CN102557043A - Method for preparing silicon tetrafluoride and anhydrous hydrogen fluoride by taking sodium fluorosilicate as raw material - Google Patents
Method for preparing silicon tetrafluoride and anhydrous hydrogen fluoride by taking sodium fluorosilicate as raw material Download PDFInfo
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- CN102557043A CN102557043A CN201110446235XA CN201110446235A CN102557043A CN 102557043 A CN102557043 A CN 102557043A CN 201110446235X A CN201110446235X A CN 201110446235XA CN 201110446235 A CN201110446235 A CN 201110446235A CN 102557043 A CN102557043 A CN 102557043A
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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
The present invention relates to the fluorine chemical technical field, especially relating to a kind of is the method for feedstock production silicon tetrafluoride and anhydrous hydrogen fluoride with the Sodium Silicofluoride 98min.
Background technology
Silicon tetrafluoride is employed a kind of electronics special gas in semi-conductor and the optical fiber processed and applied, is a kind of important component in the ion implantation that adopts of silicon-based semiconductor devices manufacturing.Silicon tetrafluoride will have wide practical use at microelectronic industry.Anhydrous hydrogen fluoride (AHF) is widely used in industries such as nuclear power, chemical industry, oil, is strong oxidizer, is the basic raw material of producing element fluorine, various fluorinated refrigerant, inorganic fluoride and organic fluoride.
The method (application number is 201010504248.3) that the Chinese patent name is called sulfuric acid acidation preparation with sodium fluosilicate silicon tetrafluoride and anhydrous hydrogen fluoride discloses and has a kind ofly prepared the method for silicon tetrafluoride and anhydrous hydrogen fluoride by Sodium Silicofluoride 98min and sulfuric acid reaction, and this process step is that a. Sodium Silicofluoride 98min and excess sulfuric acid obtain silicon tetrafluoride gas hydrogen fluoride at stirring reaction below 150 ℃ and stay in the solid residue; B. the silicon tetrafluoride gas that produces of step a obtains high-purity silicon tetrafluoride gas through dedusting, cooling, drying, refining, compression; C. continue to be warming up to 200 ℃, hydrogen fluoride gas is overflowed; D. the step c hydrogen fluoride gas of overflowing obtains the anhydrous hydrogen fluoride gas Sodium Silicofluoride 98min through dedusting, cooling, drying, refining, compression; Have and make the Sodium Silicofluoride 98min low value-added, that generate for processing of waste of phosphate fertilizer industry by-product obtain comprehensive utilization; Fluorine, element silicon are changed into have high added value, broad-spectrum silicon tetrafluoride and anhydrous hydrogen fluoride, but there is following shortcoming in above-mentioned technological process:
(1) reacted excess sulfuric acid is prone to equipment is caused corrosion among the step a; (2) silicon tetrafluoride gas realizes overflowing respectively to reach separating through control reaction temperature with hydrogen fluoride gas; Because there is complicated suction exothermic process in reaction process; It is very big that temperature is accurately controlled difficulty, therefore only depends on control reaction temperature to realize separating, and purity is not high; (3) generate SiHF on Sodium Silicofluoride 98min and the excess sulfuric acid reaction theory
5, again by SiHF
5Easy decomposes is SiF
4And HF, therefore only depend on control reaction temperature to realize separating, difficulty is bigger; (4) in detail openly silicon tetrafluoride and hydrofluoric dedusting of said process, cooling, drying, refining, the detailed process compressed.
