CN103708470B - SiF 4preparation method - Google Patents

SiF 4preparation method Download PDF

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CN103708470B
CN103708470B CN201310711119.5A CN201310711119A CN103708470B CN 103708470 B CN103708470 B CN 103708470B CN 201310711119 A CN201310711119 A CN 201310711119A CN 103708470 B CN103708470 B CN 103708470B
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sif
gaseous state
preparation
gas
mixture
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CN103708470A (en
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李丹阳
刘瑞
龚亚云
林乐洪
章林
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GUIZHOU TIANHE GUORUN ADVANCED MATERIALS TECHNOLOGY CO., LTD.
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GUIZHOU TIANHE GUORUN ADVANCED MATERIALS TECHNOLOGY Co Ltd
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Abstract

The present invention relates to chemical field, in particular to a kind of SiF 4preparation method.SiF 4preparation method, comprise the following steps: siliceous mineral raw material or siliceous metal oxide are mixed with fluorochemical, obtains mixture; Described mixture is reacted, obtains gaseous state SiF 4.This SiF provided by the invention 4preparation method, its cost of material is cheap more many than traditional raw material (vitriol oil and Fluorspar Powder or anhydrous hydrofluoric acid), and then reduces SiF 4preparation cost.

Description

SiF 4preparation method
Technical field
The present invention relates to chemical field, in particular to a kind of SiF 4preparation method.
Background technology
Silicon tetrafluoride (SiF 4) be a kind of important basic chemical industry product, SiF 4can be used for the etching reagent of silicon nitride, tantalum silicide etc., P-type dopant, epitaxial deposition diffuse si source etc., also can be used for preparing electronic-grade silane or silicon.SiF 4be the synthetic materials of silicoorganic compound, for the manufacture of silicofluoric acid and silicon fluoride, the stiffening agent of cement and artificial marble, also generates for plasma etching, solar cell, the photosensitive cylinder of duplicating machine, amorphous silicon film and chemical vapor deposition etc.SiF 4or the raw material of photoconductive fiber pure quartz glass.In addition, SiF 4also be widely used in the stiffening agent etc. preparing silicofluoric acid and aluminum fluoride, chemical analysis, fluorizating agent, oil well probing, magnesium alloy casting, catalyzer, fumigant, cement and artificial marble.Therefore, SiF 4there is the very large market demand capacity.
In the related, SiF 4preparation mainly contain following methods: sulfuric acid process and hydrogen fluoride; Sulphate method is that silicofluoride, Fluorspar Powder, silicate fluoride solution and the strong sulfuric acid response utilizing the silicofluoric acid of phosphate fertilizer plant's by-product to prepare prepares silicon tetrafluoride; Hydrogen fluoride is under the high temperature conditions, and silica flour and anhydrous hydrofluoric acid are mixed with silicon tetrafluoride.
But in above two kinds of methods, first method needs the vitriol oil and the Fluorspar Powder of at substantial; The price of anhydrous hydrofluoric acid used in second method is high; Therefore, in the related, SiF is prepared 4method there is the higher defect of cost.
Summary of the invention
The object of the present invention is to provide a kind of SiF 4preparation method, to solve the above problems.
A kind of SiF is provided in embodiments of the invention 4preparation method, comprise the following steps:
Siliceous mineral raw material or siliceous metal oxide are mixed with fluorochemical, obtains mixture;
Described mixture is reacted, obtains gaseous state SiF 4.
This SiF provided by the invention 4preparation method, by being reacted by the mixture of siliceous mineral raw material or siliceous metal oxide and fluorochemical, and then obtain the SiF of gaseous state 4.
The method is at preparation SiF 4process in, its raw material used is siliceous mineral raw material or siliceous metal oxide and fluorochemical, and its cost of material is cheap more many than traditional raw material (vitriol oil and Fluorspar Powder or anhydrous hydrofluoric acid), and then reduces SiF 4preparation cost.
Accompanying drawing explanation
Fig. 1 shows the SiF that the embodiment of the present invention 1 provides 4the schema of preparation method;
Fig. 2 shows the SiF that the embodiment of the present invention 2 provides 4the schema of preparation method;
Fig. 3 shows the SiF that the embodiment of the present invention 3 provides 4the schema of preparation method;
Fig. 4 shows the SiF that the embodiment of the present invention 4 provides 4the schema of preparation method;
Fig. 5 shows the SiF that the embodiment of the present invention 5 provides 4the schema of preparation method.
Embodiment
Also by reference to the accompanying drawings the present invention is described in further detail below by specific embodiment.
A kind of SiF provided by the invention 4preparation method, comprise the following steps:
