CA2150841C - Method for the preparation of magnesium hydride - Google Patents
Method for the preparation of magnesium hydrideInfo
- Publication number
- CA2150841C CA2150841C CA002150841A CA2150841A CA2150841C CA 2150841 C CA2150841 C CA 2150841C CA 002150841 A CA002150841 A CA 002150841A CA 2150841 A CA2150841 A CA 2150841A CA 2150841 C CA2150841 C CA 2150841C
- Authority
- CA
- Canada
- Prior art keywords
- magnesium
- hydride
- pressure
- hydrogen
- highly reactive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H19/00—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof
- C07H19/02—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof sharing nitrogen
- C07H19/04—Heterocyclic radicals containing only nitrogen atoms as ring hetero atom
- C07H19/16—Purine radicals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/04—Hydrides of alkali metals, alkaline earth metals, beryllium or magnesium; Addition complexes thereof
Abstract
A method for the preparation of magnesium hydride in the presence of a catalyst for the absorbing of hydrogen with hydride formation is desired where finely dispersed, highly reactive magnesium is added as catalyst to the finely divided magnesium that is to be hydrogenated and the hydrogenation is carried out at a temperature of 250 °C and a pressure of 0.5 to 5 MPa.
Description
4 ~ ~
MET~IOD FOR THE PREPARATION OF
~ N~SIIlM HYDRIDE
The invention relates to a method for the preparation of magnesium hydride, which can be used particularly in active magnesium hydride/magnesium/hydrogen storage systems, that absorb hydrogen reversibly.
of the metal hydride/metal systems, which come into consideration as reversible hydrogen storage systems, the MgH2-Mg system is distinguished by the highest proportion by weight of reversibly bound hydrogen (7.65~ by weight) and, with that, the highest energy density per unit weight of the storage material (2,332 Wh/~g).
Up to now, the unsatisfactory kinetics of this system stood in the way of the use of such storage systems for mobile purposes. For example, it is known that pure magnesium can be hydrogenated only under drastic conditions and even then only very slowly and incompletely.
Attempts have therefore been made to improve the ability to hydrogenate magnesium by doping or alloying the magnesium with foreign metals, such as Al, In, Fe, Mg2Ni, Mg2Cu or LaNi5. Admittedly, it was possible to achieve improvements by NY2-35810.1 _ these means with respect to the kinetics. However, important disadvantages remained, such as the need for drastic conditions for the first hydrogenation of the doped magnesium. Moreover, the storage capacities of such systems was less than the theoretically expected value.
Starting out from this state of the art, the European patent 0 112 548 is concerned with the problem of improving the magnesium hydride/magnesium/hydrogen storage system and, in particular, with improving doping. The European patent 0 112 548 teaches a method of the above-described class with the disting~ h;ng feature that magnesium hydride or metallic magnesium is reacted in a very finely dispersed form by contact with a solution of a metal complex and/or an organometallic compound of a metal of the 6th to 8th subsidiary group of the periodic system, optionally in the presence of hydrogen, the respective transition metal being deposited at the surface of the magnesium hydride and/or magnesium particles.
However, it is a disadvantage of this method that metal complexes or organometallic compounds have to be used, which generally are expensive, and frequently are dangerous to handle and/or are toxic. Such a method is therefore not entirely satisfactory for economic and environmental reasons as well as with respect to sources of danger for the personnel charged with carrying out the method.
NY2-35810.1 21S08~1 -~he German Of ~enlegungsschr~ ft ~0 39 ~78 te~c:hes a ~ethod for h~ltc~."enating ma~nesium, ~or Which ~agnesiu;~ hydride wlth a pa~ticle ~:iz~ of ~ 400 ~m ~c added in an amount of ~t least 1.~ by w~ight, based on the magnes~u~ to ~e ~l~.lro~enated, as cataly~t to the f~nely divided magnesium tnat ~a to ~e hydrogenat~d and the hydroqenation is carried out at a temperaturQ o~ 2 250~C and a pressure of 4.5 to ~ MPa by constant st~rring.
By the~ ~eans, the re~ulting ~agne6ium hydride i5 obtained a~ a finely divided, flowable, ~eadily handled product.
q~he hyd~ nation r~action itself i~ promoted by th~ ~irrin~.
