CA1182273A - Method for the production of aluminium or magnesium phosphide - Google Patents
Method for the production of aluminium or magnesium phosphideInfo
- Publication number
- CA1182273A CA1182273A CA000401279A CA401279A CA1182273A CA 1182273 A CA1182273 A CA 1182273A CA 000401279 A CA000401279 A CA 000401279A CA 401279 A CA401279 A CA 401279A CA 1182273 A CA1182273 A CA 1182273A
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- CA
- Canada
- Prior art keywords
- reaction vessel
- phosphorus
- metal
- reaction
- finely divided
- 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
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Catalysts (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
- Powder Metallurgy (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
ABSTRACT
The invention is directed to a process of im-proving the production of phosphide of aluminum or mag-nesium in which the finely divided metal or an alloy of the two metals is reacted with yellow phosphorus at a temper-ature between 300 and 600°C in an inert gas atmosphere and in the presence of a catalytically effective amount of the element chlorine, bromine, or iodine or a compound of such element with phosphorus, sulfur, hydrogen, ammonium, zinc, or the metal being reacted. The improvement consists in slowly feeding both the yellow phosphorus in liquid form and the finely divided metal into the reaction vessel.
The invention is directed to a process of im-proving the production of phosphide of aluminum or mag-nesium in which the finely divided metal or an alloy of the two metals is reacted with yellow phosphorus at a temper-ature between 300 and 600°C in an inert gas atmosphere and in the presence of a catalytically effective amount of the element chlorine, bromine, or iodine or a compound of such element with phosphorus, sulfur, hydrogen, ammonium, zinc, or the metal being reacted. The improvement consists in slowly feeding both the yellow phosphorus in liquid form and the finely divided metal into the reaction vessel.
Description
PROCESS FOR PREPARING ALUMINUM
OR MAGNESIUM PHOSPHIDE
This invention relates ~o an improvement in the production of the phosphide of aluminum or magnesium in which the finely divided metal or an alloy of the two metals is reacted with yellow phosphorus at a temperature between 300 and 600C in an inert gas atmospherence and in the presence of chlorine, bromine, iodine, or a compound of such elements with phosphorus, sulfur, hydroger" ammo-nium, zinc, or the metal being reacted.
According to a particularly preferred form, first the finely divided or gritty metal is intimately mixed .15 with the catalyst. The mixture is heated in a suitable reactor capable of being enclosed in an inert gas atomos-phere, for example, under nitrogen at normal pressure to the reaction between 300 and 600C. When the desired reac-tion temperature is reached liquid yellow phosphorus is added at such a speed that the heat of reaction liberated is led off without problem and the temperature can be main-tained in the range between 300 and 600C.
.~
It has now be found that this process can be made still safer and be more readily controlled and above all be made par-tially or even fully continuous if the finely divi-ded metal is also slowly added into the reaction vessel.
According to the present invention there is provi-ded a process for preparing aluminium or magnesium phosphide by reacting the finely divided metal or an alloy of the two metals and liquid yellow phosphorus at a termpera-ture bet-ween 300 and 600 C in an inert gas atmosphere and in the presence of a catalytically effective amount of -the element chlorine, bromine, or iodine or a compound of such element with phosphorus, sulfur, hydrogen, ammonium, zinc, or -the metal being reacted, the improvement comprising slowly add-]5 ing to the reaction vessel both the liqu~d phosphorus and the finely divided metal.
If the process of the invention is carried out in a substantially cylindrical reaction vessel, which is heated Erom below the bo-ttom then there are clearly formed four different zones which from the top to the bottom can be des-cribed as follows:
Zone 1: In this uppermost zone there exists only gas, namely a rnixture of -the inert gas employed and phos-phorus vapor. Since in this zone in the most extreme case -there is only reached a maximum tempera-ture of about 200 C, the vapor pressure of -the phosphorus is rela-tively small so that the gas mixture consists chiefly of the inert gas em-ployed.
Zone 2: Here is the vaporization zone of the yellow phosphorus. In this zone there prevail temperature which are slightly above the boiling point of the yellow phosphorus.
Also in zone there exists only gas, which now indeed consis-ts for the greatest part of phosphorus vapor.
