NO156084B - PROCEDURE FOR THE PREPARATION OF ALUMINUM PHOSPHIDE AND / OR MAGNESIUM PHOSPHIDE OR A MIXTURE PHOSPHIDE OF ALUMINUM AND MAGNESIUM. - Google Patents
PROCEDURE FOR THE PREPARATION OF ALUMINUM PHOSPHIDE AND / OR MAGNESIUM PHOSPHIDE OR A MIXTURE PHOSPHIDE OF ALUMINUM AND MAGNESIUM. Download PDFInfo
- Publication number
- NO156084B NO156084B NO821427A NO821427A NO156084B NO 156084 B NO156084 B NO 156084B NO 821427 A NO821427 A NO 821427A NO 821427 A NO821427 A NO 821427A NO 156084 B NO156084 B NO 156084B
- Authority
- NO
- Norway
- Prior art keywords
- phosphide
- magnesium
- phosphorus
- reaction vessel
- aluminum
- Prior art date
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims description 18
- 239000011777 magnesium Substances 0.000 title claims description 18
- 229910052749 magnesium Inorganic materials 0.000 title claims description 18
- 238000000034 method Methods 0.000 title claims description 12
- 229910052782 aluminium Inorganic materials 0.000 title claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 10
- 239000005953 Magnesium phosphide Substances 0.000 title claims description 8
- IHGSAQHSAGRWNI-UHFFFAOYSA-N 1-(4-bromophenyl)-2,2,2-trifluoroethanone Chemical compound FC(F)(F)C(=O)C1=CC=C(Br)C=C1 IHGSAQHSAGRWNI-UHFFFAOYSA-N 0.000 title claims description 4
- 239000000203 mixture Substances 0.000 title description 11
- 229910052751 metal Inorganic materials 0.000 claims description 34
- 239000002184 metal Substances 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 12
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 4
- 150000002739 metals Chemical class 0.000 claims description 3
- 239000011541 reaction mixture Substances 0.000 claims description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 40
- 229910052698 phosphorus Inorganic materials 0.000 description 40
- 239000011574 phosphorus Substances 0.000 description 40
- 239000007789 gas Substances 0.000 description 9
- 238000003860 storage Methods 0.000 description 8
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 6
- 239000011630 iodine Substances 0.000 description 6
- 229910052740 iodine Inorganic materials 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000007306 turnover Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004260 weight control Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc 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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
- C01B25/082—Other phosphides of boron, aluminium, gallium or indium
- C01B25/085—Other phosphides of boron, aluminium, gallium or indium of aluminium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
- C01B25/081—Other phosphides of alkali metals, alkaline-earth metals or magnesium
Description
Foreliggende oppfinnelse vedrører en fremgangsmåte til fremstilling av aluminiumfosfid og/eller magnesiumfosfid eller et blandingsfosfid av aluminium og magnesium. The present invention relates to a method for producing aluminum phosphide and/or magnesium phosphide or a mixed phosphide of aluminum and magnesium.
Gjenstanden for norsk patentsøknad nr. 803141 (ålment til-gjengelig fra 13.5.1981) er en fremgangsmåte til fremstilling av fosfider av aluminium eller magnesium, hvor de finfordelte metaller, eller en legering av de to metaller ved en temperatur mellom 300 og 600°C i inertgassatmosfære og i nærvær av klor, brom, jod eller en forbindelse av de nevnte elementer med fosfor, svovel, hydrogen, ammonium, zink eller metallet som skal omsettes som katalysator, omsettes med gult fosfor. The subject of Norwegian patent application no. 803141 (generally available from 13.5.1981) is a method for producing phosphides of aluminum or magnesium, where the finely divided metals, or an alloy of the two metals at a temperature between 300 and 600°C in an inert gas atmosphere and in the presence of chlorine, bromine, iodine or a compound of the aforementioned elements with phosphorus, sulphur, hydrogen, ammonium, zinc or the metal to be reacted as a catalyst, is reacted with yellow phosphorus.