Summary of the invention
Technical problem to be solved by this invention provides a kind of can the minimizing significantly corrosion on Equipment, and the silicon tetrafluoride that obtains and hydrogen fluoride product purity are high, energy-conserving and environment-protective be the method for feedstock production silicon tetrafluoride and anhydrous hydrogen fluoride with the Sodium Silicofluoride 98min.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of is the method for feedstock production silicon tetrafluoride and anhydrous hydrogen fluoride with the Sodium Silicofluoride 98min, comprises the steps:
(1) the Sodium Silicofluoride 98min solid is dewatered through the moisture eliminator drying, the mass percent of moisture is lower than 1wt% in the Sodium Silicofluoride 98min solid, and the water vapor that drying is come out is sent into the sodium hydroxide solution cooling and absorbing of soda-wash tower with 30wt%;
(2) with in the 1:1 adding in molar ratio of the sulfuric acid in the sulfuric acid of dried Sodium Silicofluoride 98min solid and the 100～104wt% rotary kiln reactor drum; Under the condition that Sodium Silicofluoride 98min in the described rotary kiln reactor drum and sulfuric acid mixture material in temperature are 160～220 ℃; Behind reaction 30～180min, generate sodium sulfate solid and silicon tetrafluoride and hydrogen fluoride mixed gas;
(3) with silicon tetrafluoride and hydrogen fluoride mixed gas from the rotary kiln reactor head discharge send into the gas mixture washing tower and remove solid dust and water vapor after; Send into compressor pressurizes to 0.5～1.5MPaG; Be pre-chilled to-20～-30 ℃ through condensing surface again, wherein the washings of gas mixture washing tower is the sulfuric acid of 98wt%;
(4) after the overhead product interchanger through rectifying tower is cooled to-25～-35 ℃ earlier with the silicon tetrafluoride after the precooling and hydrogen fluoride mixed gas; Sending into rectifying tower separates; Controlling described rectifying tower working pressure is 0.6～0.75MPaG; The overhead condensation actuator temperature of controlling described rectifying tower is-80～-70 ℃, and extraction purity is the anhydrous hydrogen fluoride of 99.95wt% at the bottom of the tower of rectifying tower, delivers to the anhydrous hydrogen fluoride storage tank stores after the cold water cooler of process is cooled to 10～15 ℃;
(5) described silicon tetrafluoride from the cat head of rectifying tower with the liquid form extraction; The liquid silicon tetrafluoride of extraction is the decompression vaporization after the overhead product interchanger of rectifying tower reclaims cold, sends into the silicon tetrafluoride washing tower, behind the micro-hydrogen fluoride and water that exists in the absorption silicon tetrafluoride gas; Obtain the silicon tetrafluoride gas that purity is 99.5wt%; After the pressurization cooling, send into the silicon tetrafluoride storage tank again, wherein the washings of silicon tetrafluoride washing tower is the sulfuric acid of 98wt%.
The outer wall of described rotary kiln reactor drum is provided with chuck, is provided with 300～500 ℃ of stack gases that are used to heat in the described chuck.
The sulfuric acid that described gas mixture washing tower and described silicon tetrafluoride washing tower are discharged adds after an amount of sulphur trioxide is configured to sulfuric acid that concentration is 100-104wt%, sends into the rotary kiln reactor drum as reaction raw materials.
Reaction formula of the present invention is following:
Compared with prior art, the invention has the advantages that:
(1) solid Sodium Silicofluoride 98min and fluid sulphuric acid reaction process adopt the rotary kiln reactor drum; Can realize liquid, solid biphase thorough mixing, make reaction more abundant, reaction efficiency is high; The rotary kiln reactor drum is the overcoat heating-type simultaneously; Overcoat adopts 300～500 ℃ of stack gas heating, and heating efficiency is high, and energy-saving effect is remarkable;
(2) adopt the sulfuric acid scrubbing tower to carry out wet dedusting, efficiency of dust collection is high, and sulfuric acid or water-retaining agent can be removed the water that raw material is brought reactive system into simultaneously, avoids having the equipment corrosion that produces because of water; Sulfuric acid after dedusting and suction directly uses as raw material, does not produce the three wastes;
(3) through selecting suitable rectifying tower working pressure and service temperature, make silicon tetrafluoride and hydrogen fluoride realize separating more efficiently, obtain more highly purified silicon tetrafluoride and anhydrous hydrogen fluoride simultaneously;
(4) reaction raw materials employing concentration is the sulfuric acid of 100-104wt%, and can guarantee does not have water in the reaction process, thereby has avoided corrosion on Equipment; Facility investment and working cost reduce significantly;
(5) compare with the method (application number is 201010504248.3) of Chinese patent sulfuric acid acidation preparation with sodium fluosilicate silicon tetrafluoride and anhydrous hydrogen fluoride; In Sodium Silicofluoride 98min of the present invention and the vitriolic reaction process; The 1:1 reaction in molar ratio of Sodium Silicofluoride 98min and sulfuric acid; Reaction can normally be carried out, avoided the complicacy of excess sulfuric acid simultaneously corrosion on Equipment and subsequent disposal.
Description of drawings
Fig. 1 is a processing unit schema of the present invention.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
With embodiment the present invention is described further below, but protection scope of the present invention is not limited to this, protection domain is as the criterion with claim.
