CN104445209A - Preparation method of silane - Google Patents
Preparation method of silane Download PDFInfo
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- CN104445209A CN104445209A CN201410701176.XA CN201410701176A CN104445209A CN 104445209 A CN104445209 A CN 104445209A CN 201410701176 A CN201410701176 A CN 201410701176A CN 104445209 A CN104445209 A CN 104445209A
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- silicon fluoride
- silane
- preparation
- albite
- fluoride
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Abstract
The invention provides a preparation method of silane. The method comprises steps of albite decomposition reaction, silicon fluoride purification and silane preparation, wherein the albite decomposition reaction comprises steps as follows: mixing albite, fluorite and sulfuric acid with concentration of 98% at a mass ratio of 1: (1.55-2.57): (3.28-4.62) and performing reaction at the temperature of 100-200 DEG C under the self-generated pressure to obtain solid residues and silicon fluoride contained gas; the silicon fluoride purification comprises steps as follows: performing dust removal on the silicon fluoride contained gas, liquefying the silicon fluoride contained gas after dust removal to obtain a silicon fluoride liquid, removing hydrogen fluoride in the silicon fluoride liquid to obtain a silicon fluoride liquid free of hydrogen fluoride, and gasifying the silicon fluoride liquid free of hydrogen fluoride to obtain pure silicon fluoride gas; and silane preparation comprises step as follows: introducing the pure silicon fluoride gas into a sodium aluminum hydride solution for reaction to obtain a silane product. According to the preparation method, gas products including silicon fluoride and sodium aluminum hydride which are generated after albite decomposition are mainly utilized and react to prepare silane, and one novel silane preparation method capable of realizing continuous production is provided.
Description
Technical field
The present invention relates to a kind of preparation method of silane, particularly relate to a kind of method utilizing albite to prepare silane.
Background technology
At present, microelectronics is the main foundation stone of modern information technologies and military technique, is to promote scientific-technical progress, industry development, one of economic liftoff and social key factor of advancing.Unicircuit is the core of microelectronics, and its developmental level and industry size have become the important symbol of a measurement national economic strength.Electronics special gas (as silane), especially high pure electronic gas, as this new class of electronic chemical materials, are the important factors of restriction IC reliability and yield rate.Along with the develop rapidly of electronic information technology, integrated level is more and more higher, has brought up to 6N level (99.9999%), even more than 7N to the purity requirement of basic raw material (as silane), therefore prepares high pure electronic special gas technology and more seems extremely urgent.And the above high pure electronic gas of production 6N level of having the ability only has a few countries, and high-purity gas has a wide range of applications in electronic product, aerospace, high performance solar batteries, war industry, the technology of preparing of silane is not yet perfect, making method complex process, more difficult grasp, the product produced still can not meet the needs of related electronic products comprehensively, of poor quality, problem is many, can only for the manufacture of the product of low specification, therefore, bring larger trouble to user, this situation seriously constrains the development of electronic technology.Original technology adopts trichlorosilane method to produce, because have chlorine in reaction process, so anticorrosion, the material of equipment require very high, facility investment is large, and corrosion is fast, and the chlorine compound contained in product is not easy to reduce, and directly affects the purity of the finished product.
Albite is the one of feldspar, is common spectra, is the aluminosilicate (NaAlSi of sodium
3o
8).Albite chemistry Nature comparison is stablized, under general normal temperature and pressure except hydrofluoric acid almost can not by soda acid or oxygenant decompose, so albite usually has fluorochemical to produce in the process of decomposing, how utilizing albite degradation production to prepare silane is problem demanding prompt solution.
Summary of the invention
By Given this, in order to solve the problem, the invention provides a kind of albite degradation production that utilizes to prepare the method for silane.
A preparation method for silane, comprises the following steps:
Albite decomposition reaction: by albite, fluorite, 98% sulfuric acid mix according to the mass ratio of 1:1.55 ~ 2.57:3.28 ~ 4.62, and be obtained by reacting solid residue and silicon fluoride gas under 100 DEG C ~ 200 DEG C and autogenous pressure;
Purified fluorine SiClx: dust removal process is carried out to described silicon fluoride gas, the described silicon fluoride gas after dedusting that liquefies obtains silicon fluoride liquid, the hydrogen fluoride removed in described silicon fluoride liquid obtains the silicon fluoride liquid of fluoride-free hydrogen, and the silicon fluoride liquid of the described fluoride-free hydrogen that gasifies obtains pure silicon fluoride gas;
Prepare silane: passed in sodium aluminum hydride solution by described pure silicon fluoride gas and react, obtain silane product.
