IE56457B1 - Method for preparing compounds of silicon and hydrogen,especially silane - Google Patents
Method for preparing compounds of silicon and hydrogen,especially silaneInfo
- Publication number
- IE56457B1 IE56457B1 IE3016/83A IE301683A IE56457B1 IE 56457 B1 IE56457 B1 IE 56457B1 IE 3016/83 A IE3016/83 A IE 3016/83A IE 301683 A IE301683 A IE 301683A IE 56457 B1 IE56457 B1 IE 56457B1
- Authority
- IE
- Ireland
- Prior art keywords
- magnesium
- hydride
- reaction
- silane
- silicon
- Prior art date
Links
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 4
- 239000001257 hydrogen Substances 0.000 title claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 title description 3
- 239000010703 silicon Substances 0.000 title description 3
- 150000001875 compounds Chemical class 0.000 title 1
- 229910012375 magnesium hydride Inorganic materials 0.000 claims abstract description 23
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 22
- -1 halogen silanes Chemical class 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011777 magnesium Substances 0.000 claims abstract description 11
- 239000012190 activator Substances 0.000 claims abstract description 10
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 3
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 3
- 150000004820 halides Chemical class 0.000 claims abstract description 3
- 150000002681 magnesium compounds Chemical class 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 230000000737 periodic effect Effects 0.000 claims abstract description 3
- 150000003512 tertiary amines Chemical class 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 20
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 4
- 238000005984 hydrogenation reaction Methods 0.000 claims description 3
- 239000005046 Chlorosilane Substances 0.000 claims description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical class Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 238000005580 one pot reaction Methods 0.000 claims 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 229910003910 SiCl4 Inorganic materials 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052987 metal hydride Inorganic materials 0.000 description 5
- 150000004681 metal hydrides Chemical class 0.000 description 5
- 150000004756 silanes Chemical class 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 150000004678 hydrides Chemical class 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012280 lithium aluminium hydride Substances 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- 101100219382 Caenorhabditis elegans cah-2 gene Proteins 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000001343 alkyl silanes Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical class B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- BUMGIEFFCMBQDG-UHFFFAOYSA-N dichlorosilicon Chemical compound Cl[Si]Cl BUMGIEFFCMBQDG-UHFFFAOYSA-N 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/04—Hydrides of silicon
- C01B33/043—Monosilane
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0896—Compounds with a Si-H linkage
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Silicon Polymers (AREA)
- Catalysts (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
1. Process for the preparation of silicon hydride compounds, in particular of silane (SiH4 ) from halogen silanes, characterized in that halogen silanes, in particular tetrachlorosilane, are reacted with magnesium hydride in a solvent in the absence of additional catalysts and/or activators, which magnesium hydride is obtained by reacting magnesium with hydrogen in the presence of a catalyst consisting of a halide of a metal of sub-Groups IV to VIII of the periodic System and of an organic magnesium compound or of a magnesium hydride and optionally in the presence of a polycyclic aromatic compound or af a tertiary amine and optionally in the presence of a magnesium halide MgX2 where X = Cl, Br, l.
Description
This invention relates to a process for the preparation of silicon hydride compounds, in particular silane (SiH) which is used industrially for the production (J of highly pure silicon.
Of t.hf? ’wo conventional methods for the synthesis of silane, namely the protolytic decomposition of magnos- j. ium silicide (M^Si) and the reaction of tetrachlorosilane with metal hydrides (Gmelin's Handbuch d. Anorg.Chem., S_i , Supplement Volume 1, page 59 ( 1 982 )), the latter has the advantage, inter alia, that the silane can be obtained free from unwanted impurities, in particular of higher silanes.
Since the discovery of lithium aluminium hydride and its use for the synthesis of metal hydrides and hydrides; of other elements (Finholt, Bond, Wilzbach and Schlesinger, J .Amer.Chem.Soc. 69 , 2962 (1 947)), the reaction of SiCl^ with LiAlH^ is regarded-as the best and simplest laboratory method for the preparation of silane (Norman, Webster, Jolly, Inorg.Syn. 1 1 , 170 (1968)). Silane prepared by this method is suitable for the production of silicon for the semi-conductor and solar cell industry since it is free from boron hydride compounds and higher silanes (Gmelin's Handbuch, loc.cit page 63). For industrial application of this reaction on a large scale, however, the relatively high cost of lithium aluminium hydride is found to be a disadvantage. There has therefore been no lack of attempts in the last 20 to 25 years to replace LiAlH^, which is suitable for this purpose but expensive, by less expensive metal hydrides, if necessary in complex φ form. According to Zakharkin et al (Bull. Acad. Sci.(USSR), Chem. Sci. Div. (1962, 1784) and Antipin et al (J.Appl.