Etter en spesielt foretrukket utførelsesform blandes i According to a particularly preferred embodiment, mix in
første rekke godt det finpulveriserte eller grusformede metall med katalysatoren. Blandingen oppvarmes i et egnet lukkbart reaksjonskar i inertgassatmosfæren, eksempelvis under nitrogen ved normaltrykk til reaksjonstemperaturen mellom 300 og 600°C. Når den ønskede reaksjonstemperatur er nådd, tildoseres flytende gult fosfor med slik hastighet at den frigjorte reaksjonsvarme kan bortføres uten problem og temperaturen kan holdes i området mellom 300 og 600°C. first row well the finely powdered or gravel-shaped metal with the catalyst. The mixture is heated in a suitable closable reaction vessel in the inert gas atmosphere, for example under nitrogen at normal pressure to the reaction temperature between 300 and 600°C. When the desired reaction temperature has been reached, liquid yellow phosphorus is added at such a rate that the released heat of reaction can be removed without problem and the temperature can be kept in the range between 300 and 600°C.
Det er nå funnet at denne fremgangsmåte ved hjelp av en fremgangsmåteendring kan utformes enda sikrere og lettere beherskbar og fremfor alt del- eller sågar helkontinuerlig, når man også tildoserer det finfordelte metall langsomt i reaksjonskaret. It has now been found that, with the help of a process change, this method can be designed even safer and easier to control and, above all, partially or even completely continuous, when the finely divided metal is also dosed slowly into the reaction vessel.
Fremgangsmåten ifølge oppfinnelsen er følgelig karakterisert ved at det gule fosfor i flytende form og det finfordelte metall tildoseres samtidig og langsomt i reaksjonskaret. The method according to the invention is consequently characterized in that the yellow phosphorus in liquid form and the finely divided metal are dosed simultaneously and slowly into the reaction vessel.
Gjennomføres fremgangsmåten ifølge oppfinnelsen i et i det vesentlige sylindrisk reaksjonskar, som oppvarmes over den nedre bunn, så danner det seg tydelig fire forskjellige soner som ovenifra og nedad kan beskrives som følger: 1. sone: I denne øverste sone eksisterer bare gass, nemlig en blanding av den anvendte inertgass og fosfordamp. Da det i denne sone i de mest ekstreme tilfeller bare hersker en maksimaltemperatur på ca. 200° er fosforets damptrykk relativt lavt, således at gassblandingen hovedsakelig består av den anvendte inertgass. If the method according to the invention is carried out in an essentially cylindrical reaction vessel, which is heated above the lower bottom, then four distinct zones are clearly formed which can be described from top to bottom as follows: 1st zone: In this uppermost zone only gas exists, namely a mixture of the inert gas used and phosphorus vapor. As in this zone, in the most extreme cases, only a maximum temperature of approx. At 200°, the vapor pressure of the phosphorus is relatively low, so that the gas mixture mainly consists of the inert gas used.
2. sone: Her er fordampningssonen av det gule fosfor. 2nd zone: Here is the evaporation zone of the yellow phosphorus.
I denne sone hersker temperaturer som ligger litt over det gule fosfors kokepunkt. Også i denne sone eksisterer bare gass som nå riktignok for den største del består av fosfordamp. 3. sone: Her befinner det seg nå i det øverste sjikt av beholderfyllingen den egentlige reaksjonssone, hvori fosfordamp kommer i berøring med dét finfordelte metall og det allerede dannede fosfid. In this zone, temperatures slightly above the boiling point of yellow phosphorus prevail. Also in this zone, only gas exists, which now, admittedly, for the most part consists of phosphorus vapour. 3rd zone: Here, in the topmost layer of the container filling, is the actual reaction zone, in which phosphorus vapor comes into contact with the finely divided metal and the already formed phosphide.
I denne sone som befinner seg på reaksjonstemperatur mellom 300 og 600°C, foregår det en sterkt eksoterm reaksjon mellom fosfordampen og det finfordelte metall. Da fosfordampen reagerer meget hurtig med metallet, trenger den ikke meget dypt inn i beholderfyllingen, men bare ca. 10-15 cm. Innen beholderfyllingen blir derfor gassfasen i retning ovenifra og nedad meget hurtig fattigere på fosfordamp. 4. sone: I denne nederste sone består gassfasen praktisk talt bare enda av inertgass, fordi fosfordampen ikke trenger inn i denne dybde. Det faste stoff består praktisk talt bare av det dannede fosfid og inneholder i alle fall mindre mengder av ikke-omsatt metall. Et mindre overskudd av metall gir sikkerhet for at det dannede fosfid er fritt for fosfor. In this zone, which is at a reaction temperature between 300 and 600°C, a strongly exothermic reaction takes place between the phosphorus vapor and the finely divided metal. As the phosphorus vapor reacts very quickly with the metal, it does not penetrate very deeply into the container filling, but only approx. 10-15 cm. Before the container is filled, therefore, the gas phase in the direction from top to bottom very quickly becomes poorer in phosphorus vapour. 4th zone: In this lowest zone, the gas phase practically only consists of inert gas, because the phosphorus vapor does not penetrate to this depth. The solid consists practically only of the phosphide formed and in any case contains smaller amounts of unreacted metal. A small excess of metal ensures that the phosphide formed is free of phosphorus.