Tl~ ~asi~ o~ thls me~hod i~ th~t ~in~ly dividQd ~agn~ium hydrlde, when added to the magnesium that is to be hyd~G~nated, exerts an autocatalytic ef~ect.
Surpri~ingly, it ha~ now been fo~nd that an add~t~on of f~nely di~per~d, bighly reac~ve magn~sium to ordinary ~agnesium powd~r permitR ~h~ latter to b~ hydrogen~ted in an advantageou~
manner~ In other words, the addition of a catalytia amount of finely disper~e~, highly reaotlve ma~nesi~ indu~s the cimpl~
hydro~enation of a ~ommercial magnesium.
NY2-35810. 1 8 4 ~ ~
One object of the present invention i8 to provide a method for preparing an active magnesium hydride-magnesium hydro~en storage ~ystem, which reversibly absorb~
hydrogen, comprising:
adding 1% to 10% by weight of a finely di6persed, highly reactive magnesium as a catalyst to fin~ly disper~ed magne~ium to be hydrogenated; and hydrogenating at a temperature of at least 250 C at a pressure of O.5 to 5 MPa while stirring constantly.
Amounts of 1 to 10 and preferably 2 to 5% by weight, based on the magnesium to be hydrogenated, are adequate here.
Optionally, the highly reactive magnesium can be produced in situ.
The concept of finely dispersed, highly reactive magnesium comprises activated forms of metallic magnesium, which can be produced by numerous methods known in the art, for example, by the method of the German Offenlegungsschrift 33 40 492, from magnesium hydride, magnesium anthracene and/or its derivatives or magnesium butadiene and/or its alkyl or phenyl NY2-35810.1 - 21508~1 '_ derivatives by thermal decomposition. The German Offenle~u~ schrift 33 40 492 teaches that these activated forms of metallic magnesium are suitable for the reversible production of active magnesium hydride under moderate conditions of pressure and temperature. This highly reactive magnesium differs completely-from conventional commercial magnesium particularly with respect to the hydrogenation conditions that are to be employed, so that the hydrogen absorption is reported already at 150~C under normal pressure.
As a modification of the thermal decomposition of magnesium anthracene to highly reactive magnesium, the possibility of decomposing it with the help of ultrasound is pointed out by J. Treber (Thesis, Kaiserlautern (1989)).
K. J. Klabunde et al. (J. Organomet. Chem., 71, 309-13 (1974)) describe the production of highly reactive magnesium by atomic vaporization.
R. C. Fuson (J. Am. Chem. Soc., 79, 928 (1957)) confirms the possibility of obtaining a reactive magnesium by intensive grind ing .
According to R. D. Rieke, magnesium can be obtained in an active form by reducing magnesium halides with alkali metals, particularly with potassium in tetrahydrofuran (THF) (Acc. Chem.
NY2-35810.1 6 Res., 10, 301 (1977)) or 1,2-dimethoxyethane, optionally with the addition of naphthalene as electron transfer agent (Arnold &
Kullenovi'c, Synth. Commun., 7, 223 (1977); Rieke et al., J. Org.
Chem., 46, 4323 (1981)).
The possibility of easily hydrogenating highly reactive, finely dispersed forms of magnesium is state of the art. All the more surprising is the observation that the addition of a catalytic amount of highly reactive magnesium metal makes the technically simple hydrogenation of conventional, commercial magnesium powder possible.
A preferred form of the inventive method described here lies in initiating the hydrogenation of magnesium by adding an active magnesium metal, which was obtained previously by dehydrogenating magnesium hydride, in catalytic amounts, the genesis of this magnesium hydride being of subordinate importance.
The method fulfills the aforementioned conditions in that it is economic, does not have an adverse impact on the environment and does not require larger amounts of organometallic complexes or compounds.
Although the inventive method resorts to using a small amount of partly highly pyrophoric magnesium metal as catalyst NY2-35810.1 21~08~1 ~, for hydrogenating conventional commercial magnesium, the finely divided magnesium hydride obtained is a non-pyrophoric powder, which can be handled well.
