CN115196638B - Silicon tetrachloride impurity removal method - Google Patents
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Abstract
The invention discloses a silicon tetrachloride impurity removal method, which comprises the following steps: introducing crude silicon tetrachloride into a dedusting tower to remove high-boiling substances and silicon powder, so as to obtain a liquid-phase product; pressurizing the liquid-phase product, and then delivering the liquid-phase product into a membrane separator to remove other chlorides in the chlorosilane, so as to obtain a high-pressure chlorosilane mixture; and (3) decompressing and removing light 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 invention effectively removes other chlorides in the chlorosilane by utilizing a membrane separation technology, combines membrane separation and rectification, realizes the purpose of energy conservation, and ensures that the time for replacing the membrane is far less than the time for regenerating an adsorbent or drying plasma, thereby effectively inhibiting the extension of the production period and the increase of the impurity removal cost of unit silicon tetrachloride.
Description
Technical Field
The invention belongs to the technical field of polysilicon production, and particularly relates to a silicon tetrachloride impurity removal method.
Background
Silicon tetrachloride, also known as tetrachlorosilane, is an inorganic compound of the formula SiCl 4 The melting point is-70 ℃ and the boiling point is 57.6 ℃ at normal temperature and normal pressure, and the material is heated or decomposed and released by water to generate silicic acid or orthosilicic acid, and hydrogen chloride is further released. SiCl 4 Mainly used for producing optical fibers, which requires SiCl in raw materials 4 The purity of the product reaches 6N (mass fraction) to ensure good performance of the optical fiber product. At present, siCl is produced 4 The byproduct method of polysilicon is mostly adopted, i.e. SiHCl is produced by the improved Siemens method 3 During (2) collecting byproduct SiCl 4 SiCl obtained by this method 4 Contains high polymer, silicon powder and SiHCl 3 、PCl 3 、BCl 3 And metal chloride (TiCl) 4 、AlCl 3 、FeCl 3 ) Equal impurity. For the preparation of high purity SiCl in the industry 4 Various schemes are proposed, namely 3 methods of adsorption method, rectification method and plasma method from the perspective of impurity removal thought, and the methods have different purification effects and impurity selectivity according to SiCl 4 The composition of the impurities in the above-mentioned materials can be used singly or in combination.
In the method (CN 201510884606.0) for purifying optical-fiber-grade silicon tetrachloride by total reflux rectification, silicon tetrachloride waste liquid enters a light-removal rectifying tower, tower bottom liquid consisting of silicon tetrachloride and phosphorus trichloride is discharged from the bottom of the tower, enters a silicon tetrachloride purifying tower, part of the tower bottom liquid is refluxed after being condensed by a tower top condenser, and the other part of the tower bottom liquid is extracted to obtain an optical-fiber-grade silicon tetrachloride product, but a large amount of energy is consumed by separate rectification purification, and the cost is high.
In the purification method (CN 201811075032.2) of the silicon tetrachloride serving as a byproduct of polysilicon, crude silicon tetrachloride is adsorbed by a zwitterionic ion exchange resin to obtain purified silicon tetrachloride, and after purification is finished, the ion exchange resin can be regenerated by rinsing with water.
A method for removing impurities from silicon tetrachloride and a device thereof (CN 201911112197.7) are characterized in that crude silicon tetrachloride is added into dry anhydrous ionic liquid for electrolysis and then heated in a water bath, and steam obtained by heating is condensed to obtain high-purity silicon tetrachloride.
In order to solve the problems, it is particularly important to develop an energy-saving and economical silicon tetrachloride impurity removal method.
