DE2317282C3 - Process for the preparation of polymeric phosphorus nitride oxides - Google Patents
Process for the preparation of polymeric phosphorus nitride oxidesInfo
- Publication number
- DE2317282C3 DE2317282C3 DE19732317282 DE2317282A DE2317282C3 DE 2317282 C3 DE2317282 C3 DE 2317282C3 DE 19732317282 DE19732317282 DE 19732317282 DE 2317282 A DE2317282 A DE 2317282A DE 2317282 C3 DE2317282 C3 DE 2317282C3
- Authority
- DE
- Germany
- Prior art keywords
- melamine
- urea
- phosphorus nitride
- preparation
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- -1 phosphorus nitride Chemical class 0.000 title claims description 11
- 229910052698 phosphorus Inorganic materials 0.000 title claims description 10
- 239000011574 phosphorus Substances 0.000 title claims description 10
- 238000000034 method Methods 0.000 title claims description 9
- 238000002360 preparation method Methods 0.000 title claims 2
- 229920000877 Melamine resin Polymers 0.000 claims description 14
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 8
- DZHMRSPXDUUJER-UHFFFAOYSA-N [amino(hydroxy)methylidene]azanium;dihydrogen phosphate Chemical compound NC(N)=O.OP(O)(O)=O DZHMRSPXDUUJER-UHFFFAOYSA-N 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 229940005657 pyrophosphoric acid Drugs 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 description 8
- 235000011007 phosphoric acid Nutrition 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 229920000388 Polyphosphate Polymers 0.000 description 3
- 150000001408 amides Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000001205 polyphosphate Substances 0.000 description 3
- 235000011176 polyphosphates Nutrition 0.000 description 3
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 239000004114 Ammonium polyphosphate Substances 0.000 description 1
- 239000005696 Diammonium phosphate Substances 0.000 description 1
- SQSPRWMERUQXNE-UHFFFAOYSA-N Guanylurea Chemical compound NC(=N)NC(N)=O SQSPRWMERUQXNE-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 1
- 229920001276 ammonium polyphosphate Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001912 cyanamides Chemical class 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 235000019837 monoammonium phosphate Nutrition 0.000 description 1
- 239000006012 monoammonium phosphate Substances 0.000 description 1
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- IVIIAEVMQHEPAY-UHFFFAOYSA-N tridodecyl phosphite Chemical compound CCCCCCCCCCCCOP(OCCCCCCCCCCCC)OCCCCCCCCCCCC IVIIAEVMQHEPAY-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/092—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more metal atoms
- C01B21/0923—Metal imides or amides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
Gegenstand der vorliegenden Erfindung ist ein Verfahren zur Herstellung polymerer Phosphornitridoxide (PNO)n mit niedrigem Schüttgewicht durch Erhitzen einer Mischung aus konzentrierter Phosphorsäure, Pyrophosphorsäure, Phosphorpentoxid, Monoammoniumdihydrogenmonophosphat oder Harnstoffphosphat und Harnstoff.The present invention relates to a process for producing polymeric phosphorus nitride oxides (PNO) n with a low bulk density by heating a mixture of concentrated phosphoric acid, pyrophosphoric acid, phosphorus pentoxide, monoammonium dihydrogen monophosphate or urea phosphate and urea.
Wie aus Gmelins Handbuch der anorganischen Chemie, 8. Auflage, Band 16, P, Teil C, S. 329 bis 331 ersichtlich ist, gehen die bisher beschriebenen Verfahren zur Herstellung von Phosphornitridoxid im allgemeinen von Phosphamid PO(NHXNH2) oder Phosphoramidochloriden PO(NH2)Cl2 und PO(N H2J2Cl aus, die man durch Reaktion von Phosphoroxidchlorid und Ammoniak gewinnt. Es können zwar grundsätzlich die nicht aufgetrennten Reaktionsprodukte von POCI3 und Ammoniak thermisch in Phosphornitridoxid umgewandelt werden, doch sind in diesem Falle die Ausbeuten geringer.As can be seen from Gmelin's Handbook of Inorganic Chemistry, 8th Edition, Volume 16, P, Part C, pp. 329 to 331, the processes described so far for the production of phosphorus nitride oxide are generally based on phosphamide PO (NHXNH 2 ) or phosphoramidochlorides PO ( NH 2 ) Cl 2 and PO (NH 2 J 2 Cl, which are obtained by the reaction of phosphorus oxychloride and ammonia. In principle, the unseparated reaction products of POCI3 and ammonia can be thermally converted into phosphorus nitride oxide, but in this case the yields are less.