Chem.(USSR) 42, 416 (1969)), SiCl4, HSiCl^ and alkoxysilanes react, with NaAllI^ or KAlII^ in THF or diglyme even at low ί.(·ιηρ«.·ι ,it ni '«.·:» Ι.ο I or m silane in high yields. Not hint, is known about the industrial application of this method to the synthesis of silane.
It is significant in relation to the present invention that the simple, binary hydrides of alkali metals and alkaline earth metals such as NaH, MgH^ and CaH^ have not hitherto been used as such for the preparation of silane but only after their conversion into complex hydrides of aluminium (by a reaction with AlCl^: GB-A 832 333 C.A. 16765 (1960), Vit et al, Czech. 126672 (1962/68), C.A. 7θ . 39392 (1969)) or in the presence of activators or catalysts. The reason for this is presumably the low solubility and/or reactivity of the binary metal hydrides which are produced from the elements at high temperatures and pressures. Zinc haiides, zinc hydrides and zinc alkyls and zinc oxide (GB-A 909 950, C.A. 58 (1963) 2185) and metallic zinc and zinc alloys (US-A 3 050 366, C.A. 58 (1963) 280) have been recommended as catalysts for the reaction of NaH, CaH2 or MgH2 with SiCl4, but the ZnCl2 required as catalyst" for the reaction of SiCl^ with, for example, NaH in THF is used in a molar ratio of SnCl2 : SiCl^ = 1:2, i.e. in virtually stoichiometric quantity. Boron alkyls and aluminium alkyls (DE-C 1 034 1 59, C.A. 56 , 16764 ; Jenkner, Chemiker Ztg. 85, 264/72 (1961)) and boron and aluminium hydrides (DE-C 1 085 505, C.A. 21505 (1961) and DE-C 1 096 341, C.A. 26388 (1961)) have also been recommended as catalysts or activators for the 'production of SiH^ from NaH and SiCl4, but when these catalystrs or activators are employed there is a risk of the silane containing the unwanted alkyl silanes (when AlR^ is used as activator) or boron compounds (when boron activators are used) as impurities. According to SU-A 126 672, C.A. 84 166812 (1976). on the other hand, these disadvantages do not arise when NaAlH^ is used as activator.
The experiments described in GB-A 909 950 for the preparation of silane SiH^ using magnesium hydride should -3b<· ρ.ι ι t ί ru 1 u c 1 y noted. Th'’ s«i i d document explicitly states that magnesium hydrides arc? unsuitable tor the preparation of high purity silane by a reaction with halogen silanes.
It is clear from what has been said above that no simple and economical technical solution is as yet available for the production of silane from binary metal hydrides by their reaction with halogen silanes. „ According to EP-A 0 003 564, however, metallic magnesium may be hydrogenated under mild reaction conditions with the aid of homogeneous transition metal catalysts to produce a magnesium hydride which in contrast to magnesium hydride prepared by the conventional method (high temperature hydrogenation) is highly reactive.
The process described there is one in which magnesium is reacted with hydrogen in the presence of a catalyst consisting of a halide of a metal of sub-Groups IV to VIII of the Periodic System and of an organic magnesium compound or of a magnesium hydride and optionally in the presence of a polycyclic aromatic compound or of a tertiary amine or optionally in the presence of a magnesium halide MgX2where X = Cl, Br or I.
It has now surprisingly been found that magnesium hydride which is readily available by this method is eminently suitable for the production of silanes from tetrachlorosilane or other chlorosilanes without the use of any further catalysts or activators.
When carried out in a cyclic or linear ether or a polyether such as THF or glyme as solvent, the reaction will take place even at room temperature or at slightly elevated temperature (50 to 70°C) and gives rise to the corresponding silanes in high yields.
In combination with.the above mentioned synthesis of magnesium hydride, therefore, silane is obtained by a two-stage synthesis from the inexpensive raw materials, Mg. and, for example, SiCl^, as follows: -4Catalyst Mg + H2 -> Mg2 Activator MgH2 + SiCl4 -> SiH4 + 2 MgCl2· Another advantage of this method is that the hydrogenation of magnesium and subsequent reaction of MgH2 with SiCl2 can be carried out in one and the same reaction vessel using, for example, THF as reaction medium.
Alternatively, the MgH2 prepared according to EP-A 0 003 564 may be isolated in solid form and then used in another suitable solvent for the reaction with chloro10 silanes, e.g. SiCl4> The invention is described in more detail below with the aid of the following Examples without, however, being limited to these.