Step 101: siliceous mineral raw material or siliceous metal oxide are mixed with fluorochemical, obtains mixture;
Siliceous mineral raw material or siliceous metal oxide obtain the mixture of question response after mixing with fluorochemical, to carry out follow-up preparation manipulation.
Step 102: reacted by mixture, obtains gaseous state SiF 4;
After obtaining mixture, by being reacted by mixture, and then obtain gaseous state SiF 4.
The method is at preparation SiF 4process in, its raw material used is siliceous mineral raw material or siliceous metal oxide and fluorochemical, and its cost of material is cheap more many than traditional raw material (vitriol oil and Fluorspar Powder or anhydrous hydrofluoric acid), and then reduces SiF 4preparation cost.
In addition, this SiF provided by the invention 4preparation method, processing step is few, simple to operate, can also obtain mixed oxide in reaction process, and then adds the added value in preparation process.
In order to make the SiF of the embodiment of the present invention one 4preparation method better applied, be more effectively applied to preparation highly purified SiF 4process in, above-mentioned all flow processs can also specifically be carried out according to following step, are now described in detail and explain:
Step 201: siliceous mineral raw material or siliceous metal oxide are mixed with fluorochemical, obtains mixture;
In step 201, for ease of realizing the operation of mixing, siliceous mineral raw material or siliceous metal oxide are particle or Powdered, and generally speaking, siliceous mineral raw material comprises bauxitic clay, flyash, iron ore or oxide containing silicon; It is 95-500 object particulate state SiO that siliceous metal oxide comprises particle diameter 2; Silicone content in the material of above-mentioned lifted kind is high, and then is beneficial to increase SiF 4output.In addition, be easy to make reaction process occur, the fluorochemical in above-described embodiment can be preferably: mass concentration is HF solution, the NH of 25-40% 4f, NH 4hF 2, CaF 2, NaF or AlF 3.
And in order to make above-mentioned siliceous mineral raw material or siliceous metal oxide and fluorochemical can react completely as much as possible at the mixture of composition, preferably, the weight percentage that fluorochemical accounts for mixture is 20%-80%.
In addition, above-mentioned siliceous mineral raw material or siliceous metal oxide and fluorochemical, when composition mixture, can must mix as far as possible; Preferably, the particle diameter of siliceous mineral raw material is less than 7 millimeters; NH 4f, NH 4hF 2, CaF 2, NaF or AlF 3particle diameter be less than 7 millimeters.
Step 202: reacted by mixture, obtains gaseous state SiF 4;
In the process that mixture is carried out reacting, preferably, when fluorochemical comprises NH 4f, NH 4hF 2, CaF 2, NaF or AlF 3time, the concrete steps of reaction can be: by mixture 600 DEG C of-1300 DEG C of high-temperature calcinations 3 hours-15 hours, obtain gaseous state SiF 4; By high-temperature calcination, mixture is easy to react, and calcines predetermined time in above-mentioned predetermined temperature range, can make abundant reaction, and then forms a large amount of gaseous state SiF 4.Meanwhile, preferably, by the process of mixture reaction, be chosen in air atmosphere and react, by mixture reaction in air atmosphere, be beneficial to and improve gaseous state SiF 4output.
In addition, when to comprise mass concentration be the HF solution of 25-40% to fluorochemical, the concrete steps of reaction can be: by mixture 100 DEG C-200 DEG C reactions 3 hours-15 hours, obtain gaseous state SiF 4, mass concentration be the HF solution of 25-40% under the condition of 100 DEG C-200 DEG C then can fully and siliceous mineral raw material or siliceous metal oxide react, and then form gaseous state SiF 4.
In the present embodiment, siliceous mineral raw material or siliceous metal oxide and fluorochemical are in the process of reacting, and its chemical reaction occurred is as follows:
M xO y·nSiO 2+AF z→M xO y+A 2O z+SiF 4↑
In addition, in the present embodiment, in order to obtain highly purified SiF 4, by mixture reaction, after obtaining in the step of gaseous state SiF4, also comprise: by gaseous state SiF 4the SiF that purity is 99%-99.9% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4gas.
In addition, on the basis of above-mentioned steps, present invention also offers following specific embodiment: please refer to Fig. 1-Fig. 5:
Embodiment 1: with flyash and NH 4f is that high-purity Si F prepared by raw material 4
Step 301: particle diameter is all less than 7mm flyash (Al 2o 3nSiO 2) and NH 4f mixes, and obtains mixture;
Wherein, NH 4the weight percentage that F accounts for mixture is 30%;
Step 302: by mixture 600 DEG C of high-temperature calcinations 3 hours, obtain gaseous state SiF 4;
Step 303: by gaseous state SiF 4the SiF that purity is 99.0% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4gas.
In the present embodiment, the chemical reaction of generation is as follows:
SiO 2+4NH 4F→SiF 4↑+4NH 3↑+2H 2O
Embodiment 2: with coarse particles SiO 2and CaF 2for high-purity Si F prepared by raw material 4
Step 401: be 95-500 object particulate state SiO by particle diameter 2with the CaF that particle diameter is less than 7 millimeters 2mix, obtain mixture;
Wherein, CaF 2the weight percentage accounting for mixture is 40%;
Step 402: by mixture 1100 DEG C of high-temperature calcinations 2 hours, obtain gaseous state SiF 4;
Step 403: by gaseous state SiF 4the SiF that purity is 99.9% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4gas.
In the present embodiment, the chemical reaction of generation is as follows:
SiO 2+2CaF 2→SiF 4↑+2CaO
Embodiment 3: with bauxitic clay (Al 2o 3mTiO 2nSiO 2) and AlF 3for high-purity Si F prepared by raw material 4
Step 501: particle diameter is the bauxitic clay (Al being less than 7mm 2o 3mTiO 2nSiO 2) and AlF 3mix, obtain mixture;
Wherein, AlF 3the weight percentage accounting for mixture is 50%;
Step 502: by mixture 1300 DEG C of high-temperature calcinations 15 hours, obtain gaseous state SiF 4;
Step 503: by gaseous state SiF 4the SiF that purity is 99.9% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4gas.
In the present embodiment, the chemical reaction of generation is as follows:
3SiO 2+4AlF 3·3H 2O→2Al 2O 3+3SiF 4↑+12H 2O
Embodiment 4: with coarse-grain SiO 2with NH 4hF 2for high-purity Si F prepared by raw material 4
Step 601: coarse-grain SiO particle diameter being all less than 7 millimeters 2with NH 4hF 2mix, obtain mixture;
Wherein, NH 4hF 2the weight percentage accounting for mixture is 60%;
Step 602: by mixture 700 DEG C of high-temperature calcinations 5 hours, obtain gaseous state SiF 4;
Step 603: by gaseous state SiF 4the SiF that purity is 99.3% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4gas.
In the present embodiment, the chemical reaction of generation is as follows:
SiO 2+2NH 4HF 2→SiF 4↑+2NH 3↑+2H 2O
Embodiment 5: with iron ore and NaF for high-purity Si F prepared by raw material 4
Step 701: iron ore particle diameter being all less than 7 millimeters mixes with NaF, obtains mixture;
Wherein, NaF accounts for the weight percentage of mixture is 40%;
Step 702: by mixture 900 DEG C of high-temperature calcinations 5 hours, obtain gaseous state SiF 4;
Step 703: by gaseous state SiF 4the SiF that purity is 99.5% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4gas.
SiO 2+4NaF+2H 2O→SiF 4↑+4NaOH
In above-mentioned all embodiments, by gaseous state SiF 4the SiF that purity is 99%-99.9% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4the step of gas is specially:
S1: by gaseous state SiF 4carry out gas-liquid separation and vitriol oil drying successively, obtain the gaseous state SiF removing water vapour and/or ammonia 4;
The water vapour generated in whole reaction system or ammonia can be gone out by gas-liquid separation and vitriol oil drying, and then obtain the gaseous state SiF removing water vapour and/or ammonia 4;
S2: will the gaseous state SiF of water vapour or ammonia be removed 4by molecular sieve adsorption, obtain the gaseous state SiF removing granule foreign and sour gas 4;
Molecular sieve adsorption can by gaseous state SiF 4in the granule foreign that is mixed in the sour gas that contains and reaction system remove;
S3: will the gaseous state SiF of granule foreign and sour gas be removed 4carry out cryogenic condensation, obtain the SiF that purity is 99%-99.9% 4liquid;
Concrete, the temperature of cryogenic condensation is preferably :-70 DEG C--and 60 DEG C, SiF 4gas at such a temperature, can change liquid into, and the gas completely that do not eliminate in preorder operation still exists with gas phase at such a temperature, by the operation of cryogenic condensation and then be easy to obtain the SiF that purity is 99%-99.9% 4liquid.
S4: by SiF 4liquid gasification, obtains the SiF that purity is 99%-99.9% 4gas.
By the SiF that will obtain 4liquid gasification, and then the SiF obtaining that purity is 99%-99.9% 4gas, and then realize highly purified SiF 4the preparation of gas.
In addition, in above-mentioned step, the used vitriol oil can be recycled, and such as, can pass through will distill in vaporizer containing the hydrofluoric vitriol oil, again for purifying after being then concentrated into required concentration.
Table 1 shows above-mentioned five embodiments at preparation SiF 4the data of the parameter in the process of gas and each embodiment productive rate, please refer to table 1:
The Data Comparison table of each embodiment of table 1
The preparation SiF that the embodiment of the present invention provides can be found out by table 1 4method there is the effects such as low cost, high quality, high yield, high purity.
To sum up, this SiF provided by the invention 4preparation method have: the effect that processing step is few, simple to operate, cost is low.And by the described gaseous state SiF of control 4the SiF that purity is 99%-99.9% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4gas, and above-mentioned all operations all can be achieved by existing equipment.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (6)