Ebenso umständlich ist die Herstellung von Phosphornitridoxid durch thermische Zersetzung von PNO2H2, die neben wenig PNO viel P2O5 und NH3 liefert.The production of phosphorus nitride oxide by thermal decomposition of PNO 2 H 2 , which, in addition to a little PNO, supplies a lot of P 2 O 5 and NH 3, is just as laborious.
In der älteren Anmeldung, deutsche Offenlegungsschrift 23 51 886, werden Amidpolyphosphate beschrieben, die durch Erhitzen von Ammoniumorthophosphat, Harnstoffphosphat, Melaminphosphat, Phosphorpentoxid, Polyphosphorsäure oder Orthophosphorsäure oder eines Gemisches aus mindestens zwei dieser Verbindungen mit Melamin, Dicyandiamid, Guanidin oder Guanylharnstoff oder einem Gemisch aus mindestens zwei dieser Verbindungen in Gegenwart von Harnstoff als Kondensationsmittel in einem Molverhältnis von Harnstoff : Phosphorsäure (als H3PO4) : Cyanamid-Derivat von 0,8 bis 1,5 : 1 :0,05 bis 1 auf Temperaturen von 150 bis 350°C erhalten werden. Die Amidpolyphosphate unterscheiden sich von den Phosphornitridoxiden dadurch, daß sie ionogen sind und Wasserstoff enthalten. Sie stellen Abkömmlinge der Polyphosphate dar, bei denen OH-Gruppen durch Amid-Reste ersetzt sind.In the earlier application, German Offenlegungsschrift 23 51 886, amide polyphosphates are described, which by heating ammonium orthophosphate, urea phosphate, melamine phosphate, phosphorus pentoxide, polyphosphoric acid or orthophosphoric acid or a mixture of at least two of these compounds with melamine, dicyandiamide, guanidine or guanylurea or a mixture of at least two of these compounds in the presence of urea as a condensing agent in a molar ratio of urea: phosphoric acid (as H 3 PO 4 ): cyanamide derivative of 0.8 to 1.5: 1: 0.05 to 1 at temperatures of 150 to 350 ° C can be obtained. The amide polyphosphates differ from the phosphorus nitride oxides in that they are ionic and contain hydrogen. They are descendants of polyphosphates in which OH groups have been replaced by amide residues.
Überraschenderweise wurde nun gefunden, daß man auf einfachem Wege und in guter Ausbeute Produkte
mit niedrigem Schüttgewicht erhält, wenn man die in einem Moiverhältnis von 1:3 bis 1:6 gemischten
Ausgangsstoffe in einer ersten Stufe auf 400°C bis zum Nachlassen der Gasentwicklung und in einer zweiten
Stufe auf 600 bis 800° C im trockenen Luft- bzw. Sauerstoffstrom erhitzt.
Die Reaktion wird ganz allgemein in der Weise durchgeführt, daß man konzentrierte Phosphorsäure,
Pyrophosphorsäure, P2O5 oder Ammoniumphosphat
bzw. Harnstoffphosphat mit Harnstoff unter Feuchtigkeitsausschluß in Gefäßen aus V2A- oder V4A-Stahl in
den angegebenen Molverhältnissen allmählich aufSurprisingly, it has now been found that products with a low bulk density are obtained in a simple way and in good yield if the starting materials, mixed in a molar ratio of 1: 3 to 1: 6, are in a first stage at 400 ° C. until the evolution of gas subsides and heated in a second stage to 600 to 800 ° C in a stream of dry air or oxygen.