Embodiment 1
The present invention is a kind of to be the method for feedstock production silicon tetrafluoride and anhydrous hydrogen fluoride with the Sodium Silicofluoride 98min, as shown in Figure 1 comprising the steps:
(1) the Sodium Silicofluoride 98min solid is dewatered through moisture eliminator 1 drying, the mass percent of moisture is lower than 1wt% in the Sodium Silicofluoride 98min solid, and the water vapor that drying is come out is sent into the sodium hydroxide solution cooling and absorbing of soda-wash tower 2 usefulness 30wt%;
(2) with in sulfuric acid in the sulfuric acid of 100～104wt% and the dried Sodium Silicofluoride 98min solid 1:1 adding in molar ratio rotary kiln reactor drum 3; Under the condition that Sodium Silicofluoride 98min in the control rotary kiln reactor drum 3 and sulfuric acid mixture material in temperature are 160～220 ℃; Behind reaction 30～180min, generate sodium sulfate solid and silicon tetrafluoride and hydrogen fluoride mixed gas;
(3) with silicon tetrafluoride and hydrogen fluoride mixed gas from rotary kiln reactor drum 3 tops discharge send into gas mixture washing tower 4 and remove solid dust and water vapor after; Send into compressor 5 and be pressurized to 0.5MPaG; Be pre-chilled to-20 ℃ through condensing surface 6 again, wherein the washings of gas mixture washing tower 4 is the sulfuric acid of 98wt%;
(4) after the overhead product interchanger 8 through rectifying tower 7 is cooled to-25 ℃ earlier with the silicon tetrafluoride after the precooling and hydrogen fluoride mixed gas; Sending into rectifying tower 7 separates; Controlling these rectifying tower 7 working pressures is 0.6MPaG; The overhead condenser (not shown) temperature of control rectifying tower 7 is-70 ℃, and extraction purity is the anhydrous hydrogen fluoride of 99.95wt% at the bottom of the tower of rectifying tower 7, delivers to anhydrous hydrogen fluoride storage tank stores 10 after the cold water cooler 9 of process is cooled to 10 ℃;
(5) above-mentioned silicon tetrafluoride from the cat head of rectifying tower 7 with the liquid form extraction; The liquid silicon tetrafluoride of extraction through valve decompression vaporization, is sent into silicon tetrafluoride washing tower 11 after the overhead product interchanger 8 of rectifying tower 7 reclaims cold, behind the micro-hydrogen fluoride and water that exists in the absorption silicon tetrafluoride gas; Obtain the silicon tetrafluoride gas that purity is 99.5wt%; After the pressurization cooling, send into silicon tetrafluoride storage tank 12 again, wherein the washings of silicon tetrafluoride washing tower 11 is the sulfuric acid of 98wt%.
In this specific embodiment, the outer wall of rotary kiln reactor drum 3 is provided with chuck, is provided with 300～500 ℃ of stack gases that are used to heat in the described chuck; The sulfuric acid of discharging with silicon tetrafluoride washing tower 11 of gas mixture washing tower 4 adds after an amount of sulphur trioxides are configured to sulfuric acid that concentration is 100-104wt%, sends into rotary kiln reactor drum 3 as reaction raw materials.
With embodiment 1; Its difference is: in the step (3) with silicon tetrafluoride and hydrogen fluoride mixed gas from rotary kiln reactor drum 3 tops discharge send into gas mixture washing tower 4 and remove solid dust and water vapor after; Send into compressor 5 and be pressurized to 1.0MPaG; Be pre-chilled to-25 ℃ through condensing surface 6 again, wherein the washings of gas mixture washing tower 4 is the sulfuric acid of 98wt%; In the step (4) with the silicon tetrafluoride after the precooling and hydrogen fluoride mixed gas after the overhead product interchanger 8 through rectifying tower 7 is cooled to-30 ℃ earlier; Sending into rectifying tower 7 separates; Controlling these rectifying tower 7 working pressures is 0.7MPaG; The overhead condenser (not shown) temperature of control rectifying tower 7 is-75 ℃, and extraction purity is the anhydrous hydrogen fluoride of 99.95wt% at the bottom of the tower of rectifying tower 7, delivers to anhydrous hydrogen fluoride storage tank stores 10 after the cold water cooler 9 of process is cooled to 12 ℃.