1. a SiF 4preparation method, it is characterized in that, comprise the following steps:
Siliceous mineral raw material or siliceous metal oxide are mixed with fluorochemical, obtains mixture;
Described fluorochemical comprises NH 4f, NH 4hF 2, CaF 2, NaF or AlF 3;
Reacted by described mixture, described mixture, 600 DEG C of-1300 DEG C of high-temperature calcinations 3 hours-15 hours, obtains gaseous state SiF 4;
By described gaseous state SiF 4the SiF that purity is 99%-99.9% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4gas.
2. SiF according to claim 1 4preparation method, it is characterized in that, described, siliceous mineral raw material is mixed with fluorochemical, obtain in the step of mixture:
The weight percentage that described fluorochemical accounts for described mixture is 20%-80%.
3. SiF according to claim 2 4preparation method, it is characterized in that, described siliceous mineral raw material comprises bauxitic clay, flyash, iron ore or oxide containing silicon;
It is 95-500 object particulate state SiO that described siliceous metal oxide comprises particle diameter 2.
4. SiF according to claim 3 4preparation method, it is characterized in that, described siliceous mineral raw material is the particle or Powdered that particle diameter is less than 7 millimeters;
Described NH 4f, NH 4hF 2, CaF 2, NaF or AlF 3particle diameter be all less than 7 millimeters.
5. the SiF according to any one of claim 1-4 4preparation method, it is characterized in that, described by described gaseous state SiF 4the SiF that purity is 99%-99.9% is obtained after being purified by gas-liquid separation, vitriol oil drying, molecular sieve adsorption and condensation 4step in, specifically comprise:
By described gaseous state SiF 4carry out gas-liquid separation and vitriol oil drying successively, obtain the gaseous state SiF removing water vapour and/or ammonia 4;
By the gaseous state SiF of described removal water vapour or ammonia 4by molecular sieve adsorption, obtain the gaseous state SiF removing granule foreign and sour gas 4;
By the gaseous state SiF of described removal granule foreign and sour gas 4carry out cryogenic condensation, obtain the SiF that purity is 99%-99.9% 4liquid;
By described SiF 4liquid gasification, obtains the SiF that purity is 99%-99.9% 4gas.
6. SiF according to claim 5 4preparation method, it is characterized in that, the temperature of described cryogenic condensation is-70 DEG C--60 DEG C.
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CN104071820B (en) * 2014-07-21 2017-06-13 扬州百德光电有限公司 A kind of method that calcirm-fluoride is produced by the LCD glass etching liquid that gives up
CN105110359B (en) * 2015-09-09 2017-03-29 洛阳国兴矿业科技有限公司 A kind of method that utilization low-grade bauxite prepares aluminium fluoride
CN105271239B (en) * 2015-10-28 2017-10-03 内江师范学院 A kind of method that using plasma method prepares nano-metal silicon
CN105347348A (en) * 2015-11-26 2016-02-24 中国船舶重工集团公司第七一八研究所 Water removal method for silicon tetrafluoride
CN109205646B (en) * 2017-07-07 2021-08-10 中国科学院过程工程研究所 Method for enriching alumina in fly ash and method for preparing solid white carbon black
CN110681667B (en) * 2018-07-05 2022-02-18 中国科学院过程工程研究所 Method for removing silicon dioxide in minerals and/or solid wastes
CN109205669A (en) * 2018-11-19 2019-01-15 新特能源股份有限公司 The combined preparation process of zirconium chloride and ocratation

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CN1110959A (en) * 1994-01-31 1995-11-01 南非原子能有限公司 Treatment of a chemical
CN1856442A (en) * 2003-09-25 2006-11-01 昭和电工株式会社 Method for producing tetrafluorosilane
CN101061060A (en) * 2004-11-18 2007-10-24 瓦克化学股份公司 Process for preparing element halides

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1110959A (en) * 1994-01-31 1995-11-01 南非原子能有限公司 Treatment of a chemical
CN1856442A (en) * 2003-09-25 2006-11-01 昭和电工株式会社 Method for producing tetrafluorosilane
CN101061060A (en) * 2004-11-18 2007-10-24 瓦克化学股份公司 Process for preparing element halides

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