DEP0002911BA - Process for the preparation of an effective contact mass for the synthesis of methylchlorosilanes - Google Patents
Process for the preparation of an effective contact mass for the synthesis of methylchlorosilanesInfo
- Publication number
- DEP0002911BA DEP0002911BA DEP0002911BA DE P0002911B A DEP0002911B A DE P0002911BA DE P0002911B A DEP0002911B A DE P0002911BA
- Authority
- DE
- Germany
- Prior art keywords
- synthesis
- contact mass
- copper powder
- methylchlorosilanes
- effective contact
- 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
Links
- 238000000034 method Methods 0.000 title claims description 8
- 230000015572 biosynthetic process Effects 0.000 title claims description 5
- 238000003786 synthesis reaction Methods 0.000 title claims description 5
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical class C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 title claims description 3
- 238000002360 preparation method Methods 0.000 title 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000011863 silicon-based powder Substances 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 239000005751 Copper oxide Substances 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229910000431 copper oxide Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
Description
Die für die Kontaktsynthese von Methylchlorsilanen aus Methylchlorid und Silicium bisher angewandte Kontaktmasse besteht aus einem Gemisch von Kupfer- und Siliciumpulver, der zur Erzielung einer genügenden Wirksamkeit bei ungefähr 1000°C in einer reduzierenden Atmosphäre vorgesintert werden musste. Dieser Arbeitsgang bedeutet infolge der hohen, in der Nähe des Schmelzpunktes von Kupfer liegenden Temperatur eine wesentliche Erschwerung der Herstellung.The contact compound previously used for the contact synthesis of methylchlorosilanes from methyl chloride and silicon consists of a mixture of copper and silicon powder, which had to be pre-sintered at around 1000 ° C in a reducing atmosphere to achieve sufficient effectiveness. Due to the high temperature, which is close to the melting point of copper, this operation makes production considerably more difficult.
Der Erfindung liegt die Aufgabe zugrunde, die Herstellung derartiger Kontaktmassen zu vereinfachen, was dadurch erreicht wird, dass eine Mischung von teilweise oder völlig oxydiertem Kupferpulver mit Siliciumpulver im Wasserstoffstrom erhitzt wird (250 - 400°C).The invention is based on the object of simplifying the production of such contact masses, which is achieved by heating a mixture of partially or fully oxidized copper powder with silicon powder in a hydrogen stream (250-400 ° C.).
Das neue Verfahren wird dadurch noch verbessert, dass die Mischung von oxydiertem Kupferpulver und Siliciumpulver vor der Wärmebehandlung in dem gewünschten Mengenverhältnis zu Tabletten verpresst und die Tabletten wieder zerbröckelt werden. Eine Verstärkung des Sinterungseffektes wird erreicht, wenn man die unreduzierte Kontaktmasse zunächst im Stickstoffstrom auf etwa 250 - 400°C vorerhitzt und dann rasch auf Wasserstoff umschaltet.The new process is further improved in that the mixture of oxidized copper powder and silicon powder is pressed into tablets in the desired proportions before the heat treatment and the tablets are crumbled again. The sintering effect is enhanced if the unreduced contact mass is first preheated to around 250 - 400 ° C in a nitrogen stream and then quickly switched to hydrogen.
Die bei der Verbrennung des Wasserstoffs zu Wasser unter gleichzeitiger Reduktion des Kupferoxyds zu Kupfer freiwerdende Reaktionswärme ruft den gewünschten Sinterungseffekt an zahlreichen Einzelstellen hervor, und zwar überall dort, wo sich Kupferoxydpartikelchen in der Masse befinden.The heat of reaction released during the combustion of the hydrogen to water with simultaneous reduction of the copper oxide to copper causes the desired sintering effect at numerous individual points, namely wherever there are copper oxide particles in the mass.
Durch die erwähnte Vorerhitzung im Stickstoffstrom sind die örtlich auftretenden Temperaturen dann noch wesentlich höher, wodurch der Sinterungsprozess noch mehr gefördert wird.As a result of the aforementioned preheating in a stream of nitrogen, the locally occurring temperatures are then significantly higher, which promotes the sintering process even more.
In beiden Fällen lässt man die erhaltene Kontaktmasse im Wasserstoff- oder Stickstoffstrom erkalten, nachdem das sich bei der Reduktion gebildete Wasser herausgetrieben ist.In both cases, the contact mass obtained is allowed to cool in a stream of hydrogen or nitrogen after the water formed during the reduction has been driven out.
Der Sinterungsvorgang wird dabei zweckmässig in dem verwendeten Syntheserohr durchgeführt.The sintering process is expediently carried out in the synthesis tube used.
Als Kupferpulver wird zweckmässig elektrolytisch hergestelltes Kupferpulver verwendet.Electrolytically produced copper powder is expediently used as the copper powder.
Beispiel: Als besonders vorteilhafte Kontaktmasse im Sinne der Erfindung wurde folgende Masse festgestellt:Example: The following mass was found to be a particularly advantageous contact mass within the meaning of the invention:
Kristallisiertes Silicium mit einem Gehalt von mehr als 90% Silicium wird in einer Kugelmühle fein gemahlen. Hiervon werden 7,5 Gewichtsteile mit einem Gewichtsteil elektrolytisch abgeschiedenem und durch längeres Liegenlassen an der Luft teilweise oxydiertem Kupferpulver innig vermischt. Die Masse wird unter Zugabe von etwas Wasser zu Tabletten verpresst und nach Zerbröckelung in erbsengrosse Stücke in das Reaktionsrohr eingefüllt. Zunächst wird im Stickstoffstrom die Feuchtigkeit ausgetrieben und die Masse auf 250 - 400° vorerhitzt, dann wird rasch auf Wasserstoff umgeschaltet, wobei das Kupferoxyd reduziert wird und dadurch örtlich eine geringe Sinterung mit dem Silicium erfährt. Anschliessend lässt man die Masse im Wasserstoffstrom erkalten, wonach sie gebrauchsfähig ist.Crystallized silicon with a silicon content of more than 90% is finely ground in a ball mill. 7.5 parts by weight of this are intimately mixed with one part by weight of electrolytically deposited copper powder which has been partially oxidized by leaving it in the air for a long time. The mass is compressed into tablets with the addition of a little water and, after crumbling, poured into pea-sized pieces into the reaction tube. First of all, the moisture is expelled in a stream of nitrogen and the mass is preheated to 250 - 400 °, then it is quickly switched to hydrogen, whereby the copper oxide is reduced and thus locally undergoes a slight sintering with the silicon. The mass is then left to cool in a stream of hydrogen, after which it is ready for use.
Claims (5)
Family
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