DE1056099B - Process for the production of boron hydrogen - Google Patents
Process for the production of boron hydrogenInfo
- Publication number
- DE1056099B DE1056099B DEK34214A DEK0034214A DE1056099B DE 1056099 B DE1056099 B DE 1056099B DE K34214 A DEK34214 A DE K34214A DE K0034214 A DEK0034214 A DE K0034214A DE 1056099 B DE1056099 B DE 1056099B
- Authority
- DE
- Germany
- Prior art keywords
- boron
- stage
- reaction
- production
- halides
- 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.)
- Pending
Links
- 229910052796 boron Inorganic materials 0.000 title claims description 16
- 238000000034 method Methods 0.000 title claims description 8
- 239000001257 hydrogen Substances 0.000 title claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 title claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims description 4
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- -1 boron halides Chemical class 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 8
- 150000004678 hydrides Chemical class 0.000 claims description 8
- 239000002841 Lewis acid Substances 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 5
- 150000007517 lewis acids Chemical class 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 229910000102 alkali metal hydride Inorganic materials 0.000 claims 1
- 150000008046 alkali metal hydrides Chemical class 0.000 claims 1
- 150000004820 halides Chemical class 0.000 claims 1
- 150000002897 organic nitrogen compounds Chemical class 0.000 claims 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 2
- LALRXNPLTWZJIJ-UHFFFAOYSA-N triethylborane Chemical group CCB(CC)CC LALRXNPLTWZJIJ-UHFFFAOYSA-N 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- AIGRXSNSLVJMEA-FQEVSTJZSA-N ethoxy-(4-nitrophenoxy)-phenyl-sulfanylidene-$l^{5}-phosphane Chemical compound O([P@@](=S)(OCC)C=1C=CC=CC=1)C1=CC=C([N+]([O-])=O)C=C1 AIGRXSNSLVJMEA-FQEVSTJZSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910000104 sodium hydride Inorganic materials 0.000 description 1
- 239000012312 sodium hydride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000375 suspending agent 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
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/026—Higher boron hydrides, i.e. containing at least three boron atoms
-
- 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
-
- 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
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
- C01B6/10—Monoborane; Diborane; Addition complexes thereof
-
- 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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
Description
Verfahren zur Herstellung von Borwasserstoffen Gegenstand der Patentanmeldung
K 31447 IVa/12 i ist ein Verfahren zur Herstellung von Borwasserstoffen,
das durch Umsetzen von Borhalogeniden mit Alkalihydriden in Gegenwart von organischen
Aminen und von Alkalihydrid aktivierenden Verbindungen gekennzeichnet ist. Das Verfahren
wird in zwei Stufen ausgeübt, deren erste Stufe als Reaktionsprodukt ein N-Alkylborazan
ergibt, aus dem in einer zweiten Stufe nach Zugabe einer sogenannten stärkeren Lewissäure
zum Borazan freier Borwasserstoff resultiert.
Die Reaktion gemäß Gleichung (1) läuft bei einer Temperatur bis zu 100° C in Gegenwart eines Lösungs- oder Suspensionsmittels ab. Als Aktivator für das Alkalihydrid wird eine organische Verbindung eines Elements der I. bis V., vorzugsweise der III. Gruppe des Periodischen Systems verwendet.The reaction according to equation (1) runs at a temperature up to 100 ° C in the presence of a solvent or suspending agent. As an activator for the alkali hydride is an organic compound of an element from I. to V., preferably the III. Group of the Periodic Table used.
Zur Durchführung der zweiten Stufe des Verfahrens entsprechend Gleichung (2) wird nach weitgehendem Verbrauch des Alkalihydrids die Temperatur erhöht, und es werden weitere Mengen des als Lewissäure wirkenden Borhalogenids zugegeben, Zwobei das Borhalogenid den Borwasserstoff aus dem Borazan verdrängt.To carry out the second stage of the procedure according to equation (2) the temperature is increased after extensive consumption of the alkali hydride, and further amounts of the boron halide acting as Lewis acid are added, two of them the boron halide displaces the boron hydrogen from the borazane.