Based on the preparation method of above-mentioned silane, the step that described albite decomposes comprises: at 100 DEG C ~ 200 DEG C, preheat 15 minutes ~ 30 minutes to described albite and fluorite, and removing moisture wherein, obtains dry albite and fluorite raw material; Again the sulfuric acid of 98% is joined in the albite of described drying and fluorite raw material and react the solid residue obtained for 2 hours ~ 5 hours containing calcium sulfate, sodium sulfate and Tai-Ace S 150 and the gaseous products containing silicon fluoride.In this step, described temperature of reaction can be 100 DEG C, 150 DEG C, 180 DEG C, 200 DEG C, is preferably 120 DEG C ~ 200 DEG C; The described reaction times is preferably 2.5 hours ~ 4 hours.
Based on the preparation method of above-mentioned silane, the step of described purified fluorine SiClx comprises: employing dust removal filter removes the dust in described silicon fluoride gas; Described silicon fluoride liquid is obtained with the silicon fluoride gas after dedusting described in water condensation; Remove the impurity hydrogen fluoride in this silicon fluoride liquid at the gas hydrazine adopting ice acetone to cool, obtain the silicon fluoride liquid of described fluoride-free hydrogen; In encloses container, the silicon fluoride liquid of fluoride-free hydrogen described in distillation or pressure distillation, prepares described pure silicon fluoride gas.
Based on the preparation method of above-mentioned silane, the described step preparing silane comprises: the temperature of reaction of described silicon fluoride and sodium aluminum hydride is 200 DEG C ~ 220 DEG C.
Based on the preparation method of above-mentioned silane, prepare in the step of silane described, the mass ratio of described silicon fluoride and described sodium aluminum hydride is 2 ~ 3:40 ~ 50.
Based on the preparation method of above-mentioned silane, described sodium aluminum hydride solution adopts molten sodium, pulverous aluminium and hydrogen react in organic solvent and obtain.
Based on the preparation method of above-mentioned silane, described organic solvent is diglyme or tetrahydrofuran solution.
Compared with prior art, silane is prepared in the gaseous product silicon fluoride after the present invention mainly utilizes albite to decompose and sodium aluminum hydride reaction, provide a kind of silane new, can quantity-produced preparation method; The cost compare of albite is low, and the decomposition reaction mild condition of albite, lower to the requirement of equipment, and utilize silicon fluoride gas to turn waste into wealth, so, preparation method's cost compare of silane provided by the invention is low, reduces the quantity discharged of fluorine element in albite decomposition course, decreasing pollution environment.In addition, the present invention adopts dry albite and fluorite and sulfuric acid reaction can improve the rate of decomposition of speed of response and albite, thus is conducive to the productive rate improving described silane.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
A preparation method for silane, comprises the following steps:
Albite decomposes: first albite and fluorite are preheated about 30 minutes at 100 DEG C, the sulfuric acid adding 98% again makes three react 5 hours under 100 DEG C and autogenous pressure, obtain the solid residue containing calcium sulfate, sodium sulfate and Tai-Ace S 150 and the gaseous products containing silicon fluoride, wherein, albite, fluorite, 98% the mass ratio of sulfuric acid be 1:1.55:3.28, reaction principle is:
CaF
2+ H
2SO
4= 2HF + CaSO
4
2NaAlSi
3O
8+ 24HF + 4H
2SO
4= Na
2SO
4+ Al
2(SO
4)
3+ 6SiF
4↑ + 16H
2O
Purified fluorine SiClx: employing dust removal filter removes the dust in described silicon fluoride gas; Described silicon fluoride liquid is obtained with the silicon fluoride gas after dedusting described in water condensation; Remove the impurity hydrogen fluoride in this silicon fluoride liquid at the gas hydrazine adopting ice acetone to cool, obtain the silicon fluoride liquid of described fluoride-free hydrogen; In encloses container, the silicon fluoride liquid of fluoride-free hydrogen described in distillation or pressure distillation, prepares described pure silicon fluoride gas;
Prepare silane: passed in the diethylene glycol dimethyl ethereal solution of sodium aluminum hydride by described pure silicon fluoride gas, and make the mass ratio of silicon fluoride and sodium aluminum hydride solute be 1:20, and the production silane that reacts at 200 DEG C, its reaction principle is: NaAlH
4+ SiF
4=SiH
4↑+NaAlF
4.
Embodiment 2
The present embodiment is substantially identical with the preparation method of the silane that embodiment 1 provides, and difference is: in the process that albite decomposes, pre-warmed temperature is 150 DEG C, and the pre-warmed time is 20 minutes; The temperature of reaction is 150 DEG C, and the time of reaction is 3.5 hours, and albite, fluorite, 98% the mass ratio of sulfuric acid be 1:2:4; In the process preparing silane, the mass ratio of silicon fluoride and sodium aluminum hydride solute is 3:50, and temperature of reaction is 220 DEG C.
Embodiment 3
The present embodiment is substantially identical with the preparation method of the silane that embodiment 1 provides, and difference is: in the process that albite decomposes, pre-warmed temperature is 200 DEG C, and the pre-warmed time is 15 minutes; The temperature of reaction is 200 DEG C, and the time of reaction is 2 hours, and albite, fluorite, 98% the mass ratio of sulfuric acid be 1:2.5:4.6; In the process preparing silane, the mass ratio of silicon fluoride and sodium aluminum hydride solute is 1:18, and temperature of reaction is 210 DEG C.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request of the present invention protection.
