WO2011101264A1 - Separating out particles from mixtures containing fluid silicon compounds - Google Patents
Separating out particles from mixtures containing fluid silicon compounds Download PDFInfo
- Publication number
- WO2011101264A1 WO2011101264A1 PCT/EP2011/051615 EP2011051615W WO2011101264A1 WO 2011101264 A1 WO2011101264 A1 WO 2011101264A1 EP 2011051615 W EP2011051615 W EP 2011051615W WO 2011101264 A1 WO2011101264 A1 WO 2011101264A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silicon compounds
- mixtures containing
- centrifugation
- solid particles
- particles
- Prior art date
Links
- 239000002245 particle Substances 0.000 title claims abstract description 21
- 239000000203 mixture Substances 0.000 title claims abstract description 13
- 150000003377 silicon compounds Chemical class 0.000 title claims abstract description 10
- 239000012530 fluid Substances 0.000 title abstract 2
- 239000007787 solid Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000005119 centrifugation Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 230000001133 acceleration Effects 0.000 claims description 4
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical class C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 7
- 229910000077 silane Inorganic materials 0.000 description 7
- 238000001914 filtration Methods 0.000 description 5
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000005046 Chlorosilane Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical class Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 229940050176 methyl chloride Drugs 0.000 description 2
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- -1 siloxanes Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
Classifications
-
- 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
- C07F7/20—Purification, separation
Definitions
- the invention relates to a separation process for solid particles and mixtures containing liquid silicon compounds.
- Methylchlorosilanes are prepared by direct synthesis according to Müller-Rochow. Here you bring metallic silicon with methyl chloride in the presence of a
- Alkylchlorosilanes oligosilanes, carbosilanes, siloxanes,
- One of these process steps consists in the purification of the raw gas of discharged particles. This is preferably done in cyclones. The separation in the cyclones is not
- Silane stream dispersed For its cleaning is
- the invention relates to a separation process for
- the separation of the dispersed particles by means of centrifuges as separators can be carried out batchwise or, preferably, continuously, whereby a fully continuous
- centrifuges In contrast to dead-end filtration techniques, centrifuges are able to clarify liquids with high levels of contaminants without additional effort. Throughput and service life during centrifugation are in the
- the particle separation rate can be controlled by the acceleration of the mixtures in the centrifuge and the duration of the centrifugation.
- the relative centrifugal acceleration RZB is preferably at least 100 g, particularly preferably at least 500 g, in particular at least 1000 g and preferably at most
- the solids concentration in the centrifugate is preferably at most 50 ppm, particularly preferably at most 20 ppm,
- the ambient pressure during the centrifugation is preferably at least 0.1 bar, particularly preferably at least 0.5 bar and preferably at most 100 bar, more preferably at most 10 bar, in particular at most 3 bar.
- the temperature during the centrifugation is preferably at least 0 ° C, more preferably at least 10 ° C and preferably at most 100 ° C, especially at most 70 ° C.
- plate separators are used in continuous centrifugation.
- the mixtures containing liquid silicon compounds and solid particles are the product genes known as crude silane from the production of
- the organosilicon compounds are preferably methylchlorosilanes, oligosilanes, carbosilanes, siloxanes and high-boiling cracking products thereof.
- Solid particles containing mixtures can also be used.
- the crude silane preferably has a solids concentration of at least 0.01% and at most 10%.
- the metal salt reduction after a centrifugation time of 5 minutes at different speeds of 2000, 3500, and 5000 rpm and 10 minutes at 5000 rpm are compared in the table:
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention relates to a method for separating mixtures containing solid particles and fluid silicon compounds by means of centrifuging.
Description
Abtrennung von Partikeln aus flüssige Siliciumverbindungen enthaltenden Gemischen Separation of particles from mixtures containing liquid silicon compounds
Die Erfindung betrifft ein Trennverfahren für Feststoffpartikel und flüssige Siliciumverbindungen enthaltende Gemische. The invention relates to a separation process for solid particles and mixtures containing liquid silicon compounds.
Die Herstellung von Methylchlorsilanen erfolgt in der direkten Synthese nach Müller - Rochow. Hier bringt man metallisches Silicium mit Methylchlorid in Gegenwart eines Methylchlorosilanes are prepared by direct synthesis according to Müller-Rochow. Here you bring metallic silicon with methyl chloride in the presence of a
Katalysatorsystems zur Reaktion. Dabei entsteht im Reaktor ein Rohgas, welches nicht umgesetztes Methylchlorid, Catalyst system for the reaction. This produces a crude gas in the reactor, which unreacted methyl chloride,
Alkylchlorsilane, Oligosilane, Carbosilane, Siloxane, Alkylchlorosilanes, oligosilanes, carbosilanes, siloxanes,
hochsiedende Crackprodukte und Feststoffpartikel enthält. contains high-boiling cracking products and solid particles.