The reaction is generally carried out in such a way that concentrated phosphoric acid, pyrophosphoric acid, P 2 O 5 or ammonium phosphate or urea phosphate with urea with exclusion of moisture in vessels made of V2A or V4A steel in the specified molar ratios gradually
ίο 400°C erhitzt. Wenn nach ungefähr 1 Stunde die Gasentwicklung nachläßt, wird die Reaktionsmischung in einem trockenen Luft- oder Sauerstoffstrom auf 600 bis 800° C gebracht und bei diesen Temperaturen 1 Stunde gehalten. Hierbei fällt das Phosphornitridoxid inίο heated to 400 ° C. If after about 1 hour the If the evolution of gas subsides, the reaction mixture is brought to 600 in a stream of dry air or oxygen Brought to 800 ° C and held at these temperatures for 1 hour. Here, the phosphorus nitride oxide falls into
t5 fast quantitativer Ausbeute an. Eine Phosphin-Entwicklung, wie bei den obenerwähnten Verfahren, wird nicht beobachtett5 almost quantitative yield. A phosphine development as in the above-mentioned methods, is not observed
Die sich bei der Umsetzung abspielende Reaktion kann man in einfacher Weise formelmäßig etwa so darstellen:The reaction that takes place during the implementation can be described in a simple manner using a formula like this represent:
H3PO4 + 3 OQNH2J2-PNO + 5NH3 + 3 CO2 H3PO4 + 3 OQNH 2 J 2 -PNO + 5NH3 + 3 CO 2
Weiterhin wurde gefunden, daß man zu einem äußerst voluminösen Produkt gelangen kann, wenn man der Grundmischung wechselnde Mengen Melamin zusetzt und in der angegebenen Weise erhitzt. Man erhält auf diesem Wege einen anorganischen nicht brennbaren Schaumstoff. Die anzuwendende Melamin-Menge liegt zwischen 1 und 20%, bezogen auf die Gesamtmischung in Abhängigkeit vom gewünschten Schüttgewicht des herzustellenden Phosphornitridoxids. Vorzugsweise werden 2 bis 10% Melamin der Ausgangsmischung beiIt has also been found that an extremely bulky product can be obtained if the Adding varying amounts of melamine to the basic mixture and heating it in the specified manner. One receives on this way an inorganic non-combustible foam. The amount of melamine to be used is between 1 and 20%, based on the total mixture, depending on the desired bulk weight of the phosphorus nitride oxide to be produced. Preferably 2 to 10% melamine are added to the starting mixture
» einem Molverhältnis von P2O5:OC(NH2J2 von 1:4 angewandt.»A molar ratio of P 2 O 5 : OC (NH 2 J 2 of 1: 4 is used.
Je nach Melamin-Zusatz lassen sich Produkte mit verschiedenen Schüttgewichten erhalten. So erzielt man bei Zusatz von 1% Melamin ein Schüttgewicht von 85,0 g/l; bei 2% Melamin-Zusatz liegt das Schüttgewicht bei 69 g/l; 5% Melamin-Zusatz ergibt ein Produkt mit einem Schüttgewicht von 52 g/l. Erhöht man den Melamin-Zusatz auf über 10%. so werden Produkte mit einem Schüttgewicht über 83 g/l erhalten.Depending on the melamine additive, products with different bulk weights can be obtained. How to achieve with the addition of 1% melamine a bulk density of 85.0 g / l; with 2% melamine added, the bulk weight is at 69 g / l; 5% melamine addition results in a product with a bulk density of 52 g / l. If you increase the Melamine added to over 10%. in this way, products with a bulk density of more than 83 g / l are obtained.
Das Schüttgewicht des nach dem vorliegenden Verfahren ohne Melamin-Zusatz gewonnenen polymeren Phosphornitridoxids liegt bei 250 bis 300 g/l. Im Gegensatz hierzu beträgt das Schüttgewicht des nach bekannten Verfahren hergestellten Produktes ca.The bulk density of the polymer obtained by the present process without the addition of melamine Phosphorus nitride oxide is 250 to 300 g / l. In contrast to this, the bulk density of the after known processes produced product approx.