Example 1 0.68 g of the magnesium hydride prepared according to EP-A 0 003 564 using Ti catalyst was introduced under argon into an apparatus consisting of a 100 ml three-necked flask equipped with a dropping funnel, internal thermometer, magnetic stirrer and cooling finger (-78°C) and an attached gas burette filled with mercury, and the magnesium hydride was covered with a layer of 20 ml of absolute THF. A solution of 1.40 g (0.7 ml, 6.1 mmol) of SiCl4 in 20 ml of THF was added dropwise to the MgH2 suspension at room temperature with stirring. The reaction mixture was slowly heated and evolution of gas set in at about 40°C. The gas evolved was measured by means of the gas burette. The heat of the reaction temporarily raised the temperature of the reaction mixture to 65°C.
After completion of the reaction, the amount of gas evolved was 134 ml (20°C, 1 bar). MS Analysis of the gas showed it to contain 20.9 mol-% of SiH^ (remainder argon). Taking into account the total volume of the apparatus, the SiH4 -5yield war, calculated from ( l·, i s t.<> he BO'*..
Exampl u_ 2 The experiment was carried out as in Example 1, using an in situ produced suspension of M9If2 catalyst). The reaction of MgH^ with SiCl4 to form SiH^ in this case already took place at 25 to 28°C. The yield of SiH. was 76?..
Example 3 18-56 g of the magnesium hydride prepared according to EP-A 0 003 564 (Ti catalyst) was introduced under argon into an apparatus consisting of a 1-litre threenecked flask equipped with dropping funnel, internal thermometer, magnetic guide and reflux condenser (methanol 10°C) and attached to a cooling trap (-78°C), and the reactant was covered with a layer of 250 ml of absolute glyme. A solution of 107.20 g (126 ml, 0.99 mol) of (CH^)SiCl in 100 ml of glyme was added dropwise to the MgH2 suspension over a period of 3 hours with stirring, the temperature of the mixture rising to 25 to 27°CAfter all the (CH^)siCl had been added, the reaction was briefly heated to boiling in the stream of argon.
The yield of trimethylsilane condensed in the cooling trap (b.p. 6.7°C) was 80%.
Claims (6)
1. Process for the preparation of silicon hydride compounds, in particular of silane (SiH^) from halogen silanes, wherein halogen silanes, in particular tetrachlorosilane, are reacted with magnesium hydride in a solvent in the absence of additional catalysts and/or activators, which magnesium hydride is obtained by reacting magnesium with hydrogen in the presence of a catalyst consisting of a halide of a metal of sub-Groups IV to VIII of the Periodic System and of an organic magnesium compound or of a magnesium hydride and optionally in the presence of a polycyclic aromatic compound or of a tertiary amine and optionally in the presence of a magnesium halide MgX 2 where X = Cl, Br , I.
2. Process according to claim 1 , wherein open chained and cyclic mono- and polyethers, preferably THF or glycol dimethylether,are used as solvents.
3. Process according to claims 1 and 2, wherein the reaction is carried out in the temperature range of from 0 to 15O°C, preferably from 20 to 70 ft C.
4. Process according to claims 1 to 3, wherein the hydrogenation of magnesium and the subsequent reaction of magnesium hydride with chlorosilanes, preferably tetrachlorosilane, are carried out as a one pot process.
5. Process for the preparation of silicon hydride compounds substantially as hereinbefore described with reference to the Examples.
6. Silicon hydride compounds whenever prepared by a process as claimed in any of the preceding claims.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19823247362 DE3247362A1 (en) | 1982-12-22 | 1982-12-22 | METHOD FOR PRODUCING SILICON HYDROGEN COMPOUNDS, ESPECIALLY THE SILANE |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| IE833016L IE833016L (en) | 1984-06-22 |
| IE56457B1 true IE56457B1 (en) | 1991-08-14 |
Family
ID=6181324
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| IE3016/83A IE56457B1 (en) | 1982-12-22 | 1983-12-21 | Method for preparing compounds of silicon and hydrogen,especially silane |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0111924B1 (en) |
| JP (1) | JPS59131519A (en) |
| AT (1) | ATE40815T1 (en) |
| AU (1) | AU577035B2 (en) |
| CA (1) | CA1218828A (en) |