Bei der Herstellung von Chlorsilanen wird metallisches Silicium mit Chlorwasserstoff umgesetzt. In the production of chlorosilanes, metallic silicon is reacted with hydrogen chloride.
Die Stoffgemische werden jeweils in mehreren The mixtures are each in several
Verfahrensschritten aufgearbeitet . Processed process steps.
Einer dieser Verfahrensschritte besteht in der Reinigung des Rohgases von ausgetragenen Partikeln. Bevorzugt geschieht das in Zyklonen. Die Abscheidung in den Zyklonen ist nicht One of these process steps consists in the purification of the raw gas of discharged particles. This is preferably done in cyclones. The separation in the cyclones is not
vollständig. Ein weiterer Reinigungsschritt muss sich Completely. Another cleaning step has to be done
anschließen. Nach der Kondensation des Rohgases sind die connect. After the condensation of the raw gas are the
Partikel, welche aus dem Reaktor ausgetragen werden, im Particles, which are discharged from the reactor, in
Silanstrom dispergiert. Zu dessen Reinigung wird Silane stream dispersed. For its cleaning is
herkömmlicherweise die Dead End Filtration, beispielsweise mit Filterkerzen verwendet. Eine quantitative Abtrennung mittels Filtration ist problematisch. Des weiteren neigen die conventionally used the dead end filtration, for example with filter cartridges. Quantitative separation by filtration is problematic. Furthermore, the tend
Filterkerzen zu plötzlichem Verstopfen.
Gegenstand der Erfindung ist ein Trennverfahren fürFilter candles to sudden clogging. The invention relates to a separation process for
Feststoffpartikel und flüssige Siliciumverbindungen enthaltendeSolid particles and liquid silicon compounds containing
Gemische durch Zentrifugation. Bei der Zentrifugation setzen sich die Feststoffpartikel als Sediment ab und die flüssigen Siliciumverbindungen bilden das Zentrifugat, Die Partikel werden vollständig und kontinuierlich mittels Zentrifugation aus dem Silanstrom entfernt. Des Mixtures by centrifugation. During centrifugation, the solid particles settle out as sediment and the liquid silicon compounds form the centrifugate. The particles are completely and continuously removed by centrifugation from the silane stream. Of
weiteren ist es möglich, sehr feine Partikel <40nm further it is possible, very fine particles <40nm
abzuscheiden, welche mittels der aktuell gebräuchlichen Dead- End-Filtration nur mit hohem Druckverlust zurückgehalten werden können. Filterverstopfungen werden vermieden, kosten- und zeitaufwendiger Filtertausch bzw. Filterreinigung entfallen. Nachfolgende Betriebseinrichtungen werden sicher vor to be separated, which can be retained by means of the currently used dead-end filtration only with high pressure loss. Filter blockages are avoided, costly and time-consuming filter replacement or filter cleaning omitted. Subsequent operating equipment will be safe
Feststoffbelastung geschützt. Solid load protected.
Die Abtrennung der dispergierten Partikel mittels Zentrifugen als Separatoren kann diskontinuierlich oder vorzugsweise kontinuierlich erfolgen, wodurch ein vollkontinuierlicher The separation of the dispersed particles by means of centrifuges as separators can be carried out batchwise or, preferably, continuously, whereby a fully continuous
Betrieb gewährleistet werden kann. Operation can be guaranteed.
Der Austrag der abgetrennten Feststoffpartikel erfolgt The discharge of the separated solid particles takes place
diskontinuierlich, semi-kontinuierlich oder vorzugsweise vollkontinuierlich. discontinuous, semi-continuous or preferably fully continuous.
Im Gegensatz zu Dead End Filtrationstechniken sind Zentrifugen in der Lage, Flüssigkeiten mit hohen Trübstoffgehalten ohne zusätzliche Aufwand zu klären. Durchsatz und Standzeit bei der Zentrifugation sind im In contrast to dead-end filtration techniques, centrifuges are able to clarify liquids with high levels of contaminants without additional effort. Throughput and service life during centrifugation are in the
Gegensatz zur Dead End Filtration nahezu unbegrenzt.
Die Partikelabtrennungsrate kann durch die Beschleunigung der Gemische in der Zentrifuge und die Zentrifugationsdauer gesteuert werden. Die Relative Zentrifugalbeschleunigung RZB beträgt vorzugsweise mindestens 100 g, besonders bevorzugt mindestens 500 g, insbesondere mindestens 1000 g und vorzugsweise höchstens Unlike Dead End Filtration almost unlimited. The particle separation rate can be controlled by the acceleration of the mixtures in the centrifuge and the duration of the centrifugation. The relative centrifugal acceleration RZB is preferably at least 100 g, particularly preferably at least 500 g, in particular at least 1000 g and preferably at most
100000 g, besonders bevorzugt höchstens 50000 g, insbesondere höchstens 10000 g, wobei g die mittlere 100000 g, more preferably at most 50 000 g, in particular at most 10000 g, g being the average
Erdschwerebeschleunigung bedeutet. Earth gravity means.