1000 g/l.1000 g / l.
Die erhaltenen Phosphornitridoxide eignen sich sehr gut zur flammwidrigen Ausrüstung von Polyamid- und Polyurethan-Kunststoffteilen.The phosphorus nitride oxides obtained are very suitable for the flame-retardant finishing of polyamide and Polyurethane plastic parts.
35,5 g P4O10 und 60 g Harnstoff werden gut vermischt im Muffelofen allmählich auf 4000C erhitzt. Nach beendeter Gasentwicklung läßt man abkühlen, zerkleinert die erstarrte Masse und erhitzt das Reaktionsprodukt im trockenen Luftstrom auf 700"C. Nach Abkühlen auf Zimmertemperatur wird grob vorzerklcinert und anschließend gemahlen. Das weiße Pulver besitzt ein Schüttgewicht von 275 g/l.35.5 g P4O10 and 60 g of urea are mixed well in a muffle furnace at 400 0 C gradually heated. When the evolution of gas has ended, the mixture is allowed to cool, the solidified mass is comminuted and the reaction product is heated to 700 ° C. in a stream of dry air. After cooling to room temperature, it is roughly pre-crushed and then ground. The white powder has a bulk density of 275 g / l.
Analyse:Analysis:
Ber.: P 50,81, N 22,97%;
gef.: P 50,2, N 2 i,2%.Calc .: P 50.81, N 22.97%;
Found: P 50.2, N 2 i, 2%.
79 g Harnstoffphosphat und 90 g Harnstoff werden gemeinsam pulverisiert und im elektrischen Ofen langsam auf 400°C erhitzt Wenn die Gasentwicklung nachläßt, zerkleinert man nach dem Abkühlen die erstarrte, spröde Masse und erhitzt im trockenen Sauerstoff- oder Luftstrom 1,5 Stunden auf 750° C. Das voluminöse Produkt wird nach Zerkleinern gemahlen. Schüttgewicht: 260 g/l.79 g urea phosphate and 90 g urea are pulverized together and put in an electric furnace slowly heated to 400 ° C. When the evolution of gas subsides, it is crushed after cooling solidified, brittle mass and heated in a stream of dry oxygen or air for 1.5 hours to 750 ° C. The voluminous product is ground after crushing. Bulk weight: 260 g / l.
Analyse:Analysis:
Ber.: P50,81, N 22,97%;
gef.: P 49,9, N 22,4%.Calc .: P50.81, N 22.97%;
Found: P 49.9, N 22.4%.
120 g gemahlener Harnstoff und 4 g Melamin werden mit 57 g 85%iger Phosphorsäure angeteigt und 1 Stunde bei 120° C gehalten. Dann steigert man die Temperatur allmählich auf 350° C. Nach 1 Stunde zerstößt man die glasartig erstarrte Masse und erhitzt im trockenen Luftstrom auf 700° C. Das Reaktionsprodukt wird, wie oben beschrieben, weiter behandelt. Schüttgewicht: 68120 g of ground urea and 4 g of melamine are used Made into a paste with 57 g of 85% phosphoric acid and kept at 120 ° C. for 1 hour. Then you raise the temperature gradually to 350 ° C. After 1 hour, the glass-like solidified mass is crushed and heated in the dry Air flow to 700 ° C. The reaction product is treated further as described above. Bulk weight: 68
In gleicher Weise kann man verfahren unter Zusatz von 8 g Melamin. Man erhält dann ein Produkt mit einem Schüttgewicht von 54 g/l.The same procedure can be used with the addition of 8 g of melamine. A product is then obtained with a bulk weight of 54 g / l.
Analyse:Analysis:
Ber.: P 50,81, N 22,97%;
gef.: P 50,0, N 23,4%.Calc .: P 50.81, N 22.97%;
Found: P 50.0, N 23.4%.