The inventive method is explained in greater detail by means of the following Example, it is understood that the Example is provided by way of illustration and not by way of limitation:
Example Magnesium powder (Aluma, Grade S, 2845 g, 117 moles), with an average particle size of less than 75 ~m, is added to a 16 L pressure reactor under a blanket of argon. To determine the essential hydrogenation parameters, the pressure reactor is connected to a multichannel recorder. A highly active, pyrophoric magnesium powder (56.9 g, 2.3 moles), produced according to the method of the German Offenlegungsschrift 33 40 492, is added while strictly maintaining inert gas conditions.
The reactor is closed off and evacuated to a pressure of 133 Pa with the help of an oil pump. Hydrogen is then admitted to the pressure tank up to a pressure of 4.0 bar and the tank is closed off and heated with constant stirring of the solid bed to 350~C.
After 5~ hours of heating, the maximum pressure, which had built up to 9.8 bar due to the higher temperature, decreases slowly and drops to 3.3 bar after a further hour. A constant pressure of 10 bar hydrogen is applied to the reactor. This causes the internal NY2--35810.1 ~ 5 Q 8 4 temperature to rise markedly. The hydrogenation kinetics can be followed by measuring the pressure drop per unit time, hydrogen absorptions of 1.7 bar per minute being attained. As the reaction declines, the hydrogenation rate decreases, as does the evolution of heat, which is associated therewith. Stirring is continued overnight. After the reactor has cooled off, the pressure is relieved and 3088 g of a freely flowing magnesium hydride, which is not pyrophoric, is obtained from the bottom outlet.
The hydride content of a sample is determined gas volumetrically by the method of Zh. Neorgh. Khim, 6, 1961, by decomposition with H2CrO4. The hydride content is determined to be 6.95%.
Although embodiments of the invention have been described above, it i~ not limited thereto and it will be apparent to those skilled in the art that numerous modifications form part of the present invention insofar as they do not depart from the spirit, nature and scope of the claimed and described invention.
NY2--35810.1
MET~IOD FOR THE PREPARATION OF
~ N~SIIlM HYDRIDE
The invention relates to a method for the preparation of magnesium hydride, which can be used particularly in active magnesium hydride/magnesium/hydrogen storage systems, that absorb hydrogen reversibly.
of the metal hydride/metal systems, which come into consideration as reversible hydrogen storage systems, the MgH2-Mg system is distinguished by the highest proportion by weight of reversibly bound hydrogen (7.65~ by weight) and, with that, the highest energy density per unit weight of the storage material (2,332 Wh/~g).
Up to now, the unsatisfactory kinetics of this system stood in the way of the use of such storage systems for mobile purposes. For example, it is known that pure magnesium can be hydrogenated only under drastic conditions and even then only very slowly and incompletely.
Attempts have therefore been made to improve the ability to hydrogenate magnesium by doping or alloying the magnesium with foreign metals, such as Al, In, Fe, Mg2Ni, Mg2Cu or LaNi5. Admittedly, it was possible to achieve improvements by NY2-35810.1 _ these means with respect to the kinetics. However, important disadvantages remained, such as the need for drastic conditions for the first hydrogenation of the doped magnesium. Moreover, the storage capacities of such systems was less than the theoretically expected value.
Starting out from this state of the art, the European patent 0 112 548 is concerned with the problem of improving the magnesium hydride/magnesium/hydrogen storage system and, in particular, with improving doping. The European patent 0 112 548 teaches a method of the above-described class with the disting~ h;ng feature that magnesium hydride or metallic magnesium is reacted in a very finely dispersed form by contact with a solution of a metal complex and/or an organometallic compound of a metal of the 6th to 8th subsidiary group of the periodic system, optionally in the presence of hydrogen, the respective transition metal being deposited at the surface of the magnesium hydride and/or magnesium particles.
However, it is a disadvantage of this method that metal complexes or organometallic compounds have to be used, which generally are expensive, and frequently are dangerous to handle and/or are toxic. Such a method is therefore not entirely satisfactory for economic and environmental reasons as well as with respect to sources of danger for the personnel charged with carrying out the method.