With embodiment 1; Its difference is: in the step (3) with silicon tetrafluoride and hydrogen fluoride mixed gas from rotary kiln reactor drum 3 tops discharge send into gas mixture washing tower 4 and remove solid dust and water vapor after; Send into compressor 5 and be pressurized to 1.5MPaG; Be pre-chilled to-30 ℃ through condensing surface 6 again, wherein the washings of gas mixture washing tower 4 is the sulfuric acid of 98wt%;
In the step (4) with the silicon tetrafluoride after the precooling and hydrogen fluoride mixed gas after the overhead product interchanger 8 through rectifying tower 7 is cooled to-35 ℃ earlier; Sending into rectifying tower 7 separates; Controlling these rectifying tower 7 working pressures is 0.75MPaG; The overhead condenser (not shown) temperature of control rectifying tower 7 is-80 ℃, and extraction purity is the anhydrous hydrogen fluoride of 99.95wt% at the bottom of the tower of rectifying tower 7, delivers to anhydrous hydrogen fluoride storage tank stores 10 after the cold water cooler 9 of process is cooled to 15 ℃.
Claims (3)
1. one kind is the method for feedstock production silicon tetrafluoride and anhydrous hydrogen fluoride with the Sodium Silicofluoride 98min, it is characterized in that comprising the steps:
(1) the Sodium Silicofluoride 98min solid is dewatered through the moisture eliminator drying, the mass percent of moisture is lower than 1wt% in the Sodium Silicofluoride 98min solid, and the water vapor that drying is come out is sent into the sodium hydroxide solution cooling and absorbing of soda-wash tower with 30wt%;
(2) with in the 1:1 adding in molar ratio of the sulfuric acid in the sulfuric acid of dried Sodium Silicofluoride 98min solid and the 100～104wt% rotary kiln reactor drum; Under the condition that Sodium Silicofluoride 98min in the described rotary kiln reactor drum and sulfuric acid mixture material in temperature are 160～220 ℃; Behind reaction 30～180min, generate sodium sulfate solid and silicon tetrafluoride and hydrogen fluoride mixed gas;
(3) with silicon tetrafluoride and hydrogen fluoride mixed gas from the rotary kiln reactor head discharge send into the gas mixture washing tower and remove solid dust and water vapor after; Send into compressor pressurizes to 0.5～1.5MPaG; Be pre-chilled to-20～-30 ℃ through condensing surface again, wherein the washings of gas mixture washing tower is the sulfuric acid of 98wt%;
(4) after the overhead product interchanger through rectifying tower is cooled to-25～-35 ℃ earlier with the silicon tetrafluoride after the precooling and hydrogen fluoride mixed gas; Sending into rectifying tower separates; Controlling described rectifying tower working pressure is 0.6～0.75MPaG; The overhead condensation actuator temperature of controlling described rectifying tower is-80～-70 ℃, and extraction purity is the anhydrous hydrogen fluoride of 99.95wt% at the bottom of the tower of rectifying tower, delivers to the anhydrous hydrogen fluoride storage tank stores after the cold water cooler of process is cooled to 10～15 ℃;
(5) described silicon tetrafluoride from the cat head of rectifying tower with the liquid form extraction; The liquid silicon tetrafluoride of extraction is the decompression vaporization after the overhead product interchanger of rectifying tower reclaims cold, sends into the silicon tetrafluoride washing tower, behind the micro-hydrogen fluoride and water that exists in the absorption silicon tetrafluoride gas; Obtain the silicon tetrafluoride gas that purity is 99.5wt%; After the pressurization cooling, send into the silicon tetrafluoride storage tank again, wherein the washings of silicon tetrafluoride washing tower is the sulfuric acid of 98wt%.
2. according to claim 1 a kind of be the method for feedstock production silicon tetrafluoride and anhydrous hydrogen fluoride with the Sodium Silicofluoride 98min; It is characterized in that: the outer wall of described rotary kiln reactor drum is provided with chuck, is provided with 300～500 ℃ of stack gases that are used to heat in the described chuck.
3. according to claim 1 a kind of be the method for feedstock production silicon tetrafluoride and anhydrous hydrogen fluoride with the Sodium Silicofluoride 98min; It is characterized in that: the sulfuric acid that described gas mixture washing tower and described silicon tetrafluoride washing tower are discharged adds after an amount of sulphur trioxide is configured to sulfuric acid that concentration is 100-104wt%, sends into the rotary kiln reactor drum as reaction raw materials.
