DE1433361A1 - Process for the production of highly dispersed carbonyl iron powder - Google Patents
Process for the production of highly dispersed carbonyl iron powderInfo
- Publication number
- DE1433361A1 DE1433361A1 DE19641433361 DE1433361A DE1433361A1 DE 1433361 A1 DE1433361 A1 DE 1433361A1 DE 19641433361 DE19641433361 DE 19641433361 DE 1433361 A DE1433361 A DE 1433361A DE 1433361 A1 DE1433361 A1 DE 1433361A1
- Authority
- DE
- Germany
- Prior art keywords
- production
- highly dispersed
- iron powder
- carbonyl iron
- zone
- 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
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
- B22F9/305—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/20—Dry methods smelting of sulfides or formation of mattes from metal carbonyls
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
Description
N '/,OR H'.;.13M,LUiJü VOi IKiCHT)ISFiSHSM «CA HiJOt ι HiKIS ¥SH Pi JLVBBN '/, OR H'.;. 13M, LUiJü VOi IKiCHT) ISFiSHSM «CA HiJOt ι HiKIS ¥ SH Pi JLVBB
Die vorliegende lirfill·lung betrifft ein Verfahren zur Herstel- ^ von iiochdiapersem larbonyleiseipulver, welches als wertvolles ferro..la^notiachos i.fatex'ial boiia Herstellen von laagnefcdielektrischen Kernen dient und in der Riidiotechnik und der Drahtfernineldetechnik zur Anwendung gelangt.The present filling relates to a method for manufacturing ^ of iiochdiapersem larbonyle ice powder, which is considered valuable ferro..la ^ notiachos i.fatex'ial boiia Manufacture of laagnefcdielectric Cores serves and in the Riidiotechnik and the wire remote technology is applied.
Ea ist bekannt und ^eIa* igt zur praktischen Λην/endung ein Ver- ( fahren zur Herstellung von hoehdisperaei:i Carbonyleisenpulver durch na.Mpfphasenzcrsetaung von isi^enpentokarbonyl in Ge£?enwart von Ammoniak beim zuneluaenden 'l1e.:ipurnturgradi<enten nach der Reaktion $e(C0)caPe+5 CO in horizontalen oder vertikalen Iteaktoren·Ea is known and ^ EIA * igt practical Λην / ending a comparison (go for the production of hoehdisperaei: i carbonyl by na.Mpfphasenzcrsetaung isi ^ enpentokarbonyl in Ge £ enwart of ammonia in zuneluaenden 'l 1 e.:ipurnturgradi < ducks after the reaction $ e (C0) caPe + 5 CO in horizontal or vertical iteactors
Bei der Arbeit in horizontalen Reaktoren entsteht eine große Menge von ICoiapakteiaen, und das anfallende ilarbonyieioen,ulver wird durch Beiiicn^jiuioea von festem iCo'ulenstoff voriinreiAißt»When working in horizontal reactors, a large one arises Amount of ICoiapakteiaen, and the resulting ilarbonyieioen, becomes ulver torn away by the addition of solid iCo'ulene material »
In vertikalen Iieaktoren f.elingt es bei bekannben tecloiologi— schon He1;! Leu nicht, hochdisporse und zu gleicher Seit schwach auf- ι gekohlte Pulver herzustellen, welche die erforderlichen elektromagnetischen blgenschafte» aufweisen· IiS muß au zu3afcs5.licb.en Operationen, insbesondere zur Reparation der Pulver und au deren Wäraebe— h»ndlunf; ii;. Wasserstoff strom Zuflucht tfuno i-nen v/erden· Dies macht zwar !'löslich, iCarbonylelnenpulver von (^efoi^derter Güte herzustellen, dessen Ausbeute aber beträft .labei lediglieh 2—3?* von dem Gewicht der anfallenden i.'rod.dcte·In vertical actuators, it is possible to achieve he 1 ; It is not necessary to produce highly dispersed and at the same time slightly carbonized powders which have the required electromagnetic properties. ii ;. Hydrogen stream Refuge tfuno i-nen v / erden · This makes it true! 'Soluble to produce carbonyl-lenpowder of (^ efoi ^ derter quality, the yield, however, is only 2 to 3? * Of the weight of the resulting rod. dcte
Das Ziel der vorliegenden ürfindung besteht in der BeseitigungThe aim of the present invention is to eliminate it
BAD ORIGINALBATH ORIGINAL
809812/1108809812/1108
Der Erfindung ^iw£d© die Aufgabe gu^\2ndegeleg:fet @ineThe invention ^ iw £ d © the task gu ^ \ 2ndegeleg: fe t @ine
insbesondere ein Wärmereg±m©f %\w Herstellung von hohes Qualität unmittelbar im Healrtor fiü?especially a heat reg ± m © f % \ w production of high quality directly in the health gate fi?