In der DIN 58970-2 wird die Relative Zentrifugalbeschleunigung (RZB) definiert. Diese Größe wird als Vielfaches des mittleren Wertes von g angegeben. Nach der DIN kann der RZB-Wert mittels folgender Formel errechnet werden, in der r [m] der Abstand desDIN 58970-2 defines relative centrifugal acceleration (RZB). This quantity is given as a multiple of the mean value of g. According to DIN, the RZB value can be calculated using the following formula, where r [m] is the distance of the
Gemischs von der Drehachse und n [s-1] dxe Drehzahl bedeuten:
Mit der Einstellung der Feststoffkonzentration im Zentrifugat, der über dem Sediment aus den Feststoffpartikeln stehenden flüssige Siliciumverbindungen, kann sich die Aufarbeitung der flüssigen Siliciumverbindungen unmittelbar anschließen. Die Feststoffkonzentration im Zentrifugat beträgt vorzugsweise höchstens 50 ppm, besonders bevorzugt höchstens 20 ppm, Mixture of the axis of rotation and n [s -1 ] dxe speed mean: With the adjustment of the solids concentration in the centrifugate, the standing above the sediment of the solid particles liquid silicon compounds, the work-up of the liquid silicon compounds can connect directly. The solids concentration in the centrifugate is preferably at most 50 ppm, particularly preferably at most 20 ppm,
insbesondere höchstens 10 ppm. in particular at most 10 ppm.
Der Umgebungsdruck bei der Zentrifugation beträgt vorzugsweise mindestens 0,1 bar, besonders bevorzugt mindestens 0,5 bar und
vorzugsweise höchstens 100 bar, besonders bevorzugt höchstens 10 bar, insbesondere höchstens 3 bar. The ambient pressure during the centrifugation is preferably at least 0.1 bar, particularly preferably at least 0.5 bar and preferably at most 100 bar, more preferably at most 10 bar, in particular at most 3 bar.
Die Temperatur bei der Zentrifugation beträgt vorzugsweise mindestens 0 °C, besonders bevorzugt mindestens 10 °C und vorzugsweise höchstens 100 °C, insbesondere höchstens 70 °C. The temperature during the centrifugation is preferably at least 0 ° C, more preferably at least 10 ° C and preferably at most 100 ° C, especially at most 70 ° C.
Vorzugsweise werden bei der kontinuierlichen Zentrifugation Tellerseparatoren eingesetzt. Preferably, plate separators are used in continuous centrifugation.
Vorzugsweise sind die flüssigen Siliciumverbindungen und Feststoffpartikel enthaltenden Gemische die als Rohsilan bezeichneten Produktgeniische aus der Herstellung von Preferably, the mixtures containing liquid silicon compounds and solid particles are the product genes known as crude silane from the production of
Methylchlors ilanen nach Müller - Rochow und der Methylchlorosil ilanes after Müller - Rochow and the
Chlorsilanherstellung . Die Organosiliciumverbindungen sind vorzugsweise Methylchlorsilane , Oligosilane, Carbosilane, Siloxane und hochsiedende Crackprodukte davon. Die Chlorosilane production. The organosilicon compounds are preferably methylchlorosilanes, oligosilanes, carbosilanes, siloxanes and high-boiling cracking products thereof. The
Feststoffpartikel enthaltenden Gemische können auch Solid particles containing mixtures can also
Methylchlorid enthalten. Contain methyl chloride.
Das Rohsilan hat vorzugsweise hat eine Feststoffkonzentration von mindestens 0,01 % und höchstens 10%. The crude silane preferably has a solids concentration of at least 0.01% and at most 10%.
In den folgenden Beispielen sind, falls jeweils nicht anders angegeben, alle Mengenangaben auf das Gewicht bezogen, alle Drücke 0,10 MPa (abs . ) und alle Temperaturen 20°C.
Ermittlung der maximal möglichen Absenkung des Partikelgehaltes von Rohsilan mittels Zentrifugation In the following examples, all amounts are by weight unless otherwise indicated, all pressures are 0.10 MPa (abs.) And all temperatures are 20 ° C. Determination of the maximum possible reduction of the particle content of crude silane by means of centrifugation
Versuchsdurchführung Experimental Procedure
Ein Rohgas aus der Methylchlorsilansynthese nach Müller - Rochow wurde in einem Zyklon von ausgetragenen Partikeln gereinigt. Das Rohsilan enthielt noch Schwebstoffe A crude gas from the methylchlorosilane synthesis according to Müller-Rochow was purified in a cyclone of discharged particles. The crude silane still contained suspended matter
(Metallsalzpartikel) , die mittels Zentrifugation abgetrennt wurden. Mittels Variation der Drehzahl und der (Metal salt particles), which were separated by centrifugation. By means of variation of the speed and the
Zentrifugationsdauer wurde die maximal mögliche Abtrennrate ermittelt . Centrifugation the maximum possible separation rate was determined.