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Cited By (10)
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| CN103043613A (en) * | 2013-01-17 | 2013-04-17 | 昆明道尔森科技有限公司 | Preparation method of fluoride |
| CN103754825A (en) * | 2014-01-22 | 2014-04-30 | 瓮福（集团）有限责任公司 | Preparation method of anhydrous hydrogen fluoride |
| CN104671210A (en) * | 2014-12-11 | 2015-06-03 | 云南天安化工有限公司 | Direct separation method of silicon tetrafluoride and anhydrous hydrogen fluoride mixed gas |
| CN107082407A (en) * | 2017-06-22 | 2017-08-22 | 多氟多化工股份有限公司 | A kind of method of purification of anhydrous hydrofluoric acid |
| CN107188129A (en) * | 2017-07-24 | 2017-09-22 | 衢州市鼎盛化工科技有限公司 | The method that calcium fluoride containing waste material prepares hydrogen fluoride and ocratation |
| CN108658081A (en) * | 2018-08-02 | 2018-10-16 | 浙江中宁硅业有限公司 | The method and its production equipment of ocratation are produced using prodan as raw material |
| CN108862201A (en) * | 2018-09-12 | 2018-11-23 | 浙江大学 | A method of hydrogen fluoride is prepared using prodan |
| CN112897466A (en) * | 2020-10-27 | 2021-06-04 | 贵州省化工研究院 | Method for producing anhydrous hydrogen fluoride by using fluosilicic acid in phosphoric acid |
| CN113233422A (en) * | 2021-06-02 | 2021-08-10 | 四川大学 | Method and system for separating SiF4 and HF mixed gas |
| CN113816340A (en) * | 2021-10-13 | 2021-12-21 | 中国科学院过程工程研究所 | Method for preparing anhydrous hydrogen fluoride and co-producing silicon tetrafluoride from sodium fluosilicate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103043613B (en) * | 2013-01-17 | 2014-09-24 | 昆明道尔森科技有限公司 | Preparation method of fluoride |
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| CN103754825A (en) * | 2014-01-22 | 2014-04-30 | 瓮福（集团）有限责任公司 | Preparation method of anhydrous hydrogen fluoride |
| CN104671210A (en) * | 2014-12-11 | 2015-06-03 | 云南天安化工有限公司 | Direct separation method of silicon tetrafluoride and anhydrous hydrogen fluoride mixed gas |
| CN107082407B (en) * | 2017-06-22 | 2019-01-25 | 多氟多化工股份有限公司 | A kind of method of purification of anhydrous hydrofluoric acid |
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| CN107188129A (en) * | 2017-07-24 | 2017-09-22 | 衢州市鼎盛化工科技有限公司 | The method that calcium fluoride containing waste material prepares hydrogen fluoride and ocratation |
| CN108658081A (en) * | 2018-08-02 | 2018-10-16 | 浙江中宁硅业有限公司 | The method and its production equipment of ocratation are produced using prodan as raw material |
| CN108658081B (en) * | 2018-08-02 | 2023-08-22 | 浙江中宁硅业有限公司 | Method for producing silicon tetrafluoride by using sodium fluosilicate as raw material and production equipment thereof |
| CN108862201A (en) * | 2018-09-12 | 2018-11-23 | 浙江大学 | A method of hydrogen fluoride is prepared using prodan |
| CN112897466A (en) * | 2020-10-27 | 2021-06-04 | 贵州省化工研究院 | Method for producing anhydrous hydrogen fluoride by using fluosilicic acid in phosphoric acid |
| CN113233422A (en) * | 2021-06-02 | 2021-08-10 | 四川大学 | Method and system for separating SiF4 and HF mixed gas |
| CN113233422B (en) * | 2021-06-02 | 2023-03-31 | 四川大学 | Method and system for separating SiF4 and HF mixed gas |
| CN113816340A (en) * | 2021-10-13 | 2021-12-21 | 中国科学院过程工程研究所 | Method for preparing anhydrous hydrogen fluoride and co-producing silicon tetrafluoride from sodium fluosilicate |
| CN113816340B (en) * | 2021-10-13 | 2024-01-30 | 中国科学院过程工程研究所 | Method for preparing anhydrous hydrogen fluoride and co-producing silicon tetrafluoride from sodium fluosilicate |
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