Method for preparing silicon tetrafluoride and anhydrous hydrogen fluoride by taking sodium fluorosilicate as raw material

A technology of anhydrous hydrogen fluoride and silicon tetrafluoride, which is applied in the directions of fluorine/hydrogen fluoride, halogenated silicon compounds, halogenated silanes, etc. Accurate temperature control is very difficult, hydrogen fluoride gas escapes, etc., to achieve significant energy saving, avoid equipment corrosion, and fully react

Inactive Publication Date: 2012-07-11
SEDIN NINGBO ENG
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] The Chinese patent name is the method of preparing silicon tetrafluoride and anhydrous hydrogen fluoride by acidifying sodium fluorosilicate with sulfuric acid (application number is 201010504248.3) which discloses a A method for preparing silicon tetrafluoride and anhydrous hydrogen fluoride by reacting sodium with sulfuric acid, the process steps are: a. Sodium fluorosilicate and excess sulfuric acid are stirred and reacted below 150°C to obtain silicon tetrafluoride gas and hydrogen fluoride remaining in the solid residue; b. The silicon tetrafluoride gas produced in step a is dedusted, cooled, dried, refined, and compressed to obtain high-purity silicon tetrafluoride gas; c. continue to heat up to 200 ° C, hydrogen fluoride gas escapes; d. hydrogen fluoride gas escapes in step c After dedusting, cooling, drying, refining, and compression, anhydrous hydrogen fluoride gas sodium fluorosilicate is obtained, which has low added value as a by-product of the phosphate fertilizer industry. The sodium fluorosilicate produced for waste treatment has been comprehensively utilized to make fluorine, silicon

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  • Method for preparing silicon tetrafluoride and anhydrous hydrogen fluoride by taking sodium fluorosilicate as raw material
  • Method for preparing silicon tetrafluoride and anhydrous hydrogen fluoride by taking sodium fluorosilicate as raw material
  • Method for preparing silicon tetrafluoride and anhydrous hydrogen fluoride by taking sodium fluorosilicate as raw material

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Embodiment 1

[0026] A kind of method that the present invention prepares silicon tetrafluoride and anhydrous hydrogen fluoride with sodium fluorosilicate as raw material, such as figure 1 Shown include the following steps:

[0027] (1) Dry the sodium fluorosilicate solid through the drier 1 to remove water until the mass percentage of water in the sodium fluorosilicate solid is lower than 1wt%, and send the dried water vapor into the alkali washing tower 2 with 30wt% hydrogen The sodium oxide solution is cooled and absorbed;

[0028] (2) Add sulfuric acid in 100-104wt% sulfuric acid to dried sodium fluorosilicate solid in a molar ratio of 1:1 into the rotary kiln reactor 3, and control the sodium fluorosilicate and sulfuric acid in the rotary kiln reactor 3 The mixed material is reacted at a temperature of 160-220°C for 30-180 minutes to generate sodium sulfate solid and a mixed gas of silicon tetrafluoride and hydrogen fluoride;

[0029] (3) The mixed gas of silicon tetrafluoride and hy...

Embodiment 2

[0034] Same as Example 1, the difference is that in step (3), the mixed gas of silicon tetrafluoride and hydrogen fluoride is discharged from the top of the rotary kiln reactor 3 and sent to the mixed gas scrubber 4 to remove solid dust and water vapor, and then sent to the compressor 5 pressurized to 1.0MPaG, and then pre-cooled to -25°C through the condenser 6, wherein the washing liquid of the mixed gas scrubber 4 is 98wt% sulfuric acid; in step (4), the pre-cooled silicon tetrafluoride and hydrogen fluoride The mixed gas is first cooled to -30°C through the tower top product heat exchanger 8 of the rectification tower 7, and then sent to the rectification tower 7 for separation. The operating pressure of the rectification tower 7 is controlled to be 0.7MPaG, and the pressure The temperature of the top condenser (not shown in the figure) is -75°C, and anhydrous hydrogen fluoride with a purity of 99.95wt% is extracted from the bottom of the rectification tower 7, which is coo...

Embodiment 3

[0036] Same as Example 1, the difference is that in step (3), the mixed gas of silicon tetrafluoride and hydrogen fluoride is discharged from the top of the rotary kiln reactor 3 and sent to the mixed gas scrubber 4 to remove solid dust and water vapor, and then sent to the compressor 5 pressurize to 1.5MPaG, and then pre-cool to -30°C through condenser 6, wherein the washing liquid of mixed gas scrubber 4 is 98wt% sulfuric acid;

[0037]In step (4), the pre-cooled silicon tetrafluoride and hydrogen fluoride mixed gas is first cooled to -35°C through the top product heat exchanger 8 of the rectification tower 7, and then sent to the rectification tower 7 for separation. The operating pressure of rectification tower 7 is 0.75MPaG, the temperature of the top condenser (not shown in the figure) of rectification tower 7 is controlled at -80°C, and anhydrous hydrogen fluoride with a purity of 99.95wt% is produced from the bottom of rectification tower 7 , sent to anhydrous hydrogen...

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Abstract

The invention discloses a method for preparing silicon tetrafluoride and anhydrous hydrogen fluoride by taking sodium fluorosilicate as a raw material. The method is characterized by comprising the following steps of: (1) drying sodium fluorosilicate for removing water; (2) adding the dried sodium fluorosilicate and sulfuric acid into a rotary kiln reactor in the molar ratio of 1:1, and reacting at the temperature of 160-220 DEG C for 30-180 minutes to generate a sodium sulfate solid and a mixed gas of silicon tetrafluoride and hydrogen fluoride; (3) dedusting, pressurizing and precooling to between 20 DEG C below zero and 30 DEG C below zero; (4) feeding the precooled mixed gas into a rectifying tower for separating, controlling the pressure of the rectifying tower at 0.6-0.75 MPaG and the temperature of tower top condenser between 70 DEG C below zero and 80 DEG C below zero, and discharging anhydrous hydrogen fluoride from the tower bottom; and (5) discharging silicon tetrafluoride from the tower top in the form of a liquid phase, decompressing, gasifying, dedusting and feeding into a silicon tetrafluoride washing tower to obtain silicon tetrafluoride gas. The method has the advantages that: corrosion to equipment can be reduced greatly, the obtained silicon tetrafluoride and hydrogen fluoride products have high purity, and the production process has low energy consumption and is environmentally-friendly.

Description

technical field [0001] The invention relates to the technical field of fluorine chemical industry, in particular to a method for preparing silicon tetrafluoride and anhydrous hydrogen fluoride by using sodium fluorosilicate as raw material. Background technique [0002] Silicon tetrafluoride is an electronic specialty gas used in semiconductor and optical fiber processing applications, and is an important component in the ion implantation method used in the manufacture of silicon-based semiconductor devices. Silicon tetrafluoride will have broad application prospects in the microelectronics industry. Anhydrous hydrogen fluoride (AHF) is widely used in atomic energy, chemical industry, petroleum and other industries. It is a strong oxidant and a basic raw material for the production of elemental fluorine, various fluorine refrigerants, inorganic fluorides and organic fluorides. [0003] The Chinese patent name is the method for preparing silicon tetrafluoride and anhydrous h...

Claims

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Application Information

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IPC IPC(8): C01B33/107C01B7/19
Inventor 苗延军谷新春梁正陈发辉胡晓铮
Owner SEDIN NINGBO ENG
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