Utformingen av de ovenfor omtalte fire soner innen reaksjonskaret muliggjør nå en spesielt enkel og fullstendig sikker utføringsform av fremgangsmåten ifølge oppfinnelsen. Derved tildoseres det flytende gule fosfor kontinuerlig i den øvre del av reaksjonskaret, altså i gassrommet over beholderfyllingen, hvor det uhindret kan fordampe. Spesielt fordelaktig er det når inngangsåpningen for det flytende fosfor befinner seg helt øverst i reaksjonskaret, altså i den øvre 1. sone. The design of the above-mentioned four zones within the reaction vessel now enables a particularly simple and completely safe embodiment of the method according to the invention. Thereby, the liquid yellow phosphorus is continuously dosed in the upper part of the reaction vessel, i.e. in the gas space above the container filling, where it can evaporate unimpeded. It is particularly advantageous when the entrance opening for the liquid phosphorus is located at the very top of the reaction vessel, i.e. in the upper 1st zone.
Det finfordelte metall kan riktignok også tildoseres i den The finely divided metal can of course also be dosed into it
øvre ende av reaksjonskaret. Da gjør imidlertid en hurtig og heftig omsetning med den allerede i høy konsentrasjon foreliggende fosfordamp anvendelsen av spesielle lukkeorganer for inngangsåpningene nødvendig for at inntrengning av fosfordamp i transportorganet for det finfordelte metall kan hindres. Det er derfor fordelaktig å tildosere det finfordelte metall kontinuerlig i den nedre del av reaksjonskaret, nemlig således at inngangsåpningen ligger i området for beholderfyllingen. Dette kan foregå i ovennevnte 3. sone av den egentlige reaksjonssone. Det er da hensiktsmessig om-trent i høyde ved inngangsåpningen for metallet å anordne et røreorgan, hvis transportelementer beveger beholderfyllingen langs beholderomkretsen og således sørge for en jevn fordeling av nytildosert metall i reaksjonssonene. Enda mer fordelaktig er det imidlertid når tildoseringen av finfordelt metall foregår i den nederste del av reaksjonskaret, altså i ovennevnte 4. sone. I dette tilfellet er det hensiktsmessig å anordne et røreorgan, hvis transportelement beveger beholderfyllingen langs beholderomkretsen og samtidig sørger for en vertikal gjennomblanding. upper end of the reaction vessel. In that case, however, a rapid and vigorous turnover with the phosphorus vapor already present in high concentration makes the use of special closing means for the entrance openings necessary so that penetration of phosphorus vapor into the transport means for the finely divided metal can be prevented. It is therefore advantageous to dose the finely divided metal continuously into the lower part of the reaction vessel, namely in such a way that the entrance opening is in the area for the container filling. This can take place in the above-mentioned 3rd zone of the actual reaction zone. It is then appropriate to arrange a stirrer at approximately the height of the entrance opening for the metal, whose transport elements move the container filling along the container perimeter and thus ensure an even distribution of newly dosed metal in the reaction zones. However, it is even more advantageous when the addition of finely divided metal takes place in the lower part of the reaction vessel, i.e. in the above-mentioned 4th zone. In this case, it is appropriate to arrange a stirring device, whose transport element moves the container filling along the container perimeter and at the same time ensures vertical mixing.
På den omtalte måte er det mulig kontinuerlig å tildosere ekvivalente mengder av finfordelt metall, som inneholder inn-blandet katalysator, og flytende gult fosfor i reaks jonskaret og under reaksjonen fra den nederste del av reaksjonskaret, altså fra ovennevnte 4. sone , å utta det dannede fosfid, som er fritt for ikke-omsatt fosfor. Uttaket foregår gjenncm en åpning ved reaksjonskarets bunn. Den In the manner described, it is possible to continuously dose equivalent amounts of finely divided metal, which contains mixed catalyst, and liquid yellow phosphorus into the reaction ion vessel and during the reaction from the lower part of the reaction vessel, i.e. from the above-mentioned 4th zone, to discharge it formed phosphide, which is free of unreacted phosphorus. The withdrawal takes place through an opening at the bottom of the reaction vessel. It
kan foretas etter valg kontinuerlig eller porsjonsvis. can be carried out continuously or in portions according to choice.