OR MAGNESIUM PHOSPHIDE
This invention relates ~o an improvement in the production of the phosphide of aluminum or magnesium in which the finely divided metal or an alloy of the two metals is reacted with yellow phosphorus at a temperature between 300 and 600C in an inert gas atmospherence and in the presence of chlorine, bromine, iodine, or a compound of such elements with phosphorus, sulfur, hydroger" ammo-nium, zinc, or the metal being reacted.
According to a particularly preferred form, first the finely divided or gritty metal is intimately mixed .15 with the catalyst. The mixture is heated in a suitable reactor capable of being enclosed in an inert gas atomos-phere, for example, under nitrogen at normal pressure to the reaction between 300 and 600C. When the desired reac-tion temperature is reached liquid yellow phosphorus is added at such a speed that the heat of reaction liberated is led off without problem and the temperature can be main-tained in the range between 300 and 600C.
.~
It has now be found that this process can be made still safer and be more readily controlled and above all be made par-tially or even fully continuous if the finely divi-ded metal is also slowly added into the reaction vessel.
According to the present invention there is provi-ded a process for preparing aluminium or magnesium phosphide by reacting the finely divided metal or an alloy of the two metals and liquid yellow phosphorus at a termpera-ture bet-ween 300 and 600 C in an inert gas atmosphere and in the presence of a catalytically effective amount of -the element chlorine, bromine, or iodine or a compound of such element with phosphorus, sulfur, hydrogen, ammonium, zinc, or -the metal being reacted, the improvement comprising slowly add-]5 ing to the reaction vessel both the liqu~d phosphorus and the finely divided metal.
If the process of the invention is carried out in a substantially cylindrical reaction vessel, which is heated Erom below the bo-ttom then there are clearly formed four different zones which from the top to the bottom can be des-cribed as follows:
Zone 1: In this uppermost zone there exists only gas, namely a rnixture of -the inert gas employed and phos-phorus vapor. Since in this zone in the most extreme case -there is only reached a maximum tempera-ture of about 200 C, the vapor pressure of -the phosphorus is rela-tively small so that the gas mixture consists chiefly of the inert gas em-ployed.
Zone 2: Here is the vaporization zone of the yellow phosphorus. In this zone there prevail temperature which are slightly above the boiling point of the yellow phosphorus.
Also in zone there exists only gas, which now indeed consis-ts for the greatest part of phosphorus vapor.
2 -4 6~~f31P~li Zone 3: Here lS located in the uppermost layer of the container filling the true - 2a -reaction zone ln whlch phospnorus vapor comes in contact with tne flnel~ dividea metal and the alreac~ formec ~nos?hiàe. In this zone whicn lS
at the reactio. tem?erature of 300 to 600C tnere akes ?12ce the s rongl\~ e~othermic reaction between the phosphor~s vz?cr and the flnely diviaea metal.
Since .ne pnos_hor~as vapor reacts very quickly with the metal 1 does nct ~enetr2te very deeply into the contalner fi_ilns but onlv about 10 to 15 c~.
There_ore witlln _he container filling the gas phase in tne cirec.lo- rom the top cownwardlv very raplcly has a o;ered phospnorus vapor content.
Zor.e ~.: In this lowermost zone tne cas ?hase consis C practlcally only of inert ~as because the phcs?ncruc vapor does not penetrate to thls de?th. The solid material consists practicall-only of the phosphide formec and contains perhaps small amounts of unreacted metal. A sliaht excess of metal makes certain that the ?hos?hide formed is free OI phosphorus.
The forma~ion of tne previously aescribed four zones within the reaction vessel then makes possible a particula~ly simple and completely safe form o~ the process of the invention. Thereby the liquic yellow phosphorus is continuously addec into the up?er part o the reaction vessel thus in the gas space abo~e the container packing where lt can be va?orized ~ilhout hindr2nce. It is especiallv advantageous if the entrance for the liquid pnos-phorus is locatec entirely above in the reaction vessel thus ln aDove-mentioned zone 1. The finely divided metal to be sure can also be added in the upper part of the reaction vessel. Then however the quick anc vigorous reaction ~ith the phosphorus vapor already present makes .. ~
necessary the use of special closing off devices for the entrance in order to prevent the phosphorus VG,-Or frcm penetrating into the conveying device for the flnelv divided metal. Therefore it is more advan,ageous to continuously add the finely divided metal into the lower par, of the reaction vessel, namely so that the entrance is in the region of the container filling. This can occur in the above-mentioned zone 3, the true reaction zone. Then it is suitable to provide about the height of the entrance for the metal a stirrer whose conveying elements move the container packing along the periphery of the container and thus provide for a uniform distribution of the freshly added metal in the reaction zone. However, it is still more advantageous if the addition of the finely divided metal takes place in the lowest part of the reaction vessel, thus in the above-mentioned zone g. In this case it is suitable to provide a stirrer whose conveying elements move the container packing along the periphery of the container and simul-taneously provide for a thorough mixing vertically.