NY2-35810.1 21S08~1 -~he German Of ~enlegungsschr~ ft ~0 39 ~78 te~c:hes a ~ethod for h~ltc~."enating ma~nesium, ~or Which ~agnesiu;~ hydride wlth a pa~ticle ~:iz~ of ~ 400 ~m ~c added in an amount of ~t least 1.~ by w~ight, based on the magnes~u~ to ~e ~l~.lro~enated, as cataly~t to the f~nely divided magnesium tnat ~a to ~e hydrogenat~d and the hydroqenation is carried out at a temperaturQ o~ 2 250~C and a pressure of 4.5 to ~ MPa by constant st~rring.
By the~ ~eans, the re~ulting ~agne6ium hydride i5 obtained a~ a finely divided, flowable, ~eadily handled product.
q~he hyd~ nation r~action itself i~ promoted by th~ ~irrin~.
Tl~ ~asi~ o~ thls me~hod i~ th~t ~in~ly dividQd ~agn~ium hydrlde, when added to the magnesium that is to be hyd~G~nated, exerts an autocatalytic ef~ect.
Surpri~ingly, it ha~ now been fo~nd that an add~t~on of f~nely di~per~d, bighly reac~ve magn~sium to ordinary ~agnesium powd~r permitR ~h~ latter to b~ hydrogen~ted in an advantageou~
manner~ In other words, the addition of a catalytia amount of finely disper~e~, highly reaotlve ma~nesi~ indu~s the cimpl~
hydro~enation of a ~ommercial magnesium.
NY2-35810. 1 8 4 ~ ~
One object of the present invention i8 to provide a method for preparing an active magnesium hydride-magnesium hydro~en storage ~ystem, which reversibly absorb~
hydrogen, comprising:
adding 1% to 10% by weight of a finely di6persed, highly reactive magnesium as a catalyst to fin~ly disper~ed magne~ium to be hydrogenated; and hydrogenating at a temperature of at least 250 C at a pressure of O.5 to 5 MPa while stirring constantly.
Amounts of 1 to 10 and preferably 2 to 5% by weight, based on the magnesium to be hydrogenated, are adequate here.
Optionally, the highly reactive magnesium can be produced in situ.
The concept of finely dispersed, highly reactive magnesium comprises activated forms of metallic magnesium, which can be produced by numerous methods known in the art, for example, by the method of the German Offenlegungsschrift 33 40 492, from magnesium hydride, magnesium anthracene and/or its derivatives or magnesium butadiene and/or its alkyl or phenyl NY2-35810.1 - 21508~1 '_ derivatives by thermal decomposition. The German Offenle~u~ schrift 33 40 492 teaches that these activated forms of metallic magnesium are suitable for the reversible production of active magnesium hydride under moderate conditions of pressure and temperature. This highly reactive magnesium differs completely-from conventional commercial magnesium particularly with respect to the hydrogenation conditions that are to be employed, so that the hydrogen absorption is reported already at 150~C under normal pressure.
As a modification of the thermal decomposition of magnesium anthracene to highly reactive magnesium, the possibility of decomposing it with the help of ultrasound is pointed out by J. Treber (Thesis, Kaiserlautern (1989)).
K. J. Klabunde et al. (J. Organomet. Chem., 71, 309-13 (1974)) describe the production of highly reactive magnesium by atomic vaporization.
R. C. Fuson (J. Am. Chem. Soc., 79, 928 (1957)) confirms the possibility of obtaining a reactive magnesium by intensive grind ing .
According to R. D. Rieke, magnesium can be obtained in an active form by reducing magnesium halides with alkali metals, particularly with potassium in tetrahydrofuran (THF) (Acc. Chem.
NY2-35810.1 6 Res., 10, 301 (1977)) or 1,2-dimethoxyethane, optionally with the addition of naphthalene as electron transfer agent (Arnold &
Kullenovi'c, Synth. Commun., 7, 223 (1977); Rieke et al., J. Org.
Chem., 46, 4323 (1981)).
The possibility of easily hydrogenating highly reactive, finely dispersed forms of magnesium is state of the art. All the more surprising is the observation that the addition of a catalytic amount of highly reactive magnesium metal makes the technically simple hydrogenation of conventional, commercial magnesium powder possible.
A preferred form of the inventive method described here lies in initiating the hydrogenation of magnesium by adding an active magnesium metal, which was obtained previously by dehydrogenating magnesium hydride, in catalytic amounts, the genesis of this magnesium hydride being of subordinate importance.