Man verreibt 45 g Pyrophosphorsäure, 5 g Melamin ίο und 90 g Harnstoff sorgfältig und erhitzt allmählich im elektrischen Ofen auf 350 bis 380° C. Das Reaktionsprodukt wird, wie oben beschrieben, weiter behandelt.45 g of pyrophosphoric acid, 5 g of melamine and 90 g of urea are carefully rubbed in and gradually heated in electric furnace to 350 to 380 ° C. The reaction product is treated further as described above.
57 g Monoammoniumphosphat oder 66 g Diammoniumphosphat werden mit 120 g Harnstoff und 5 g Melamin vermählen und die Mischung langsam auf 400° C erhitzt. Man läßt erkalten, zerkleinert grob und .erhitzt erneut 1,5 Stunden im trockenen Luftstrom auf 700 bis 750° C. Die poröse, äußerst leichte Masse wird grob zerkleinert und gemahlen.57 g of monoammonium phosphate or 66 g of diammonium phosphate are ground with 120 g of urea and 5 g of melamine and the mixture is slowly heated to 400.degree. It is allowed to cool, coarsely crushed and heated again for 1.5 hours in a stream of dry air to 700 to 750 ° C. The porous, extremely light mass is coarsely crushed and ground.
Analyse:Analysis:
Ben: P50,81, N 22,97%;
gef.: P A 9,7, N 23,8%.Ben: P50.81, N 22.97%;
Found: P A 9.7, N 23.8%.
Bei der Umsetzung von Ammoniumpolyphosphat (NH4PO3),, verfahrt man in entsprechender Weise.When converting ammonium polyphosphate (NH4PO3), one proceeds in the same way.
Claims (2)
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19732317282 DE2317282C3 (en) | 1973-04-06 | 1973-04-06 | Process for the preparation of polymeric phosphorus nitride oxides |
NL7404563A NL7404563A (en) | 1973-04-06 | 1974-04-03 | |
BE142911A BE813373A (en) | 1973-04-06 | 1974-04-05 | PROCESS FOR PREPARING POLYMERIC PHOSPHORYL NITRIDES |
GB1513874A GB1461615A (en) | 1973-04-06 | 1974-04-05 | Preparation of polymeric phosphorous nitride oxide |
IT5020174A IT1015906B (en) | 1973-04-06 | 1974-04-05 | PROCEDURE FOR THE PREPARATION OF POLYMER PHOSPHORUS AZIDE OXIDES |
FR7412274A FR2224511B1 (en) | 1973-04-06 | 1974-04-08 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19732317282 DE2317282C3 (en) | 1973-04-06 | 1973-04-06 | Process for the preparation of polymeric phosphorus nitride oxides |
Publications (3)
Publication Number | Publication Date |
---|---|
DE2317282A1 DE2317282A1 (en) | 1974-10-24 |
DE2317282B2 DE2317282B2 (en) | 1978-04-20 |
DE2317282C3 true DE2317282C3 (en) | 1978-12-14 |
Family
ID=5877215
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE19732317282 Expired DE2317282C3 (en) | 1973-04-06 | 1973-04-06 | Process for the preparation of polymeric phosphorus nitride oxides |
Country Status (3)
Country | Link |
---|---|
BE (1) | BE813373A (en) |
DE (1) | DE2317282C3 (en) |
NL (1) | NL7404563A (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2800467A1 (en) | 1978-01-05 | 1979-07-12 | Bayer Ag | FLAME RESISTANT POLYAMIDE MOLDING COMPOUNDS |
-
1973
- 1973-04-06 DE DE19732317282 patent/DE2317282C3/en not_active Expired
-
1974
- 1974-04-03 NL NL7404563A patent/NL7404563A/xx not_active Application Discontinuation
- 1974-04-05 BE BE142911A patent/BE813373A/en unknown
Also Published As
Publication number | Publication date |
---|---|
DE2317282B2 (en) | 1978-04-20 |
DE2317282A1 (en) | 1974-10-24 |
NL7404563A (en) | 1974-10-08 |
BE813373A (en) | 1974-07-31 |
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