It is possible in the manner depicted to continuously add equivalent amounts of finely divided metal, which contains the catalyst mixed therein, and liquid yellow phosphorus into the reaction vessel and during the reaction to withdraw from the lowest part of the reaction vessel, thus from the above-mentioned zone 4, the phosphide formed, which is free from unreacted phosphorus.
The withdrawal takes place through an~opening at the bottom of the reaction vessel. ~t can be carried out at will continuously or batchwise. In continuous withdrawal the product is discharged in an amount corresponding exactly to the rnetal and phosphorus added. However, it is possible just as well also to let it slowly build up in the lowermost zone in the reaction vessel, thus the above-mer,tioned zone 4, and then to discharge the phos-phice formed batchwise. However, thereby attention mus, be paid that actually there is only discharged from this zone 4 material which no longer contains unreacted phosphorus, and not perhaps also material from the reaction zone, which can happen through weisht control.
If the finely divided metal - as described above - is fed into the lower part of the reaction vessel, thus in the above-mentioned zone 3 or zone 4, then there suffices as feeding device a customary screw convever, because the solid, gritty contai.ner filling serves at the same time as closing off device. Should the process of the invention be started in an empty reaction vessel, it .is therefore suitable first to introduce onlv f inely divided metal until the entrance for the metal is covered, and only then to beg.in the slow addition of the liquid phosphorus. However it is still more advantageous if the reaction vessel first is filled with the corresponding phos-phide from an earlier production until it is above the entrance for the metal, and then simultaneously there is begun the addition of the liquid phosphorus and the finelv divided metal.
The process of ,he invention is explained in more detail in the following examples. Unless olherwise stated all percents are weight percents.
Example 1 As reaction vessel there served a cylindrical container having a diameter of about 80 crn and a height of about 100 cm which was provided with a stirrer, a coolins system, temperature probes at various heights, an inlet line for inert gas and a line for waste gas. The bottom of the container was heatable by a gas burner from the outside to temperatures U? to 500C. Connected thereto was a supply vessel for liquid phosphorus having a pump which permitted at will the rotation of the liquid yellow phosphorus in the supply vessel or to feed it into the reaction vessel, as well as a supply vessel for the finely divided metal to be reacted with a conveying device for the adding of the metal into the reaction vessel. At the bottcr~
of the reaction vessel there was located a small opening provided with a locking off device for dis-charge of product. For reasons of safety the reaction vessel was provided with a rupture disc to counter an~ possible increase in pressure. The reaction vessel was rinsed before and after the reaction with nitrogen, during the reaction the reaction mixture was covered with argon. The waste gas was led off over a water receiver having a glass fiber filter and a post-connected activated,carbon filter.
Before the beginning of the reaction there were located in the reaction vessel 50 kg of magnesium phosphide from an earlier production, in the supply vessel for the metal a mixture of 200 kg of magnesium and 0.8 kg of iodine, in the supply vessel for ~he liquid phosphorus this was rotated.
Then the reaction vessel W2S heated at the bottom to 300C. Then there were fed into the reaction vessel 10 kg of magnesium and the feeding in of the liquid phosphorus was begun with a speed of 0.4 to 1 kg per minute. Simultaneously more magnesium was also added. Through the heat of reaction the temperature increased in the lower part of thte xeaction vessel to 550C. Then the addition of the phosphorus and the magnesium was so regulated that the temperature was maintained at 550C and the weight ratio between phosphorus and magnesium was around 0.85:1. After about 180 kg of magnesium phosphide had formed in the reaction vessel there were discharged through the withdrawal opeing 100 kg of product within 10 minutes while continuously adding further phosphorus and magnesium. The with-drawal opening was again closed. After there had again formed about 180 kg o~ magnesium phosphide.
this was a'gain discharged and subsequently the entire process was again re2eated. After using up the supply of 200 kg of magnesium the addition of phosphorus was stopped. The product still located in teh reaction vessel was again heated briefly and discharged. Including the magnesium phosphide present in the reaction vessel in the course of 5 hours there were discharged 415 kg of product having a magnesium phosphide content of 92~.