The method fulfills the aforementioned conditions in that it is economic, does not have an adverse impact on the environment and does not require larger amounts of organometallic complexes or compounds.
Although the inventive method resorts to using a small amount of partly highly pyrophoric magnesium metal as catalyst NY2-35810.1 21~08~1 ~, for hydrogenating conventional commercial magnesium, the finely divided magnesium hydride obtained is a non-pyrophoric powder, which can be handled well.
The inventive method is explained in greater detail by means of the following Example, it is understood that the Example is provided by way of illustration and not by way of limitation:
Example Magnesium powder (Aluma, Grade S, 2845 g, 117 moles), with an average particle size of less than 75 ~m, is added to a 16 L pressure reactor under a blanket of argon. To determine the essential hydrogenation parameters, the pressure reactor is connected to a multichannel recorder. A highly active, pyrophoric magnesium powder (56.9 g, 2.3 moles), produced according to the method of the German Offenlegungsschrift 33 40 492, is added while strictly maintaining inert gas conditions.
The reactor is closed off and evacuated to a pressure of 133 Pa with the help of an oil pump. Hydrogen is then admitted to the pressure tank up to a pressure of 4.0 bar and the tank is closed off and heated with constant stirring of the solid bed to 350~C.
After 5~ hours of heating, the maximum pressure, which had built up to 9.8 bar due to the higher temperature, decreases slowly and drops to 3.3 bar after a further hour. A constant pressure of 10 bar hydrogen is applied to the reactor. This causes the internal NY2--35810.1 ~ 5 Q 8 4 temperature to rise markedly. The hydrogenation kinetics can be followed by measuring the pressure drop per unit time, hydrogen absorptions of 1.7 bar per minute being attained. As the reaction declines, the hydrogenation rate decreases, as does the evolution of heat, which is associated therewith. Stirring is continued overnight. After the reactor has cooled off, the pressure is relieved and 3088 g of a freely flowing magnesium hydride, which is not pyrophoric, is obtained from the bottom outlet.
The hydride content of a sample is determined gas volumetrically by the method of Zh. Neorgh. Khim, 6, 1961, by decomposition with H2CrO4. The hydride content is determined to be 6.95%.
Although embodiments of the invention have been described above, it i~ not limited thereto and it will be apparent to those skilled in the art that numerous modifications form part of the present invention insofar as they do not depart from the spirit, nature and scope of the claimed and described invention.
NY2--35810.1
Claims (2)
1. A method for preparing an active magnesium hydride-magnesium hydrogen storage system, which reversibly absorbs hydrogen, comprising:
adding 1% to 10% by weight of a finely dispersed, highly reactive magnesium as a catalyst to finely dispersed magnesium to be hydrogenated; and hydrogenating at a temperature of at least 250°C at a pressure of 0.5 to 5 MPa while stirring constantly.
adding 1% to 10% by weight of a finely dispersed, highly reactive magnesium as a catalyst to finely dispersed magnesium to be hydrogenated; and hydrogenating at a temperature of at least 250°C at a pressure of 0.5 to 5 MPa while stirring constantly.