Es wurde nun gefunden, daß die Erhöhung der Temperatur für die Durchführung der zweiten Verfahrensstufe nicht erforderlich ist. Für die Herstellung von niederen Borwasserstoffen, wie Diboran, ist die Beibehaltung der gleichen Temperatur, wie sie bei der Reaktion gemäß der ersten Stufe angewandt wurde, oder sogar eine Temperaturerniedrigung angebracht. Es hat sich herausgestellt, daß bei Erhöhung der Temperatur in der Mehrzahl höhere Borwasserstoffe, wie Pentaboran, erhalten werden. Dabei ist es zweckmäßig, den Aktivator für das Alkalihydrid vor der weiteren Zugabe des Borhalogenids abzutrennen.It has now been found that increasing the temperature to carry out the second stage of the procedure is not required. For making lower Boron hydrocarbons, like diborane, is maintaining the same temperature as it was applied in the reaction according to the first stage, or even a temperature decrease appropriate. It has been found that when the temperature is increased in the majority higher boron hydrogens such as pentaborane can be obtained. It is useful to to separate off the activator for the alkali hydride before further addition of the boron halide.
Beispiel 24 Gewichtsteile Natriumhy drid, suspendiert in 220 Gewichtsteilen eines Mineralöls vom Kp.1mmHg 180 bis 220° C, wurden bei 80° C mit 14 Gewichtsteilen Bortriäthyl, sodann mit 37,5 Gewichtsteilen Triäthylamin versetzt, worauf unter Rühren bei derselben Temperatur 43 Gewichtsteile Bortrichlorid eingeleitet wurden. Zum Entfernen des Alkalihydridaktivators (Bortriäthyl) wurde das Reaktionsgefäß sodann kurz evakuiert und nach Erniedrigung der Temperatur auf etwa 40° C weitere 43,5 Gewichtsteile Bortrichlorid eingeleitet. Es entstand zur Hauptsache Diboran, welches zur Bestimmung in Triäthylamin eingeleitet wurde. Erhalten wurden 29 Gewichtsteile N-Triäthylborazan. Daneben entstanden noch etwa 3 Gewichtsteile flüssige Äthylborwasserstoffe. Wird an Stelle von Bortriäthyl Borsäuremethylester als Aktivator bei einer Temperatur von 90 bis 110° C (erste Stufe) verwendet, so sind die Ausbeuten um etwa 5 bis 8% niedriger.Example 24 parts by weight of sodium hydride suspended in 220 parts by weight of a mineral oil with a bp.1mmHg 180 to 220 ° C, were at 80 ° C with 14 parts by weight Boron triethyl, then treated with 37.5 parts by weight of triethylamine, whereupon below Stirring at the same temperature 43 parts by weight of boron trichloride were introduced. The reaction vessel was used to remove the alkali hydride activator (boron triethyl) then briefly evacuated and further after lowering the temperature to about 40 ° C 43.5 parts by weight of boron trichloride initiated. The main thing that arose was diborane, which was initiated for determination in triethylamine. 29 parts by weight were obtained N-triethylborazane. In addition, about 3 parts by weight of liquid ethyl borohydrocarbons were formed. Used instead of boron triethyl boric acid methyl ester as an activator at a temperature from 90 to 110 ° C (first stage) used, the yields are around 5 to 8% lower.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK34214A DE1056099B (en) | 1958-03-01 | 1958-03-01 | Process for the production of boron hydrogen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK34214A DE1056099B (en) | 1958-03-01 | 1958-03-01 | Process for the production of boron hydrogen |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1056099B true DE1056099B (en) | 1959-04-30 |
Family
ID=7219955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEK34214A Pending DE1056099B (en) | 1958-03-01 | 1958-03-01 | Process for the production of boron hydrogen |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1056099B (en) |
-
1958
- 1958-03-01 DE DEK34214A patent/DE1056099B/en active Pending
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