Example 2 There were present in the reaction ~essel described in Example 1 a mixture of 100 kg of --&--magnesium and 0.3 kg of iodine in the supply vessel for the metal there was present a mixture of a further 150 kg of magnesium and 0.5 ky of iodine.
Then the reaction vessel was heated at the bottom of 300 C. Then phosphorus was added at such a speed that the temperature in the lower part of the reaction vessel slowly increased to 550C. Through control of the addition of phosphorus this tempera-ture was maintained until altogether 82 kg of phosphorus was used. Then there were simultaneously added magnesium and phosphorus in the weight ratio 1:0.83 at such 2 velocity that the temperature in the lower part of tne reaction vessel continuously remained between 500 and 550C. At the same time there was continuously discharged through the withdrawal opening product in such amount that it exactly corresponded to the amount of magnesium and phosphorus added thus altogether 150 kg of magnesium and 123 kg of phosphorus. Finally the product still found in the reaction vessel was heated again briefly and further discharged continuously. The yield in all amounted to 450 kg with an average content of magnesium phosphide of 90~.
Example 3 There were present in the reaction vessel described in Example 1 a mixture of 50 kg of a gritty aluminum-magnesium alloy having a magnesi~un content of 5~ and 0.2 kg of iodine. There was present in the suppl~ vessel for the metal a mixture of a further 200 kg of the alloy mentioned and 0.6 kg of iodine. Then the reaction vessel was heated at the bo-ttom to 450C. Then there was begun the addition of phosphorus and alloy. Thereby the phosphorus was first added with relatively greater ~ Z7~7 speed in order to compensate for the excess of alloy present, until ln all there was reached a weight ratlo of phosphorus to alloy o~ 1. The heat~ng remined on until a temperature of 500C was reached in the lower part of the reaction vessel. Subse-~uently there were added more phosphorus and alloy in the wieght ratio of 1.1:1 until the reaction vessel contained about 200 kg of product. From this point on tnere was continuously discharged through the withdrawal opening product at the same velocity that phosphorus and alloy were added. The addition was so adjusted that the temperature dic not exceed 550C. After use of the entire alloy the addition of the phosphorus was stopped, the heating set in operation and the remainder of the product continuously further discharged. In all there were obtained 520 kg of gritty product with a phosphide content of 90~ of theory.
Example 4 There were present in the reaction vessel described in ~xample 1 130 kg of aluminum phosphide from an earlier production, in the suppl~7 vessel for th~ metal there was a mixture of 250 kg of aluminum and 1 kg of iodine. Then the reaction vessel was heated at the bottom to 480C and there were introduced 20 kg of aluminum. Then there were simultalleously added aluminum and phosphorus and after reacting a temperature of 500C the heating stopped. The excess of metal present was compen-sated for by an at first somewhat quicker addition of phosphorus, then there took place the addition of aluminum and phosphorus with a constant weight ratio of 1:1.1 at such velocity that the temperature of i70 C was not exceeded. After there were found in the reaction vessel ln all 230 kg of product there was discharged 130 kg of product with constant addition of aluminum and phosphorus. This process was repeated until the 250 kg of aluminum were use~
up. In all there were discharged 501 kg of product with an aluminum phosphide content of 95~, around a fur.her lii kg was left in the reaction vessel as a heel for ~he next product.
at the reactio. tem?erature of 300 to 600C tnere akes ?12ce the s rongl\~ e~othermic reaction between the phosphor~s vz?cr and the flnely diviaea metal.
Since .ne pnos_hor~as vapor reacts very quickly with the metal 1 does nct ~enetr2te very deeply into the contalner fi_ilns but onlv about 10 to 15 c~.
There_ore witlln _he container filling the gas phase in tne cirec.lo- rom the top cownwardlv very raplcly has a o;ered phospnorus vapor content.