Ved kontinuerlig uttak uttas produktet i den nøyaktig til With continuous withdrawal, the product in it is withdrawn exactly until
den kontinuerlige tildoserte metall og fosfor svarende mengde. Likeledes er det imidlertid også mulig at man lar den nederste sone i reaksjonskaret, altså ovennevnte 4. sone, langsomt bygge seg opp <p>g deretter porsjonsvis uttar det dannede fosfid. Derved må det imidlertid påsees at virkelig bare material fra denne 4. sone tas ut, som ikke mer inneholder ikke-omsatt fosfor, og ikke f.eks. også material fra reaksjonssonen, hvilket kan foregå ved vektkontroll. the continuous dosed metal and phosphorus equivalent amount. Likewise, however, it is also possible to allow the lowest zone in the reaction vessel, i.e. the above-mentioned 4th zone, to slowly build up <p>g then take out the formed phosphide in portions. In doing so, however, it must be ensured that only material from this 4th zone is taken out, which no longer contains unconverted phosphorus, and not e.g. also material from the reaction zone, which can take place during weight control.
Tildoseres det finfordelte metall som omtalt ovenfor, i den nedre del av reaksjonskaret, altså i ovennevnte 3. eller 4. sone, så er det tilstrekkelig som doseringsorgan å anvende en vanlig transportsnekke, fordi den faste sandformede beholder-fylling samtidig tjener som lukkeorgan. Skal fremgangsmåten ifølge oppfinnelsen nystartes i et tomt reaksjonskar er det derfor hensiktsmessig i første rekke bare å innføre finfordelt metall inntil inngangsåpningen for metall er overdekket, og først deretter å begynne med den langsomme tildosering av flytende fosfor. Enda mer fordelaktig er det imidlertid hvis reaksjonskaret i første rekke fylles en gang til over inngangsåpningen for metallet med det tilsvarende fosfid fra en tidligere produksjon og deretter samtidig begynner med dosering av flytende fosfor og finfordelt metall. If the finely divided metal as mentioned above is dosed in the lower part of the reaction vessel, i.e. in the above-mentioned 3rd or 4th zone, then it is sufficient as a dosing device to use an ordinary transport auger, because the solid sand-shaped container filling also serves as a closing device. If the method according to the invention is to be restarted in an empty reaction vessel, it is therefore appropriate in the first instance only to introduce finely divided metal until the entrance opening for metal is covered, and only then to begin with the slow addition of liquid phosphorus. It is even more advantageous, however, if the reaction vessel is first filled once more above the entrance opening for the metal with the corresponding phosphide from a previous production and then simultaneously begins dosing liquid phosphorus and finely divided metal.
Oppfinnelsen skal forklares nærmere ved hjelp av noen eksempler. Alle prosentangivelser er vektprosent, hvis intet annet er angitt. The invention will be explained in more detail with the help of some examples. All percentages are by weight, unless otherwise stated.
Eksemp_el_l Example_el_l
Som reaksjonskar tjente en sylindrisk beholder med en dia-meter på ca. 80 cm og en høyde på ca. 100 cm, som var utstyrt med rører og røreorgan, et kjølesystem, temperatur-følere i forskjellige høyder, tilførsel for inertgass og en avgassledning. Bunnen av beholderen var oppvarmbar ved hjelp av en gassbrenner utenifra til temperaturer inntil 5 00°C. Tilsluttet var et forrådskar for flytende gult fosfor med en pumpe som etter valg muliggjør å sirkulere det flytende gule fosfor i forrådskaret eller å indosere det i reaksjonskaret, samt et forrådskar for finfordelt metall som skal omsettes med et transportorgan for tildosering av metall i reaksjonskaret. Ved bunnen av reaksjonskaret befant det seg en liten med et lukkeorgan utstyrt åpning til uttak av produktet. Av sikkerhetsgrunner var reaksjonskaret utstyrt med en rysteskive for å imøtegå en mulig trykkøkning. Reaksjonskaret ble før og etter omsetningen spylt med nitrogen, under omsetningen ble reaksjonsblandingen overlagret med argon. Avgassen ble bortledet over et vannforlag med et glassfiberfilter og et etterkoblet aktivkullfilter. A cylindrical container with a diameter of approx. 80 cm and a height of approx. 100 cm, which was equipped with stirrers and stirrers, a cooling system, temperature sensors at different heights, supply for inert gas and an exhaust gas line. The bottom of the container could be heated using a gas burner from the outside to temperatures up to 500°C. Attached was a storage vessel for liquid yellow phosphorus with a pump which, by choice, enables the liquid yellow phosphorus to be circulated in the storage vessel or to be dosed into the reaction vessel, as well as a storage vessel for finely divided metal which is to be exchanged with a transport device for dosing metal into the reaction vessel. At the bottom of the reaction vessel there was a small opening equipped with a closing device for withdrawing the product. For safety reasons, the reaction vessel was equipped with a shaking disc to counter a possible pressure increase. The reaction vessel was flushed with nitrogen before and after the reaction, during the reaction the reaction mixture was superimposed with argon. The exhaust gas was led away over a water source with a glass fiber filter and a subsequent activated carbon filter.