2. The method as set forth in claim 1, wherein said finely dispersed, highly reactive magnesium is added in an amount of 2% to 5% by weight.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4419456A DE4419456A1 (en) | 1994-06-03 | 1994-06-03 | Process for the production of magnesium hydride |
| DEP4419456.0-41 | 1994-06-03 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2150841A1 CA2150841A1 (en) | 1995-12-04 |
| CA2150841C true CA2150841C (en) | 1999-04-20 |
Family
ID=6519728
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002150841A Expired - Fee Related CA2150841C (en) | 1994-06-03 | 1995-06-02 | Method for the preparation of magnesium hydride |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP0685425B1 (en) |
| JP (1) | JP3474317B2 (en) |
| CA (1) | CA2150841C (en) |
| DE (2) | DE4419456A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10954344B2 (en) | 2018-08-15 | 2021-03-23 | Evonik Operations Gmbh | SiOC-bonded, linear polydimethylsiloxane-polyoxyalkylene block copolymers |
| US11021575B2 (en) | 2018-08-15 | 2021-06-01 | Evonik Operations Gmbh | Process for producing acetoxy-bearing siloxanes |
Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE59603454D1 (en) * | 1995-05-26 | 1999-12-02 | Goldschmidt Ag Th | Process for the production of X-ray amorphous and nanocrystalline metal powder |
| JP2001163603A (en) * | 1999-12-08 | 2001-06-19 | Sanyo Electric Co Ltd | Metal hydride and manufacturing method thereof |
| JP4099350B2 (en) * | 2002-06-07 | 2008-06-11 | 株式会社水素エネルギー研究所 | Method for producing alkali metal borohydride |
| CN100431945C (en) * | 2007-01-23 | 2008-11-12 | 太原理工大学 | Method for preparing magnesium based hydrogen storage material |
| CN101910052B (en) * | 2009-03-05 | 2012-09-05 | 生物焦炭技术研究株式会社 | Method for producing magnesium-based hydride |
| JP5495010B2 (en) * | 2009-07-31 | 2014-05-21 | バイオコーク技研株式会社 | Magnesium oxide reduction method and reaction apparatus |
| JP5635478B2 (en) * | 2011-10-27 | 2014-12-03 | 東邦チタニウム株式会社 | Method for producing titanium hydride |
| KR102270863B1 (en) | 2013-09-25 | 2021-06-30 | 다이헤이요 세멘토 가부시키가이샤 | Method for producing metal hydride |
| CN107995905B (en) * | 2015-04-02 | 2021-03-30 | 雅宝德国有限责任公司 | Highly reactive metal hydrides, method for the production thereof and use thereof |
| MA41837A (en) * | 2015-04-02 | 2018-02-06 | Albemarle Germany Gmbh | PROCESS FOR THE PRODUCTION OF ORGANOMETALLIC COMPOUNDS |
| EP3168273B1 (en) | 2015-11-11 | 2018-05-23 | Evonik Degussa GmbH | Curable polymers |
| EP3321304B1 (en) | 2016-11-15 | 2019-06-19 | Evonik Degussa GmbH | Mixtures of cyclic branched d/t-type siloxanes and their ensuing products |
| EP3415547B1 (en) | 2017-06-13 | 2020-03-25 | Evonik Operations GmbH | Method for producing sic-linked polyether siloxanes |
| EP3415548B1 (en) | 2017-06-13 | 2020-03-25 | Evonik Operations GmbH | Method for producing sic-linked polyether siloxanes |
| EP3438158B1 (en) | 2017-08-01 | 2020-11-25 | Evonik Operations GmbH | Production of sioc-linked siloxanes |
| EP3467006B1 (en) | 2017-10-09 | 2022-11-30 | Evonik Operations GmbH | Mixtures of cyclic branched d/t-type siloxanes and their ensuing products |
| JP7257653B2 (en) * | 2019-08-29 | 2023-04-14 | 新東工業株式会社 | Method for producing magnesium hydride and method for producing tetrahydroborate |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH337181A (en) * | 1954-07-12 | 1959-03-31 | Bayer Ag | Process for the production of magnesium hydride |
| 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 |
| DE3247360A1 (en) * | 1982-12-22 | 1984-07-05 | Studiengesellschaft Kohle mbH, 4330 Mülheim | METHOD FOR PRODUCING ACTIVE MAGNETIC SIUMHDRID MAGNESIUM HYDROGEN STORAGE SYSTEMS |
| US5069894A (en) * | 1978-02-02 | 1991-12-03 | Studiengesellschaft Kohle Mbh | Process for preparing finely divided highly reactive magnesium and use thereof |
| DE2804445A1 (en) * | 1978-02-02 | 1979-08-09 | Studiengesellschaft Kohle Mbh | METHOD FOR MANUFACTURING MAGNESIUM HYDRIDS |