Zor.e ~.: In this lowermost zone tne cas ?hase consis C practlcally only of inert ~as because the phcs?ncruc vapor does not penetrate to thls de?th. The solid material consists practicall-only of the phosphide formec and contains perhaps small amounts of unreacted metal. A sliaht excess of metal makes certain that the ?hos?hide formed is free OI phosphorus.
The forma~ion of tne previously aescribed four zones within the reaction vessel then makes possible a particula~ly simple and completely safe form o~ the process of the invention. Thereby the liquic yellow phosphorus is continuously addec into the up?er part o the reaction vessel thus in the gas space abo~e the container packing where lt can be va?orized ~ilhout hindr2nce. It is especiallv advantageous if the entrance for the liquid pnos-phorus is locatec entirely above in the reaction vessel thus ln aDove-mentioned zone 1. The finely divided metal to be sure can also be added in the upper part of the reaction vessel. Then however the quick anc vigorous reaction ~ith the phosphorus vapor already present makes .. ~
necessary the use of special closing off devices for the entrance in order to prevent the phosphorus VG,-Or frcm penetrating into the conveying device for the flnelv divided metal. Therefore it is more advan,ageous to continuously add the finely divided metal into the lower par, of the reaction vessel, namely so that the entrance is in the region of the container filling. This can occur in the above-mentioned zone 3, the true reaction zone. Then it is suitable to provide about the height of the entrance for the metal a stirrer whose conveying elements move the container packing along the periphery of the container and thus provide for a uniform distribution of the freshly added metal in the reaction zone. However, it is still more advantageous if the addition of the finely divided metal takes place in the lowest part of the reaction vessel, thus in the above-mentioned zone g. In this case it is suitable to provide a stirrer whose conveying elements move the container packing along the periphery of the container and simul-taneously provide for a thorough mixing vertically.
It is possible in the manner depicted to continuously add equivalent amounts of finely divided metal, which contains the catalyst mixed therein, and liquid yellow phosphorus into the reaction vessel and during the reaction to withdraw from the lowest part of the reaction vessel, thus from the above-mentioned zone 4, the phosphide formed, which is free from unreacted phosphorus.
The withdrawal takes place through an~opening at the bottom of the reaction vessel. ~t can be carried out at will continuously or batchwise. In continuous withdrawal the product is discharged in an amount corresponding exactly to the rnetal and phosphorus added. However, it is possible just as well also to let it slowly build up in the lowermost zone in the reaction vessel, thus the above-mer,tioned zone 4, and then to discharge the phos-phice formed batchwise. However, thereby attention mus, be paid that actually there is only discharged from this zone 4 material which no longer contains unreacted phosphorus, and not perhaps also material from the reaction zone, which can happen through weisht control.
If the finely divided metal - as described above - is fed into the lower part of the reaction vessel, thus in the above-mentioned zone 3 or zone 4, then there suffices as feeding device a customary screw convever, because the solid, gritty contai.ner filling serves at the same time as closing off device. Should the process of the invention be started in an empty reaction vessel, it .is therefore suitable first to introduce onlv f inely divided metal until the entrance for the metal is covered, and only then to beg.in the slow addition of the liquid phosphorus. However it is still more advantageous if the reaction vessel first is filled with the corresponding phos-phide from an earlier production until it is above the entrance for the metal, and then simultaneously there is begun the addition of the liquid phosphorus and the finelv divided metal.
The process of ,he invention is explained in more detail in the following examples. Unless olherwise stated all percents are weight percents.
Example 1 As reaction vessel there served a cylindrical container having a diameter of about 80 crn and a height of about 100 cm which was provided with a stirrer, a coolins system, temperature probes at various heights, an inlet line for inert gas and a line for waste gas. The bottom of the container was heatable by a gas burner from the outside to temperatures U? to 500C. Connected thereto was a supply vessel for liquid phosphorus having a pump which permitted at will the rotation of the liquid yellow phosphorus in the supply vessel or to feed it into the reaction vessel, as well as a supply vessel for the finely divided metal to be reacted with a conveying device for the adding of the metal into the reaction vessel. At the bottcr~
of the reaction vessel there was located a small opening provided with a locking off device for dis-charge of product. For reasons of safety the reaction vessel was provided with a rupture disc to counter an~ possible increase in pressure. The reaction vessel was rinsed before and after the reaction with nitrogen, during the reaction the reaction mixture was covered with argon. The waste gas was led off over a water receiver having a glass fiber filter and a post-connected activated,carbon filter.