Før begynnelsen av omsetningen befant det seg i reaksjonskaret 50 kg magnesiumfbsfid fra en tidligere produksjon, i forrådskaret for metall en blanding av 200 kg magnesium og 0,8 kg jod, i forrådskaret for flytende fosfor ble dette omvalset. Nå ble reaksjonskaret ved bunnen oppvarmet til 300°C. Deretter ble det inndosert 10 kg magnesium i reaksjonskaret og tildosering av flytende fosfor begynte med en hastighet fra 0,4-1 kg pr. minutt. Samtidig ble det også tildosert ytterligere magnesium. Ved hjelp av reaksjonsvarmen øker temperaturen i den nedre del av reaksjonskaret til 550°C. Before the start of the turnover, there was in the reaction vessel 50 kg of magnesium fbsfide from a previous production, in the storage vessel for metal a mixture of 200 kg of magnesium and 0.8 kg of iodine, in the storage vessel for liquid phosphorus this was re-rolled. Now the reaction vessel at the bottom was heated to 300°C. Next, 10 kg of magnesium was dosed into the reaction vessel and dosing of liquid phosphorus began at a rate of 0.4-1 kg per minute. At the same time, additional magnesium was also dosed. With the help of the reaction heat, the temperature in the lower part of the reaction vessel increases to 550°C.
Nå ble tildosering av fosfor og magnesium avstemt, således at temperaturen ble holdt på 550°C og vektforhold mellom fosfor og magnesium utgjorde rundt 0,85 : 1. Etter at det i reaksjonskaret hadde dannet seg rundt 180 kg magnesiumfosfid ble det i løpet av 10 minutter under fortløpende videre tildosering av fosfor og magnesium uttatt 100 kg produkt gjennom uttaksåpningen. Uttaksåpningen ble igjen lukket. Etter at det på nytt hadde dannet seg ca. 180 kg magnesiumfosfid ble dette igjen uttatt og endelig ble hele prosessen gjentatt enda en gang. Etter forbruk av ifylt 200 kg magnesium ble tildoseringen av fosfor innstilt. Produktet som enda befant seg i reaksjonskaret ble enda Now the addition of phosphorus and magnesium was coordinated, so that the temperature was kept at 550°C and the weight ratio between phosphorus and magnesium amounted to around 0.85:1. After around 180 kg of magnesium phosphide had formed in the reaction vessel, within 10 minutes during continuous further dosing of phosphorus and magnesium, 100 kg of product was withdrawn through the withdrawal opening. The outlet opening was closed again. After it had formed again approx. 180 kg of magnesium phosphide was taken out again and finally the whole process was repeated once more. After consumption of the filled 200 kg of magnesium, the addition of phosphorus was stopped. The product that was still in the reaction vessel remained
en gang kort oppvarmet og tatt ut. Innbefattende det i reaksjonskaret ifylte magnesiumfosfid ble det i løpet av 5 timer uttatt 415 kg produkt med et magnesiumfosfidinnhold once briefly heated and taken out. Including the magnesium phosphide filled in the reaction vessel, 415 kg of product with a magnesium phosphide content was withdrawn within 5 hours
på 92%. of 92%.