| DE3247361A1 (en) * | 1982-12-22 | 1984-06-28 | Studiengesellschaft Kohle mbH, 4330 Mülheim | METHOD FOR SEPARATING AND PURIFYING HYDROGEN |
| CA1123816A (en) * | 1978-02-06 | 1982-05-18 | Harold M. Simons | Granulating and activating metal to form metal hydride |
| DE4039278A1 (en) * | 1990-12-08 | 1992-06-11 | Goldschmidt Ag Th | METHOD FOR PRODUCING ACTIVE, REVERSIBLE H (DOWN ARROW) 2 (DOWN ARROW) RECORDING MAGNESIUM HYDRODIDE MAGNESIUM HYDROGEN STORAGE SYSTEMS |
-
1994
- 1994-06-03 DE DE4419456A patent/DE4419456A1/en not_active Withdrawn
-
1995
- 1995-05-20 DE DE59501143T patent/DE59501143D1/en not_active Expired - Fee Related
- 1995-05-20 EP EP95107714A patent/EP0685425B1/en not_active Expired - Lifetime
- 1995-06-01 JP JP13544495A patent/JP3474317B2/en not_active Expired - Fee Related
- 1995-06-02 CA CA002150841A patent/CA2150841C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10954344B2 (en) | 2018-08-15 | 2021-03-23 | Evonik Operations Gmbh | SiOC-bonded, linear polydimethylsiloxane-polyoxyalkylene block copolymers |
| US11021575B2 (en) | 2018-08-15 | 2021-06-01 | Evonik Operations Gmbh | Process for producing acetoxy-bearing siloxanes |
| US11905376B2 (en) | 2018-08-15 | 2024-02-20 | Evonik Operations Gmbh | SiOC-bonded, linear polydimethylsiloxane-polyoxyalkylene block copolymers |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07330305A (en) | 1995-12-19 |
| EP0685425A1 (en) | 1995-12-06 |
| DE4419456A1 (en) | 1995-12-07 |
| DE59501143D1 (en) | 1998-02-05 |
| EP0685425B1 (en) | 1997-12-29 |
| CA2150841A1 (en) | 1995-12-04 |
| JP3474317B2 (en) | 2003-12-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2150841C (en) | Method for the preparation of magnesium hydride | |
| JP2504651B2 (en) | Manufacturing method of active magnesium hydride-magnesium-hydrogen storage system that reversibly absorbs hydrogen | |
| Resan et al. | Effects of various catalysts on hydrogen release and uptake characteristics of LiAlH4 | |
| US6814782B2 (en) | Method for reversibly storing hydrogen on the basis of alkali metals and aluminum | |
| Liang et al. | Catalytic effect of transition metals on hydrogen sorption in nanocrystalline ball milled MgH2–Tm (Tm= Ti, V, Mn, Fe and Ni) systems | |
| EP1025040B1 (en) | Method of fabrication of complex alkali metal hydrides | |
| Fernandes et al. | Efficient catalytic properties of Co–Ni–P–B catalyst powders for hydrogen generation by hydrolysis of alkaline solution of NaBH4 | |
| JP4584716B2 (en) | Composite hydride for hydrogen storage | |
| US7314579B2 (en) | Hydrogen generation material | |
| US4368143A (en) | Composition for the storage of hydrogen and method of making the composition | |
| JPS6346001B2 (en) | ||
| US4798718A (en) | Method of preparing active magnesium-hydride of magnesium hydrogen-storer systems | |
| JP2001519312A5 (en) | ||
| JP2006504616A5 (en) | ||
| JP2002526255A (en) | Reversible hydrogen storage composition | |
| Sun et al. | The effect of doping NiCl2 on the dehydrogenation properties of LiAlH4 | |
| JP2002522209A (en) | Novel hydrogen storage material and production method by dry homogenization | |
| Liu et al. | Kinetic characteristics of sodium borohydride formation when sodium meta-borate reacts with magnesium and hydrogen | |
| Li et al. | Enhancement of the H2 desorption properties of LiAlH4 doping with NiCo2O4 nanorods | |
| JP2005512793A (en) | Hydrogen reversible storage material using doped aluminum hydride alkali metal salts | |
| US4554152A (en) | Method of preparing active magnesium-hydride or magnesium hydrogen-storer systems | |
| US5199972A (en) | Method of preparing active magnesium-hydride or magnesium hydrogen-storer systems | |
| Zhang et al. | Mechanistic insights into the remarkable catalytic activity of nanosized Co@ C composites for hydrogen desorption from the LiBH 4–2LiNH 2 system | |
| CA1285792C (en) | Process for preparing finely divided metal powders | |
| Zhong et al. | Hydrogen storage properties of Mg (Al) solid solution alloy doped with LaF3 by ball milling |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| MKLA | Lapsed |