etee guaatzlish© Behsndluiig des erhaltenenetee guaatzlish © Behsndluiig of the received
Eo wusda Qefvuoaen9 öaß das optimale Begtee zixr'E Ksa?bonjleiseii durch thermisch© Zars©t2img vöhEo wusda Qefvuoaen 9 öass the optimal Begtee zixr'E Ksa? Bonjleiseii through thermal © Zars © t2img vöh
darin besteilt, im Apparat Zones mit feossseqae&t den 5emp©3?atvxsradieaal?©a ©ntstehea zn l©se©a· Die besten WOTö-öB "bei S@mpc^?atuT(aa ersielt * die te den 2oaen in Bweichen gehaltfen %T2Mem obere .Zone 3ö2«-312°öfr sti1#&lea?@divided into it, in the apparatus Zones with feossseqae & t the 5emp © 3? atvxsradieaal? © a © ntstehea zn l © se © a · The best WOTö-öB "at S @ mpc ^? atuT (aa received * the te kept the 2oaen in B Weichten % T2Mem upper .Zone 3œ2 "-312 ° ö fr Sti1 # & lea? @
mteres uüd oberen S©ae beträgt 25^3Oo0e»mteres uüd upper S © ae is 25 ^ 3O o 0e »
Eb v/i^de festgestellt9 daß ws des? ¥©s-t@ilusg aa©Ii der E51a@ des Apparates die 2?eil@ä.^ng^iß# des dessen ©hemischa Sxisammeasetsmig imd folglicliEb v / i ^ de established9 that ws des? ¥ © s-t @ ilusg aa © Ii the E51a @ of the apparatus the 2?eil@ä.^ng^iß# des whose © hemischa Sxisammeasetsmig imd folglicli
abtoanglg siaäe- -Di© SJoiape^atm? del? beeinflußt entscheidend die Seil©hex^p?@Be dae isid©m dies© "bei steigender Temperatur ateäsuatg imd ninBsb mexülichen Eisfluß aszg ά±β oheiaißehe gue^SBaense-öaimg der Bie Seiaperatia? der unteren Zone übt auf die Dispersität der praktisch feeisien Einfluß aus, sie toestinmt aber deren Kohleaateff und Stickstoff und folgliöh die G^öSe des lustf afefcorss im Rajj-leislis^hen Bereich ( 5^) · So fütet ά±@ tussenkong in deae unteren 2one des Beatefeoss ¥öh 320% auf aur Teasvissevuas des Kohlenstoff gehalt es der Pulvea? voa O des Faktors C ^), von Ο»21·1θΓ3 auf 0,abtoanglg siaäe- -Di © SJoiape ^ atm? del? decisively influences the rope © hex ^ p? @Be dae isid © m dies © "with rising temperature ateäsuatg imd ninBsb Mexican ice flow aszg ά ± β oheiaißehe gue ^ SBaense-öaimg the Bie Seiaperatia? of the lower zone exercises on the dispersity of the practically feeisien Influence, but it toestinmt their Kohleaateff and nitrogen and consequently the G ^ öSe of the lustf afefcorss in the Rajj-leislis ^ hen area (5 ^) · So ά ± @ tussenkong in deae lower 2one des Beatefeoss ¥ öh 320% on aur Teasvissevuas the carbon content of the pulvea? voa O of the factor C ^), from Ο »21 · 1θΓ 3 to 0,
8 0 9 8 12/11088 0 9 8 12/1108
Beim Hegi^e der sinkenden Teiiperatur vom oberen zum unteren Teil des Reakto s nimmt die Intensität der Konvektion des Reaktionsgases in dieeeui («ines Gacgeniioches» welches infolge der Zersetzung des Eisenpentakarbonyls entsteht) wesentlich ab, waa zur Herstellung disperserer und schwach aufgekohlter Pulver führt«In the case of the falling partial temperature from the upper to the lower Part of the reaction takes on the intensity of the convection of the reaction gas in dieeeui ("ines Gacgeniioches" which as a result of the decomposition of iron pentacarbonyl arises) significantly, waa for the production more disperse and weakly carburized powder leads to "
Das vorgeheI la^eae Verfahren kann vorzugsweise unter folgenden Te. peraturbedingun ;en durchgei'ü;irt Werdens Temperatur in der oberen Zone des Apparates 302-3120O, in der laiütleren Zone 235-293°« und in dar unteren Zone 275->ßS20C.The previous I la ^ eae method can preferably under the following Te. The temperature in the upper zone of the apparatus is 302-312 0 O, in the outer zone 235-293 ° C and in the lower zone 275-> ßS2 0 C.