Eksemp_el_2 Example_el_2
I det i eksempel 1 omtalte reaksjonskar ble det fylt en blanding av 100 kg magnesium og 0,3 kg jod, i forrådskaret for metall befant det seg en blanding av ytterligere 150 kg magnesium og 0,5 kg jod. Nå ble reaksjonskaret ved bunnen oppvarmet til 300°C. Deretter ble fosfor tildosert med slik hastighet at temperaturen i den nedre del av reaksjonskaret! langsomt økte til 550°C. Ved styring av fosfortildoseringen ble denne temperatur opprettholdt inntil det tilsammen var forbrukt 82 kg fosfor. Deretter ble samtidig magnesium og fosfor tildosert i vektforhold 1:0,83 med slik hastighet at temperaturen i den nedre del av reaksjonskaret stadig forble mellom 500 og 550°C. Samtidig ble det gjennom uttaksåpningen kontinuerlig uttatt produkter i slike mengder at det tilsvarte nøyaktig den tilsatte mengde av magnesium og fosfor, tilsammen altså 150 kg magnesium og 123 kg fosfor. Deretter ble det produkt som enda befant seg i reaksjonskaret enda en gang kort oppvarmet og uttatt videre kontinuerlig. Utbyttet utgjorde tilsammen 450 kg med et gjennom-snittlig innhold av magnesiumfosfid på 90%. In the reaction vessel mentioned in example 1, a mixture of 100 kg magnesium and 0.3 kg iodine was filled, in the storage vessel for metal there was a mixture of a further 150 kg magnesium and 0.5 kg iodine. Now the reaction vessel at the bottom was heated to 300°C. Phosphorus was then dosed at such a rate that the temperature in the lower part of the reaction vessel! slowly increased to 550°C. When controlling the phosphorus dosage, this temperature was maintained until a total of 82 kg of phosphorus had been consumed. Magnesium and phosphorus were then dosed at the same time in a weight ratio of 1:0.83 at such a rate that the temperature in the lower part of the reaction vessel constantly remained between 500 and 550°C. At the same time, products were continuously withdrawn through the withdrawal opening in such quantities that it corresponded exactly to the added amount of magnesium and phosphorus, i.e. a total of 150 kg of magnesium and 123 kg of phosphorus. Then, the product that was still in the reaction vessel was once again briefly heated and withdrawn continuously. The yield totaled 450 kg with an average magnesium phosphide content of 90%.
Eksemp_el_3_ Example_el_3_
I det i eksempel 1 omtalte reaksjonskar ble det fylt en blanding av 50 kg av en sandformet aluminium-magnesium-legering med et magnesiuminnhold på 5% og 0,2 kg jod, i forrådskaret for metall befant det seg en blanding av ytterligere 200 kg av nevnte legering og 0,6 kg jod. Nå ble reaksjonskaret ved bunnen oppvarmet til 450°C. Deretter ble det begynt med tildosering av fosfor og legering. Derved ble fosforet i første rekke tildosert med relativt større hastighet for å utligne det tilstedeværende overskudd av legering inntil det tilsammen var oppnådd et vektforhold mellom fosfor og legering på 1,1:1. Oppvarmingen ble bibeholdt inntil det i den nedre del av reaksjonskaret var oppnådd en temperatur på 500°C. Deretter ble det tildosert ytterligere fosfor og legering i vektforhold 1,1:1, inntil reaksjonskaret inne-holdt ca. 200 kg produkt. Fra nå av ble det gjennom uttaksåpningen kontinuerlig uttatt produkt med samme hastighet som fosfor og legering ble tilført. Tildoseringen ble avstemt således at temperaturen på 550°C ikke ble overskredet. Etter forbruk av den samlede legering ble tildoseringen av fosfor innstilt, oppvarmingen satt i drift og resten av produktet uttatt videre kontinuerlig. Tilsammen ble det dannet 520 kg sandformet produkt med et fosfidinnhold på 90% av det teore-tiske . In the reaction vessel mentioned in example 1, a mixture of 50 kg of a sand-shaped aluminium-magnesium alloy with a magnesium content of 5% and 0.2 kg of iodine was filled, in the storage vessel for metal there was a mixture of a further 200 kg of said alloy and 0.6 kg of iodine. Now the reaction vessel at the bottom was heated to 450°C. The addition of phosphorus and alloy was then started. Thereby, the phosphorus was primarily dosed at a relatively greater rate to compensate for the excess of alloy present until a total weight ratio between phosphorus and alloy of 1.1:1 had been achieved. The heating was maintained until a temperature of 500°C had been reached in the lower part of the reaction vessel. Further phosphorus and alloy were then dosed in a weight ratio of 1.1:1, until the reaction vessel contained approx. 200 kg of product. From now on, product was continuously withdrawn through the withdrawal opening at the same rate as phosphorus and alloy were added. The dosage was adjusted so that the temperature of 550°C was not exceeded. After consumption of the total alloy, the addition of phosphorus was adjusted, the heating was put into operation and the rest of the product was withdrawn continuously. Altogether, 520 kg of sand-shaped product was formed with a phosphide content of 90% of the theoretical.