Analytik und Ergebnisse Analytics and results
Mittels Elementaranalyse wurde der Gehalt an einem Metallsalz im klaren Zentrifugat mit dem Metallsalzgehalt des Rohsilans von 4 ppm verglichen. By elemental analysis, the content of a metal salt in the clear centrifugate was compared with the metal salt content of the crude silane of 4 ppm.
Die Metallsalz -Reduzierung nach einer Zentrifugationsdauer von jeweils 5 Minuten bei unterschiedlicher Drehzahl von 2000, 3500, und 5000 UpM und 10 Minuten bei 5000 UpM sind in der Tabelle gegenübergestellt: The metal salt reduction after a centrifugation time of 5 minutes at different speeds of 2000, 3500, and 5000 rpm and 10 minutes at 5000 rpm are compared in the table:
Claims
1. Trennverfahren für Feststoffpartikel und flüssige 1. Separation process for solid particles and liquid
Siliciumverbindungen enthaltende Gemische durch By silicon compounds containing mixtures
Zentrifugation. Centrifugation.
2. Verfahren nach Anspruch 1, bei dem Produktgemische der 2. The method of claim 1, wherein the product mixtures of
Herstellung von Methylchlorsilanen nach Müller - Rochow filtriert werden. Production of methylchlorosilanes to Müller - Rochow be filtered.
3. Verfahren nach Anspruch 1, bei dem Produktgemische aus der Chlorsilanherstellung filtriert werden. 3. The method of claim 1, are filtered in the product mixtures from the Chlorsilanherstellung.
4. Verfahren nach Anspruch 1 bis 3, bei dem die Relative 4. The method according to claim 1 to 3, wherein the relative
Zentrifugalbeschleunigung RZB nach DIN 58970-2 mindestens 500 g beträgt. Centrifugal acceleration RZB according to DIN 58970-2 is at least 500 g.
5. Verfahren nach Anspruch 1 bis 4, bei dem kontinuierlich in Tellerseparatoren zentrifugiert wird. 5. The method of claim 1 to 4, is centrifuged continuously in Tellerseparatoren.
6. Verfahren nach Anspruch 1 bis 5, bei dem der Austrag des abgetrennten Feststoffpartikel vollkontinuierlich erfolgt. 6. The method of claim 1 to 5, wherein the discharge of the separated solid particles is carried out fully continuously.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102010002096.6 | 2010-02-18 | ||
| DE201010002096 DE102010002096A1 (en) | 2010-02-18 | 2010-02-18 | Separation of particles from mixtures containing liquid silicon compounds |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2011101264A1 true WO2011101264A1 (en) | 2011-08-25 |
Family
ID=43640377
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/EP2011/051615 WO2011101264A1 (en) | 2010-02-18 | 2011-02-04 | Separating out particles from mixtures containing fluid silicon compounds |
Country Status (2)
| Country | Link |
|---|---|
| DE (1) | DE102010002096A1 (en) |
| WO (1) | WO2011101264A1 (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2014171A (en) * | 1978-02-03 | 1979-08-22 | Goldschmidt Ag Th | Process for the manufacture of hexamethyldisilazane |
| US4307242A (en) * | 1980-10-03 | 1981-12-22 | General Electric Company | Process for removing impurities from residual silicon powder |
| DE102004005643B3 (en) * | 2004-02-04 | 2005-07-14 | Degussa Ag | Working up reaction suspensions in an inverted filter centrifuge, useful especially for recovery of triethylamine from preparation of N,O-bis-(trimethylsilyl)acetamide |
-
2010
- 2010-02-18 DE DE201010002096 patent/DE102010002096A1/en not_active Withdrawn
-
2011
- 2011-02-04 WO PCT/EP2011/051615 patent/WO2011101264A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2014171A (en) * | 1978-02-03 | 1979-08-22 | Goldschmidt Ag Th | Process for the manufacture of hexamethyldisilazane |
| US4307242A (en) * | 1980-10-03 | 1981-12-22 | General Electric Company | Process for removing impurities from residual silicon powder |
| DE102004005643B3 (en) * | 2004-02-04 | 2005-07-14 | Degussa Ag | Working up reaction suspensions in an inverted filter centrifuge, useful especially for recovery of triethylamine from preparation of N,O-bis-(trimethylsilyl)acetamide |
Also Published As
| Publication number | Publication date |
|---|---|
| DE102010002096A1 (en) | 2011-08-18 |
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