Das flüssige ELsenpentakarbonyl in ein r Menge von 10 l/St wird auf 106°0 in einem Verda ipf er vom Jjiüdaapftyp erhitzt und in Form von Dä.ipfen (zusammen uit de.i gasförmigen Auunoni'-k in einer Men e von 412 1/Bt.) in den Reaktor für theriische Zersetzung von etwa M- m Höhe und Of75 a Durchmesser geleitet·. Der Reaktor ist ;.iit einer SektiotiSelektrcheizung versehen» so daß in diesem folgende Beiiqperatiurverteilung gehalten v/irdi oben 3O3-*3Q5°C· in der Mitte 285-290°C und unten 2?5-280°0· Im. "Ergebnis entspricht das iCarbonyleisenpulver, das aus dem Filter in einer iÄenge von 13-21% von der gesamten anfallenden Pulvenaenge ausgetragen wirdf der Qualität nach den Pulvern für Drahtfernmeldetechnik (sie Tabelle).The liquid elenium pentacarbonyl in an amount of 10 l / St is heated to 106 ° 0 in a evaporator of the Jjiüdaapftyp and in the form of vapors (together uit de.i gaseous Auunoni'-k in a quantity of 412 l / Bt.) f into the reactor for decomposition of about theriische M- m height and a diameter O 75 · passed. The reactor is provided with a sectional electric heating system, so that the following temperature distribution is maintained at the top 3O3- * 3Q5 ° C · in the middle 285-290 ° C and below 2? 5-280 ° 0 · Im. "Result the iCarbonyleisenpulver, which is discharged from the filter in a iÄenge of 13-21% of the total incurred Pulvenaenge f corresponds to the quality after the powders for wire telecommunications (they table).
Das flüssige Eisenpantaicarbonyl in einer Menge von 39 1/St9 wird auf 108,5^C la einem Verda ipf er vom Kinde «pftyp erlitt zt und In Form von Dämpfen (zusammen mit dem gasförmigen Ammoniak in ei— Menge von 1629 l/St) in den Reaktor für theraische ZersetzungThe liquid Eisenpantaicarbonyl in an amount of 39 1 / St 9 108.5 ^ C la a Verda he IPF together the Child "pftyp suffered zt and in the form of vapors (with the gaseous ammonia in egg quantity 1629 l / h ) into the reactor for theraic decomposition
809812/1108809812/1108
«μ* 5 » 8fe* «Alt &Bttam$gf «5*Ui*·*, wm BmIiIw alt *tMQt MIA Mt fllart ιίίΰliw^ m@i«0«t*tf die la «N& Si»»«Μ * 5» 8fe * «Alt & Bttam $ gf« 5 * Ui * · *, wm BmIiIw alt * tMQt MIA Mt fllart ιίίΰliw ^ m @ i «0« t * tf the la «N & Si» »
««er lit«· HN^% «d «tstatt 2?^®a8%# X« mi tilt«* 19^(91 B*Iv«f (tteriMB ·1η4 3a datr«« Er lit «· HN ^%« d «t instead of 2? ^ ®a8% # X« mi tilt «* 19 ^ (91 B * Iv« f (tteriMB · 1η4 3a datr
tabelle <HiflPa3cteristlk 4m table <HiflPa3cteristlk 4m
mc*·* ia «ia«i ÜMlün «^l im «κ& Ia «Sjwi earttsw« mm· tunmc * · * ia «ia« i ÜMlün «^ l im« κ & Ia «Sjwi earttsw« mm · do
O/Οβ I* liar»O / Οβ I * liar »
EtiiselvörlußtfäkrtorenEtiiselvörlußtfäkrtoren
809812/1108809812/1108
f«liMftflfctor fürf «liMftflfctor for
ttakoeit&t UJQd Wlrbelatrömettakoeit & t UJQd Wlrbelatröme
(fouoeult-etröme)* « ^^.10"^ 0#5-»1f0 1t0(fouoeult-etröme) * «^^. 10" ^ 0 # 5- »1 f 0 1 t 0
der fla^etisieruas* - <?^·10"^ ο *^&" 0,2der fla ^ etisieruas * - <? ^ · 10 "^ ο * ^ &" 0.2
bad ORiQf^bad ORiQf ^
Elektromagnetische Parameter Dirnen·» Bereich— Bei- Bei··Electromagnetic parameters prostitutes · »Range— At- At ··
flion Muig spiel 1 spiel 2flion Muig game 1 game 2