Eksemp_el_4 Example_el_4
I det i eksempel 1 omtalte reaksjonskar ble det fylt 130 kg aluminiumf osf id fra en tidligere produksjon, i f orrådskar _; ; for metall befant det seg en blanding av 250 kg aluminium og 1 kg jod. Nå ble reaksjonskaret ved bunnen oppvarmet til 480°C og det ble innført 20 kg aluminium. Deretter ble aluminium og fosfor tildosert samtidig, og etter oppnåelse av en temperatur på 500°C ble oppvarmingen stoppet. Det tilstedeværende overskudd av metall ble utlignet ved en i første rekke noe hurtigere tildosering av fosfor, deretter foregikk tildosering av aluminium og fosfor med et konstant vektforhold på 1:1,1 med slik hastighet at temperaturen på 570°C ikke ble overskredet. Etter at det i reaksjonskaret befant seg tilsammen 230 kg produkt ble det ved samtidig dosering av aluminium og fosfor uttatt 130 kg produkt. In the reaction vessel mentioned in example 1, 130 kg of aluminum phosphate from a previous production was filled, in a storage vessel _; ; for metal there was a mixture of 250 kg of aluminum and 1 kg of iodine. Now the reaction vessel at the bottom was heated to 480°C and 20 kg of aluminum was introduced. Aluminum and phosphorus were then dosed at the same time, and after reaching a temperature of 500°C the heating was stopped. The excess metal present was offset by a somewhat faster addition of phosphorus in the first instance, then the addition of aluminum and phosphorus took place with a constant weight ratio of 1:1.1 at such a rate that the temperature of 570°C was not exceeded. After there was a total of 230 kg of product in the reaction vessel, 130 kg of product was withdrawn by simultaneous dosing of aluminum and phosphorus.
Denne prosess ble gjentatt inntil 250 kg aluminium var forbrukt. Tilsammen ble det uttatt 501 kg produkt med et aluminiumfosfidinnhold på 95%, ytterligere rundt 155 kg produkt ble tilbake som start for neste produksjon i reaksjonskaret. This process was repeated until 250 kg of aluminum had been consumed. Altogether, 501 kg of product with an aluminum phosphide content of 95% was taken out, a further around 155 kg of product was left as a start for the next production in the reaction vessel.
Claims (3)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19813117393 DE3117393A1 (en) | 1981-05-02 | 1981-05-02 | METHOD FOR PRODUCING THE PHOSPHIDES OF ALUMINUM OR MAGNESIUM |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| NO821427L NO821427L (en) | 1982-11-03 |
| NO156084B true NO156084B (en) | 1987-04-13 |
| NO156084C NO156084C (en) | 1987-07-22 |
Family
ID=6131294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO821427A NO156084C (en) | 1981-05-02 | 1982-04-30 | PROCEDURE FOR THE PREPARATION OF ALUMINUM PHOSPHIDE AND / OR MAGNESIUM PHOSPHIDE OR A MIXTURE PHOSPHIDE OF ALUMINUM AND MAGNESIUM. |
Country Status (16)
| Country | Link |
|---|---|
| JP (1) | JPS582210A (en) |
| AT (1) | AT394843B (en) |
| AU (1) | AU549936B2 (en) |
| BR (1) | BR8202525A (en) |
| CA (1) | CA1182273A (en) |
| DE (1) | DE3117393A1 (en) |
| DK (1) | DK157911C (en) |
| ES (1) | ES8304518A2 (en) |
| FI (1) | FI821507L (en) |
| FR (1) | FR2504908A2 (en) |
| GB (1) | GB2097775A (en) |
| IT (1) | IT1156465B (en) |
| MX (1) | MX157403A (en) |
| NO (1) | NO156084C (en) |
| SE (1) | SE452147B (en) |
| ZA (1) | ZA822828B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9511495D0 (en) * | 1995-06-07 | 1995-08-02 | Degesch De Chile Ltda | Composition, process and apparatus for producing phosphine - containing gas |