| DE (2) | DE3247362A1 (en) |
| DK (1) | DK161696C (en) |
| ES (1) | ES8406982A1 (en) |
| IE (1) | IE56457B1 (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3340492A1 (en) * | 1983-11-09 | 1985-05-15 | Studiengesellschaft Kohle mbH, 4330 Mülheim | METHOD FOR PRODUCING FINE DISTRIBUTED, HIGHLY REACTIVE MAGNESIUM AND THE USE THEREOF |
| DE3409172A1 (en) * | 1984-03-13 | 1985-09-26 | D. Swarovski & Co., Wattens, Tirol | METHOD FOR PRODUCING SILANE |
| EP0316472A1 (en) * | 1987-11-17 | 1989-05-24 | Ethyl Corporation | Silane production from magnesium hydride |
| US4725419A (en) * | 1985-05-17 | 1988-02-16 | Ethyl Corporation | Silane production from magnesium hydride |
| US4824657A (en) * | 1985-11-27 | 1989-04-25 | E. I. Du Pont De Nemours And Company | Process for reducing silicon, germanium and tin halides |
| US5061470A (en) * | 1990-08-03 | 1991-10-29 | Ethyl Corporation | Silane production from hydridomagnesium chloride |
| JPH0548070U (en) * | 1991-11-28 | 1993-06-25 | 喜和 石渡 | Banknote storage and payout device |
| DE4239246C1 (en) * | 1992-11-21 | 1993-12-16 | Goldschmidt Ag Th | Process for the preparation of SiH-containing organopolysiloxanes |
| DE4313130C1 (en) * | 1993-04-22 | 1994-05-26 | Goldschmidt Ag Th | Silanes and organosilicon hydrides prodn. - by redn. of corresp. silicon halides with non-pyrophoric storage magnesium hydride in THF etc., with continuous removal of halide deposits |
| DE102004062449A1 (en) * | 2004-12-17 | 2006-07-06 | Klaus Dr. Rennebeck | Fuel cell system for water mineralization comprises fuel cell based on micro hollow fiber, which contains electrolytes, which carries separately from each other anode and cathode wherein electrolyte is micro hollow fiber-matrix electrolyte |
| NO326254B1 (en) * | 2005-12-22 | 2008-10-27 | Sinvent As | Process for producing silane |
| DE102009056731A1 (en) | 2009-12-04 | 2011-06-09 | Rev Renewable Energy Ventures, Inc. | Halogenated polysilanes and polygermanes |
| CN105668573A (en) * | 2010-12-23 | 2016-06-15 | 爱迪生太阳能公司 | Systems for producing silane |
| US8388914B2 (en) | 2010-12-23 | 2013-03-05 | Memc Electronic Materials, Inc. | Systems for producing silane |
| US8821825B2 (en) | 2010-12-23 | 2014-09-02 | Sunedison, Inc. | Methods for producing silane |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3050366A (en) * | 1959-07-15 | 1962-08-21 | Du Pont | Production of silane by the use of a zinc catalyst |
| DE2804445A1 (en) * | 1978-02-02 | 1979-08-09 | Studiengesellschaft Kohle Mbh | METHOD FOR MANUFACTURING MAGNESIUM HYDRIDS |
| DE2908928A1 (en) * | 1979-03-07 | 1980-09-18 | Studiengesellschaft Kohle Mbh | METHOD FOR PRODUCING ORGANOLITHIUM COMPOUNDS IN ADDITION TO LITHIUM HYDROID |
| DE3536797A1 (en) * | 1985-10-16 | 1987-04-16 | Studiengesellschaft Kohle Mbh | METHOD FOR PRODUCING HALOGEN MAGNESIUM ALANATE AND THE USE THEREOF |
-
1982
- 1982-12-22 DE DE19823247362 patent/DE3247362A1/en not_active Withdrawn
-
1983
- 1983-12-20 AT AT83112798T patent/ATE40815T1/en not_active IP Right Cessation
- 1983-12-20 EP EP83112798A patent/EP0111924B1/en not_active Expired
- 1983-12-20 DE DE8383112798T patent/DE3379199D1/en not_active Expired
- 1983-12-21 CA CA000443887A patent/CA1218828A/en not_active Expired
- 1983-12-21 ES ES528246A patent/ES8406982A1/en not_active Expired
- 1983-12-21 JP JP58243066A patent/JPS59131519A/en active Granted
- 1983-12-21 AU AU22755/83A patent/AU577035B2/en not_active Ceased
- 1983-12-21 DK DK590083A patent/DK161696C/en not_active IP Right Cessation
- 1983-12-21 IE IE3016/83A patent/IE56457B1/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| AU577035B2 (en) | 1988-09-15 |
| ES528246A0 (en) | 1984-08-16 |
| DK161696C (en) | 1992-01-27 |
| ATE40815T1 (en) | 1989-03-15 |
| DK590083A (en) | 1984-06-23 |
| JPS59131519A (en) | 1984-07-28 |
| EP0111924A2 (en) | 1984-06-27 |
| IE833016L (en) | 1984-06-22 |
| AU2275583A (en) | 1984-06-28 |
| JPH0553727B2 (en) | 1993-08-10 |
| DK590083D0 (en) | 1983-12-21 |
| DK161696B (en) | 1991-08-05 |
| EP0111924B1 (en) | 1989-02-15 |
| EP0111924A3 (en) | 1986-10-29 |
| CA1218828A (en) | 1987-03-10 |
| DE3379199D1 (en) | 1989-03-23 |
| ES8406982A1 (en) | 1984-08-16 |
| DE3247362A1 (en) | 1984-06-28 |
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| MM4A | Patent lapsed |