Before the beginning of the reaction there were located in the reaction vessel 50 kg of magnesium phosphide from an earlier production, in the supply vessel for the metal a mixture of 200 kg of magnesium and 0.8 kg of iodine, in the supply vessel for ~he liquid phosphorus this was rotated.
Then the reaction vessel W2S heated at the bottom to 300C. Then there were fed into the reaction vessel 10 kg of magnesium and the feeding in of the liquid phosphorus was begun with a speed of 0.4 to 1 kg per minute. Simultaneously more magnesium was also added. Through the heat of reaction the temperature increased in the lower part of thte xeaction vessel to 550C. Then the addition of the phosphorus and the magnesium was so regulated that the temperature was maintained at 550C and the weight ratio between phosphorus and magnesium was around 0.85:1. After about 180 kg of magnesium phosphide had formed in the reaction vessel there were discharged through the withdrawal opeing 100 kg of product within 10 minutes while continuously adding further phosphorus and magnesium. The with-drawal opening was again closed. After there had again formed about 180 kg o~ magnesium phosphide.
this was a'gain discharged and subsequently the entire process was again re2eated. After using up the supply of 200 kg of magnesium the addition of phosphorus was stopped. The product still located in teh reaction vessel was again heated briefly and discharged. Including the magnesium phosphide present in the reaction vessel in the course of 5 hours there were discharged 415 kg of product having a magnesium phosphide content of 92~.
Example 2 There were present in the reaction ~essel described in Example 1 a mixture of 100 kg of --&--magnesium and 0.3 kg of iodine in the supply vessel for the metal there was present a mixture of a further 150 kg of magnesium and 0.5 ky of iodine.
Then the reaction vessel was heated at the bottom of 300 C. Then phosphorus was added at such a speed that the temperature in the lower part of the reaction vessel slowly increased to 550C. Through control of the addition of phosphorus this tempera-ture was maintained until altogether 82 kg of phosphorus was used. Then there were simultaneously added magnesium and phosphorus in the weight ratio 1:0.83 at such 2 velocity that the temperature in the lower part of tne reaction vessel continuously remained between 500 and 550C. At the same time there was continuously discharged through the withdrawal opening product in such amount that it exactly corresponded to the amount of magnesium and phosphorus added thus altogether 150 kg of magnesium and 123 kg of phosphorus. Finally the product still found in the reaction vessel was heated again briefly and further discharged continuously. The yield in all amounted to 450 kg with an average content of magnesium phosphide of 90~.
Example 3 There were present in the reaction vessel described in Example 1 a mixture of 50 kg of a gritty aluminum-magnesium alloy having a magnesi~un content of 5~ and 0.2 kg of iodine. There was present in the suppl~ vessel for the metal a mixture of a further 200 kg of the alloy mentioned and 0.6 kg of iodine. Then the reaction vessel was heated at the bo-ttom to 450C. Then there was begun the addition of phosphorus and alloy. Thereby the phosphorus was first added with relatively greater ~ Z7~7 speed in order to compensate for the excess of alloy present, until ln all there was reached a weight ratlo of phosphorus to alloy o~ 1. The heat~ng remined on until a temperature of 500C was reached in the lower part of the reaction vessel. Subse-~uently there were added more phosphorus and alloy in the wieght ratio of 1.1:1 until the reaction vessel contained about 200 kg of product. From this point on tnere was continuously discharged through the withdrawal opening product at the same velocity that phosphorus and alloy were added. The addition was so adjusted that the temperature dic not exceed 550C. After use of the entire alloy the addition of the phosphorus was stopped, the heating set in operation and the remainder of the product continuously further discharged. In all there were obtained 520 kg of gritty product with a phosphide content of 90~ of theory.