| CN1107447C (en) * | 1999-04-27 | 2003-05-07 | 华仁沈阳农药有限公司 | Process for synthesizing magnesium phosphide as fumigating insecticide of storehouse |
| FR2886060B1 (en) * | 2005-05-18 | 2007-07-27 | Centre Nat Rech Scient | PROCESS FOR PREPARING ANODE FOR ION-LITHIUM BATTERY |
| GB201221425D0 (en) * | 2012-11-28 | 2013-01-09 | Faradion Ltd | Metal-containing compound |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL57196C (en) * | 1940-03-13 | |||
| DE736700C (en) * | 1940-03-13 | 1943-06-28 | Schering Ag | Manufacture of products containing magnesium phosphide |
| US2984577A (en) * | 1957-10-24 | 1961-05-16 | Monsanto Chemicals | Process for the production of boron phosphide |
| FR1310236A (en) * | 1961-01-09 | 1963-03-06 | ||
| US3309176A (en) * | 1961-03-29 | 1967-03-14 | Rca Corp | Low temperature synthesis of compound semiconductors |
| GB1175511A (en) * | 1966-01-10 | 1969-12-23 | Albright & Wilson Mfg Ltd | Manufacture of Metal Phosphides |
| CH515852A (en) * | 1966-04-07 | 1971-11-30 | Freyberg Werner Dr | Magnesium phosphide mg3p2 fumigating agent for cereals |
| DE1567520B2 (en) * | 1966-04-07 | 1973-01-04 | Freyberg, Werner, Dr., 6149 Kirschhausen | Process for the production of magnesium phosphide |
| DE2945647C2 (en) * | 1979-11-12 | 1990-01-04 | Degesch Gmbh, 6000 Frankfurt | Process for the production of aluminum phosphide and / or magnesium phosphide |
-
1981
- 1981-05-02 DE DE19813117393 patent/DE3117393A1/en active Granted
-
1982
- 1982-04-20 CA CA000401279A patent/CA1182273A/en not_active Expired
- 1982-04-22 FR FR8206960A patent/FR2504908A2/en active Granted
- 1982-04-26 ZA ZA822828A patent/ZA822828B/en unknown
- 1982-04-26 GB GB8212058A patent/GB2097775A/en not_active Withdrawn
- 1982-04-29 FI FI821507A patent/FI821507L/en not_active Application Discontinuation
- 1982-04-29 IT IT67565/82A patent/IT1156465B/en active
- 1982-04-29 MX MX192492A patent/MX157403A/en unknown
- 1982-04-30 NO NO821427A patent/NO156084C/en unknown
- 1982-04-30 ES ES511837A patent/ES8304518A2/en not_active Expired
- 1982-04-30 SE SE8202737A patent/SE452147B/en not_active IP Right Cessation
- 1982-04-30 AU AU83160/82A patent/AU549936B2/en not_active Expired
- 1982-04-30 BR BR8202525A patent/BR8202525A/en unknown
- 1982-04-30 AT AT0169382A patent/AT394843B/en not_active IP Right Cessation
- 1982-04-30 DK DK196182A patent/DK157911C/en not_active IP Right Cessation
- 1982-05-01 JP JP57074437A patent/JPS582210A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| FR2504908A2 (en) | 1982-11-05 |
| MX157403A (en) | 1988-11-22 |
| BR8202525A (en) | 1983-04-19 |
| DE3117393C2 (en) | 1990-06-28 |
| FI821507L (en) | 1982-11-03 |
| CA1182273A (en) | 1985-02-12 |
| NO821427L (en) | 1982-11-03 |
| NO156084C (en) | 1987-07-22 |
| GB2097775A (en) | 1982-11-10 |
| AU549936B2 (en) | 1986-02-20 |
| ES511837A0 (en) | 1983-03-01 |
| SE8202737L (en) | 1982-11-03 |
| ATA169382A (en) | 1991-12-15 |
| ES8304518A2 (en) | 1983-03-01 |
| AT394843B (en) | 1992-06-25 |
| JPS582210A (en) | 1983-01-07 |
| DK157911B (en) | 1990-03-05 |
| AU8316082A (en) | 1982-11-11 |
| FI821507A0 (en) | 1982-04-29 |
| IT1156465B (en) | 1987-02-04 |
| DK196182A (en) | 1982-11-03 |
| SE452147B (en) | 1987-11-16 |
| ZA822828B (en) | 1983-02-23 |
| DK157911C (en) | 1990-08-27 |
| DE3117393A1 (en) | 1982-11-11 |
| IT8267565A0 (en) | 1982-04-29 |
| FR2504908B2 (en) | 1984-10-19 |
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