method for silicon tetrachloride according to claim 1, wherein the membrane in the membrane separator in S2 is an organic polymer reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic polymer reverse osmosis membrane is a trimesoyl chloride-polyether sulfone membrane.
6. A method for removing impurities from silicon tetrachloride according to claim 1, wherein the high-pressure chlorosilane mixed solution in S2 comprises silicon tetrachloride and trichlorosilane.
7. An impurity removal method for silicon tetrachloride according to claim 1, wherein the theoretical plate number of the lightness-removing column in S3 is 60 to 80, and the reflux ratio is 3 to 5.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780958A (en) * | 2010-03-30 | 2010-07-21 | 中国天辰工程有限公司 | Method for rectifying trichlorosilane and silicon tetrachloride |
| CN102642839A (en) * | 2012-05-09 | 2012-08-22 | 特变电工新疆硅业有限公司 | Processing process of industrial grade silicon tetrachloride |
| CN105502409A (en) * | 2015-12-04 | 2016-04-20 | 天津大学 | Method and device for purifying silicon tetrachloride of optical fiber grade through total reflux distillation |
| CN106477584A (en) * | 2016-10-09 | 2017-03-08 | 洛阳中硅高科技有限公司 | Optical fiber level silicon tetrachloride and preparation method thereof |
| CN114735709A (en) * | 2022-06-15 | 2022-07-12 | 北京化工大学 | Device and method for producing electronic grade trichlorosilane by combination of rectification, adsorption and membrane separation |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780958A (en) * | 2010-03-30 | 2010-07-21 | 中国天辰工程有限公司 | Method for rectifying trichlorosilane and silicon tetrachloride |
| CN102642839A (en) * | 2012-05-09 | 2012-08-22 | 特变电工新疆硅业有限公司 | Processing process of industrial grade silicon tetrachloride |
| CN105502409A (en) * | 2015-12-04 | 2016-04-20 | 天津大学 | Method and device for purifying silicon tetrachloride of optical fiber grade through total reflux distillation |
| CN106477584A (en) * | 2016-10-09 | 2017-03-08 | 洛阳中硅高科技有限公司 | Optical fiber level silicon tetrachloride and preparation method thereof |
| CN114735709A (en) * | 2022-06-15 | 2022-07-12 | 北京化工大学 | Device and method for producing electronic grade trichlorosilane by combination of rectification, adsorption and membrane separation |
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