A silicon tetrachloride purification process and system
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A technology of silicon tetrachloride and process, applied in the direction of silicon halide compound, halosilane, etc., can solve the problems of poor purification effect and so on
Active Publication Date: 2016-01-06
ZHEJIANG FUSHITE GROUP
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[0010] The invention provides a silicon tetrachloride purification process to solve the problem of poor purification effect in the existing process
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Embodiment 1
[0038] A fixed bed reactor is adopted, the reaction temperature is controlled at 300°C, 350°C, 400°C, 450°C, 500°C, the gas residence time is 30s, the particle size of activated alumina is 3-5mm, and the average specific surface area is 340m 2 / g, the particle size of active silica gel is 75~150μm, and the average specific surface area is 400m 2 / g, the reflux ratio of the first rectifying tower is 10: 1, the reflux ratio of the second rectifying tower is 20: 1, the tower top temperature is controlled at 56~58 ℃, and the tower bottom temperature is controlled at 70~72 ℃.
Embodiment 2
[0040] Adopt two-stage fixed-bed reactor, the temperature of the first section fixed-bed reactor is 300 ℃, the residence time 10s, the temperature of the second section fixed-bed reactor is 400 ℃, the residence time 20s, all the other parameters are the same as embodiment 1.
Embodiment 3
[0042] Two-stage fixed-bed reactors were adopted, the temperature of the first fixed-bed reactor was 350° C., and the residence time was 15 seconds. The temperature of the second-stage fixed-bed reactor was 450° C., and the residence time was 25 seconds.
[0045] It can be seen from the above table that the purification efficiency of the two-stage fixed-bed reactor is significantly higher than that of the one-stage fixed-bed reactor, which may be because the residence time in the one-stage fixed-bed reactor is too long, resulting in local temperature changes and reduced impurity conversion efficiency.
[0046] In the one-stage reactor, the reaction temperature of 500°C has the best impurity removal effect, indicating that the impurity and chlorine react most fully at this temperature.
[0047] In Example 3, the reaction temperature is reduced and the gas residence time is prolonged, but the impur...
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Abstract
The invention discloses a silicon tetrachloride purifying process and system. The silicon tetrachloride purifying process comprises the following steps: (1), in the presence of a catalyst, making vaporized crude silicon tetrachloride react with chlorine under the protection of nitrogen, condensing a reactant after the reaction is ended to ensure that the silicon tetrachloride is liquefied; and (2), sequentially performing active Al2O3 adsorption, first-time rectification, active silicon gel adsorption, second-time rectification on a liquid phase obtained through condensation to obtain the silicon tetrachloride with a purity of more than 99.99999 percent. The silicon tetrachloride purifying system comprises a vaporizer, a fixed bed reactor, a gas-liquid separator, an active aluminum oxide adsorbing column, a first-stage rectifying tower, an active silicon gel adsorbing column and a second-stage rectifying tower which are sequentially connected. According to the silicon tetrachloride purifying process and system provided by the invention, chlorine is used for reacting with a hydrogen-containing compound in the crude silicon tetrachloride, after gas and liquid are separated, chloride in the crude silicon tetrachloride is removed by using adsorption and rectification which are alternatively set, and the purity of the silicon tetrachloride can reach above 99.99999 percent.
Description
technical field [0001] The invention relates to the technical field of purification of high-purity compounds, in particular to a silicon tetrachloride purification process and system. Background technique [0002] Silicon tetrachloride (SiliconTetrachloride, SiCl 4 ), is the simplest compound of chlorine and silicon, molecular weight: 160.9, melting point -70°C, boiling point 56.8°C. Industrial Grade SiCl 4 It is a colorless transparent smoky liquid at room temperature, has a suffocating irritating smell, reacts violently with water and decomposes into silicic acid and hydrochloric acid; it can be miscible with benzene, ether, chloroform and petroleum ether, and is highly corrosive . [0003] At present, the source of silicon tetrachloride is mainly the by-product of polysilicon, the by-product silicon tetrachloride during the production and disproportionation of trichlorosilane. The crude silicon tetrachloride products provided by these two sources all contain certain t...
Claims
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