Disclosure of Invention
The invention aims to solve the technical problem of providing a silicon tetrachloride impurity removal method aiming at the defects in the prior art. The method comprises the steps that crude silicon tetrachloride is introduced into the bottom of a dedusting tower provided with a condenser at the top of the dedusting tower, high-boiling substances and silicon powder are obtained at the bottom of the dedusting tower, subsequent equipment is prevented from being blocked, and liquid phase products are obtained when part of condensate liquid at the top of the dedusting tower reflows washing gas; pressurizing the liquid phase product through 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 high molecular reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, so that boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride which are dissolved in the silicon tetrachloride and the trichlorosilane can be effectively removed, the high-pressure chlorosilane mixed solution treated by the membrane separator is introduced into a buffer tank, the liquid chlorosilane mixed solution is prevented from being gasified in the process from the high-pressure membrane separator to the normal-pressure lightness-removing tower, the chlorosilane mixed solution after decompression is sent to the lightness-removing tower for separation, the trichlorosilane is obtained at the top of the lightness-removing tower, and the high-purity silicon tetrachloride product with the mass fraction of more than 99.9999% is obtained at the tower bottom.
In order to solve the technical problems, the invention adopts the following technical scheme: the silicon tetrachloride impurity removal method is characterized by comprising the following steps of:
s1, introducing crude silicon tetrachloride into a dedusting tower, and dedusting under the conditions that the operating pressure at the top of the dedusting tower is 1bar and the operating temperature at the top of the dedusting tower is 65-85 ℃, wherein high-boiling 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 step S1 through a shielding pump, and then introducing the pressurized liquid phase product into a membrane separator for impurity removal to obtain a high-pressure chlorosilane mixed solution; 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 solution obtained in the S2 into a light component removal tower for rectification, wherein the operating pressure at the top of the light component removal tower is 1bar, and the operating temperature at the top of the tower is 35-55 ℃; and the trichlorosilane is discharged from the top of the light component removal tower, and the high-purity silicon tetrachloride with the mass fraction of more than 99.9999% 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, silicon trichloride, boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and iron trichloride.
Preferably, the outlet pressure of the shielding pump in the step S2 is 1MPa to 6MPa.
Preferably, the membrane in the membrane separator in the S2 adopts an organic high molecular reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic high molecular reverse osmosis membrane is a trimesoyl chloride-polyether sulfone membrane.
Preferably, the high-pressure chlorosilane mixed solution in the step S2 comprises silicon tetrachloride and trichlorosilane.
Preferably, the theoretical plate number of the light component removing tower in the step S3 is 60-80, and the reflux ratio is 3-5.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, by arranging the membrane separator, other chlorides are separated from chlorosilane by utilizing the organic polymer reverse osmosis membrane, so that 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. According to the invention, the membrane separation and the rectification are combined, only two rectification towers are adopted, and compared with the traditional method for removing the silicon tetrachloride impurity by singly adopting the rectification, the two rectification towers are saved, and the purpose of energy saving is realized.
3. The time for replacing the film is far less than the time for regenerating the adsorbent or drying the plasma, so that the production period is effectively prolonged, and the impurity removal cost per unit silicon tetrachloride is effectively reduced.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a schematic flow chart of the silicon tetrachloride impurity removal method.
Reference numerals illustrate:
1-crude silicon tetrafluoride; 2-high boiling substances and silicon powder; 3-liquid phase product; 4-high pressure liquid phase product; 5-high-pressure chlorosilane mixed solution; 6-chlorosilane mixed solution; 7-trichlorosilane; 8-high purity silicon tetrafluoride; t101-a dust removal tower; p101-a canned motor pump; m101-a membrane separator; h101-buffer tank; t102-a light component removing tower.
Detailed Description
The crude silicon tetrachloride used in examples 1-3 consisted of: the mass fraction of silicon tetrachloride is 85%, the mass fraction of trichlorosilane is 13%, the total mass fraction of high-boiling substances and silicon powder is 1%, and the total mass fraction of boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride is 1%.