Claims (7)
1. a preparation method for silane, comprises the following steps:
Albite decomposition reaction: by albite, fluorite, 98% sulfuric acid mix according to the mass ratio of 1:1.55 ~ 2.57:3.28 ~ 4.62, and be obtained by reacting solid residue and silicon fluoride gas under 100 DEG C ~ 200 DEG C and autogenous pressure;
Purified fluorine SiClx: dust removal process is carried out to described silicon fluoride gas, the described silicon fluoride gas after dedusting that liquefies obtains silicon fluoride liquid, the hydrogen fluoride removed in described silicon fluoride liquid obtains the silicon fluoride liquid of fluoride-free hydrogen, and the silicon fluoride liquid of the described fluoride-free hydrogen that gasifies obtains pure silicon fluoride gas;
Prepare silane: passed in sodium aluminum hydride solution by described pure silicon fluoride gas and react, obtain silane product.
2. the preparation method of silane according to claim 1, it is characterized in that: the step that described albite decomposes comprises: at 100 DEG C ~ 200 DEG C, preheat 15 minutes ~ 30 minutes to described albite and fluorite, removing moisture wherein, obtains dry albite and fluorite raw material; Again the sulfuric acid of described 98% is joined reaction in the albite of described drying and fluorite raw material and within 2 hours ~ 5 hours, obtain described solid residue containing calcium sulfate, sodium sulfate and Tai-Ace S 150 and the described gaseous products containing silicon fluoride.
3. the preparation method of silane according to claim 1, is characterized in that: the step of described purified fluorine SiClx comprises: employing dust removal filter removes the dust in described silicon fluoride gas; Described silicon fluoride liquid is obtained with the silicon fluoride gas after dedusting described in water condensation; Remove the impurity hydrogen fluoride in this silicon fluoride liquid at the gas hydrazine adopting ice acetone to cool, obtain the silicon fluoride liquid of described fluoride-free hydrogen; In encloses container, the silicon fluoride liquid of fluoride-free hydrogen described in distillation or pressure distillation, prepares described pure silicon fluoride gas.
4. the preparation method of silane according to claim 1, is characterized in that: the described step preparing silane comprises: the temperature of reaction of described silicon fluoride and sodium aluminum hydride is 200 DEG C ~ 220 DEG C.
5. the preparation method of silane according to claims 1 to 4, is characterized in that: prepare in the step of silane described, and the mass ratio of described silicon fluoride and described sodium aluminum hydride is 2 ~ 3:40 ~ 50.
6. the preparation method of silane according to claims 1 to 4, is characterized in that: described sodium aluminum hydride solution adopts molten sodium, pulverous aluminium and hydrogen react in organic solvent and obtain.
7. the preparation method of silane according to claim 6, is characterized in that: described organic solvent is diglyme or tetrahydrofuran solution.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1051152A (en) * | 1989-10-25 | 1991-05-08 | 南开大学 | The synthetic method of sodium aluminum hydride |
| CN101531367A (en) * | 2009-03-13 | 2009-09-16 | 六九硅业有限公司 | Process for producing silicane |
| CN102351198A (en) * | 2011-09-20 | 2012-02-15 | 六九硅业有限公司 | Method for preparing silicon tetrafluoride |
| CN102491339A (en) * | 2011-12-19 | 2012-06-13 | 天津市泰源工业气体有限公司 | Method for preparing silane from sodium aluminum hydride and silicon tetrafluoride |
| CN103539132A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Method for recovering ammonium fluoride from potassium feldspar gas phase absorption liquid |
-
2014
- 2014-11-28 CN CN201410701176.XA patent/CN104445209A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1051152A (en) * | 1989-10-25 | 1991-05-08 | 南开大学 | The synthetic method of sodium aluminum hydride |
| CN101531367A (en) * | 2009-03-13 | 2009-09-16 | 六九硅业有限公司 | Process for producing silicane |
| CN102351198A (en) * | 2011-09-20 | 2012-02-15 | 六九硅业有限公司 | Method for preparing silicon tetrafluoride |
| CN102491339A (en) * | 2011-12-19 | 2012-06-13 | 天津市泰源工业气体有限公司 | Method for preparing silane from sodium aluminum hydride and silicon tetrafluoride |
| CN103539132A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Method for recovering ammonium fluoride from potassium feldspar gas phase absorption liquid |
Non-Patent Citations (2)
| Title |
|---|
| 徐旺生 等: "钾长石综合利用的新工艺", 《武汉化工学院学报》 * |
| 薛彦辉 等: "钾长石-萤石-硫酸体系中分解钾长石的探讨", 《化学与生物工程》 * |
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