Temperaturkoeffizient der laagne- von +20Temperature coefficient of laagne- of +20
tischen Anfangspermeabilität 0O"1 •Κ^ΙΟ*6 Di» -50 50 Belative Güte zylindrischer £ej>»table initial permeability 0 O " 1 • Κ ^ ΙΟ * 6 Di» -50 50 Belative quality cylindrical £ ej> »
ne bei einer Frequenz von 5 MHa * %q% 2»°^ 2»°° läffektive magnetische Permeabilität bei einer Frequenz von 5 HH* - J^ 3tO5 3*00 Relative Güte zylindrischer Kerne bei einer Frequenz von 50 MHs - Q» ^ 0»98 Of95 Effektive magnetische Permeabilität bei einer Frequenz von 50 Mz - M'ett 1·^° 1f60 ne at a frequency of 5 MHa * % q% 2 »° ^ 2 » °° effective magnetic permeability at a frequency of 5 HH * - J ^ 3tO5 3 * 00 Relative quality of cylindrical cores at a frequency of 50 MHs - Q »^ 0 »98 O f 95 Effective magnetic permeability at a frequency of 50 Mz - M'ett 1 · ^ ° 1f60
Ba sei darauf hingewiesen» daß in der vorliegenden Erfindung die Technologie zur Herstellung von hochdisperseia schwach aufgekohltem Karbonyleiaenpulvor entwickelt istt das sich einmal für ( die Apparatur ä#s Drahtfernmeldetechnik dank den geringen Werten von Einsselverlustfaktoren dieses Pulvers und zum anderen für radio*· technische Zwacke dank den hohen Werten der relativen Güte und der effektiven magnetischen PermeaaMlität des Pulvers in einem breiten Frequenzbereich eignet, was durch die in der Tabelle enthaltenen Angaben gut charakterisiert wird*Ba should be noted "that has developed the technology for the production of hochdisperseia weak carburized Karbonyleiaenpulvor in the present invention t the once for (the apparatus ä # s wire telecommunications, thanks to the low values of one Selver pleasure factors of this powder and the other for radio * · technical Zwacke Thanks to the high values of the relative quality and the effective magnetic permeability of the powder, it is suitable for a wide frequency range, which is well characterized by the information in the table *
809812/1108809812/1108
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DES0094341 | 1964-11-26 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1433361A1 true DE1433361A1 (en) | 1968-12-12 |
Family
ID=7518630
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19641433361 Pending DE1433361A1 (en) | 1964-11-26 | 1964-11-26 | Process for the production of highly dispersed carbonyl iron powder |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1433361A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2535073A1 (en) * | 1975-08-06 | 1977-02-17 | Hoechst Ag | METHOD OF PREPARING TERTIAER ALIPHATIC AMINES |
| DE3428121A1 (en) * | 1984-07-31 | 1986-02-13 | Basf Ag, 6700 Ludwigshafen | METHOD FOR PRODUCING IRON POWDER |
| WO2021123385A1 (en) | 2019-12-20 | 2021-06-24 | Basf Se | Optimized powder production |
-
1964
- 1964-11-26 DE DE19641433361 patent/DE1433361A1/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2535073A1 (en) * | 1975-08-06 | 1977-02-17 | Hoechst Ag | METHOD OF PREPARING TERTIAER ALIPHATIC AMINES |
| DE3428121A1 (en) * | 1984-07-31 | 1986-02-13 | Basf Ag, 6700 Ludwigshafen | METHOD FOR PRODUCING IRON POWDER |
| WO2021123385A1 (en) | 2019-12-20 | 2021-06-24 | Basf Se | Optimized powder production |
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