Example 4 There were present in the reaction vessel described in ~xample 1 130 kg of aluminum phosphide from an earlier production, in the suppl~7 vessel for th~ metal there was a mixture of 250 kg of aluminum and 1 kg of iodine. Then the reaction vessel was heated at the bottom to 480C and there were introduced 20 kg of aluminum. Then there were simultalleously added aluminum and phosphorus and after reacting a temperature of 500C the heating stopped. The excess of metal present was compen-sated for by an at first somewhat quicker addition of phosphorus, then there took place the addition of aluminum and phosphorus with a constant weight ratio of 1:1.1 at such velocity that the temperature of i70 C was not exceeded. After there were found in the reaction vessel ln all 230 kg of product there was discharged 130 kg of product with constant addition of aluminum and phosphorus. This process was repeated until the 250 kg of aluminum were use~
up. In all there were discharged 501 kg of product with an aluminum phosphide content of 95~, around a fur.her lii kg was left in the reaction vessel as a heel for ~he next product.
Claims (3)
1. In a process for preparing aluminum or magnes-ium phosphide by reacting the finely divided metal or an alloy of the two metals and liquid yellow phosphorus at a temperature between 300 and 600°C in an inert gas atmosphere and in the presence of a catalytically effective amount of the element chlorine, bromine, or iodine or a compound of such element with phosphorus, sulfur, hydrogen, ammonium, zinc, or the metal being reacted the improvement comprising slowly adding to the reaction vessel both the liquid phos-phorus and the finely divided metal.
2. A process according to claim 1 wherein the reaction vessel contains solid reaction mixture or reaction product and the liquid yellow phosphorus is fed into the upper part of the reaction vessel above the solids.
3. A process according to claim 1 or 2 wherein the finely divided metal is fed into the lower part of the reaction vessel so that it enters where the reaction vessel contains reaction mixture or reaction product.
Applications Claiming Priority (2)
| 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 |
| DEP3117393.4 | 1981-05-02 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1182273A true CA1182273A (en) | 1985-02-12 |
Family
ID=6131294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000401279A Expired CA1182273A (en) | 1981-05-02 | 1982-04-20 | Method for the production of aluminium or magnesium phosphide |
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) |
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| 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 |
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|---|---|---|---|---|
| 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 IT IT67565/82A patent/IT1156465B/en active
- 1982-04-29 FI FI821507A patent/FI821507L/en not_active Application Discontinuation
- 1982-04-29 MX MX192492A patent/MX157403A/en unknown
- 1982-04-30 DK DK196182A patent/DK157911C/en not_active IP Right Cessation
- 1982-04-30 AU AU83160/82A patent/AU549936B2/en not_active Expired
- 1982-04-30 ES ES511837A patent/ES8304518A2/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 NO NO821427A patent/NO156084C/en unknown
- 1982-04-30 SE SE8202737A patent/SE452147B/en not_active IP Right Cessation
- 1982-05-01 JP JP57074437A patent/JPS582210A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| ES511837A0 (en) | 1983-03-01 |
| SE8202737L (en) | 1982-11-03 |
| MX157403A (en) | 1988-11-22 |
| NO156084B (en) | 1987-04-13 |
| AU549936B2 (en) | 1986-02-20 |
| NO821427L (en) | 1982-11-03 |
| NO156084C (en) | 1987-07-22 |
| GB2097775A (en) | 1982-11-10 |
| DK157911B (en) | 1990-03-05 |
| DE3117393A1 (en) | 1982-11-11 |
| AT394843B (en) | 1992-06-25 |
| DK157911C (en) | 1990-08-27 |
| FR2504908A2 (en) | 1982-11-05 |
| DK196182A (en) | 1982-11-03 |
| IT8267565A0 (en) | 1982-04-29 |
| AU8316082A (en) | 1982-11-11 |
| ZA822828B (en) | 1983-02-23 |
| IT1156465B (en) | 1987-02-04 |
| SE452147B (en) | 1987-11-16 |
| FI821507L (en) | 1982-11-03 |
| JPS582210A (en) | 1983-01-07 |
| DE3117393C2 (en) | 1990-06-28 |
| FR2504908B2 (en) | 1984-10-19 |
| BR8202525A (en) | 1983-04-19 |
| ES8304518A2 (en) | 1983-03-01 |
| ATA169382A (en) | 1991-12-15 |
| FI821507A0 (en) | 1982-04-29 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MKEC | Expiry (correction) | ||
| MKEX | Expiry |