Example 1
The silicon tetrachloride impurity removal method of the embodiment comprises the following steps:
s1, introducing crude silicon tetrachloride 1 with the total mass flow rate of 100.00kg/h into the bottom of a dedusting tower T101, and dedusting under the conditions that the operating pressure at the top of the dedusting tower T101 is 1bar, the operating temperature at the top of the dedusting tower T101 is 65 ℃, the theoretical plate number is 45 and the reflux ratio is 1, wherein the bottom of the dedusting tower T101 is provided with high-boiling substances and silicon powder 2 with the mass flow rate of 1.2kg/h, and the top of the dedusting tower is provided with a liquid-phase product 3 with the mass flow rate of 98.80 kg/h;
the liquid phase product 3 comprises silicon tetrachloride, silicon trichloride, 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 substances and silicon powder is less than 1ppm;
s2, introducing the liquid phase product 3 obtained in the step 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 rate of 98.80kg/h into a membrane separator M101 under the condition that the outlet pressure of a shielding pump P101 is 6MPa to remove impurities, so as to obtain a high-pressure chlorosilane mixed solution 5 with the mass flow rate of 97.65 kg/h; introducing the high-pressure chlorosilane mixed solution 5 into a buffer tank H101 which is depressurized 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 high molecular reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic high molecular reverse osmosis membrane is a trimesoyl chloride-polyethersulfone membrane; the high-pressure chlorosilane mixed solution 5 contains 86.74% of silicon tetrachloride, 13.25% of trichlorosilane, 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 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 operating pressure at the top of the light component removal tower T102 is 1bar, the operating temperature at the top of the tower is 35 ℃, the theoretical plate number is 60, and the reflux ratio is 3; trichlorosilane 7 with the mass flow rate of 12.97kg/h is discharged from the top of the light component removal tower T102, and high-purity silicon tetrachloride 8 with the mass flow rate of 84.68kg/h is obtained from the tower kettle;
through detection, the content of silicon tetrachloride in the high-purity silicon tetrachloride 8 is 99.99996%, the content of 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 substances and silicon powder is less than 1ppm.
Example 2
The silicon tetrachloride impurity removal method of the embodiment comprises the following steps:
s1, introducing crude silicon tetrachloride 1 with the total mass flow rate of 100.00kg/h into the bottom of a dedusting tower T101, and dedusting under the conditions that the operating pressure at the top of the dedusting tower T101 is 1bar, the operating temperature at the top of the dedusting tower T101 is 85 ℃, the theoretical plate number is 65 and the reflux ratio is 5, wherein the bottom of the dedusting tower T101 is provided with high-boiling substances and silicon powder 2 with the mass flow rate of 1.05kg/h, and the top of the dedusting tower is provided with a liquid-phase product 3 with the mass flow rate of 98.95 kg/h;
the liquid phase product 3 comprises silicon tetrachloride, silicon trichloride, 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 substances and silicon powder is less than 1ppm;
s2, introducing the liquid phase product 3 obtained in the step 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 rate of 98.95kg/h into a membrane separator M101 under the condition that the outlet pressure of a shielding pump P101 is 1MPa to remove impurities, so as to obtain a high-pressure chlorosilane mixed solution 5 with the mass flow rate of 97.60 kg/h; introducing the high-pressure chlorosilane mixed solution 5 into a buffer tank H101 which is depressurized 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 adopts an organic high molecular reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic high molecular reverse osmosis membrane is a trimesoyl chloride-polyethersulfone membrane; the high-pressure chlorosilane mixed solution 5 contains 86.78% of silicon tetrachloride, 13.21% of trichlorosilane, and 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 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 operating pressure of the top of the light component removal tower T102 is 1bar, the operating temperature of the top of the tower is 55 ℃, the theoretical plate number is 80, and the reflux ratio is 5; trichlorosilane 7 with the mass flow rate of 13.32kg/h is discharged from the top of the light component removal tower T102, and high-purity silicon tetrachloride 8 with the mass flow rate of 84.28kg/h is obtained from the tower kettle;
through detection, the content of silicon tetrachloride in the high-purity silicon tetrachloride 8 is 99.99999%, the content of 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 substances and silicon powder is less than 1ppm.
Example 3
The silicon tetrachloride impurity removal method of the embodiment comprises the following steps:
s1, introducing crude silicon tetrachloride 1 with the total mass flow rate of 100.00kg/h into the bottom of a dedusting tower T101, and dedusting under the conditions that the operating pressure at the top of the dedusting tower T101 is 1bar, the operating temperature at the top of the dedusting tower T101 is 75 ℃, the theoretical plate number is 55 and the reflux ratio is 3, wherein the bottom of the dedusting tower T101 is provided with high-boiling substances and silicon powder 2 with the mass flow rate of 1.13kg/h, and the top of the dedusting tower is provided with a liquid-phase product 3 with the mass flow rate of 98.87 kg/h;
the liquid phase product 3 comprises silicon tetrachloride, silicon trichloride, 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 substances and silicon powder is less than 1ppm;
s2, introducing the liquid phase product 3 obtained in the step 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 rate of 98.87kg/h into a membrane separator M101 under the condition that the outlet pressure of a shielding pump P101 is 3MPa to remove impurities, so as to obtain a high-pressure chlorosilane mixed solution 5 with the mass flow rate of 97.62 kg/h; introducing the high-pressure chlorosilane mixed solution 5 into a buffer tank H101 which is depressurized 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 adopts an organic high molecular reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic high molecular reverse osmosis membrane is a trimesoyl chloride-polyethersulfone membrane; the high-pressure chlorosilane mixed solution 5 contains 86.77% of silicon tetrachloride, 13.22% of trichlorosilane, and 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 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 operating pressure of the top of the light component removal tower T102 is 1bar, the operating temperature of the top of the tower is 45 ℃, the theoretical plate number is 70, and the reflux ratio is 4; trichlorosilane 7 with the mass flow rate of 13.07kg/h is discharged from the top of the light component removal tower T102, and high-purity silicon tetrachloride 8 with the mass flow rate of 84.55kg/h is obtained from the tower kettle;
through detection, the content of silicon tetrachloride in the high-purity silicon tetrachloride 8 is 99.99998%, the content of 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 substances and silicon powder is less than 1ppm.
In examples 1-3, the content of each component is represented by mass fraction; in the embodiments 1-3, the device used in the silicon tetrachloride impurity removal method 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 connected in series in sequence; the top of the dedusting tower T101 is provided with a condenser.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (3)
1. The silicon tetrachloride impurity removal method is characterized by comprising the following steps of:
s1, introducing crude silicon tetrachloride into a dedusting tower, and dedusting under the conditions that the operating pressure at the top of the dedusting tower is 1bar and the operating temperature at the top of the dedusting tower is 65-85 ℃, wherein high-boiling 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;
the crude silicon tetrachloride comprises silicon tetrachloride, trichlorosilane, high-boiling residues, silicon powder, boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride; the liquid phase product comprises silicon tetrachloride, silicon trichloride, boron trichloride, phosphorus trichloride, titanium tetrachloride, aluminum trichloride and ferric trichloride;
s2, pressurizing the liquid phase product obtained in the step S1 through a shielding pump, and then introducing the pressurized liquid phase product into a membrane separator for impurity removal to obtain a high-pressure chlorosilane mixed solution; introducing the high-pressure chlorosilane mixed solution into a buffer tank which is depressurized to 1bar to obtain a chlorosilane mixed solution;
the high-pressure chlorosilane mixed solution comprises silicon tetrachloride and trichlorosilane; the outlet pressure of the shielding pump is 1 MPa-6 MPa; the membrane in the membrane separator adopts an organic high molecular reverse osmosis membrane which does not react with silicon tetrachloride and trichlorosilane, and the organic high molecular reverse osmosis membrane is a trimesoyl chloride-polyether sulfone membrane;
s3, introducing the chlorosilane mixed solution obtained in the S2 into a light component removal tower for rectification, wherein the operating pressure at the top of the light component removal tower is 1bar, and the operating temperature at the top of the tower is 35-55 ℃; and the trichlorosilane is discharged from the top of the light component removal tower, and the high-purity silicon tetrachloride with the mass fraction of more than 99.9999% is obtained from the tower bottom.
2. The method for removing impurities from silicon tetrachloride according to claim 1, wherein the theoretical plate number of the dust removing tower in S1 is 45-65, and the reflux ratio is 1-5.
3. The method for removing impurities from silicon tetrachloride according to claim 1, wherein the theoretical plate number of the lightness-removing column in S3 is 60-80, and the reflux ratio is 3-5.
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