- Purification method of hexaphenoxy cyclotriphosphazene
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The invention discloses a purification method of hexaphenoxy cyclotriphosphazene. The method comprises the following steps: firstly, adding a 5-10% sodium hydroxide solution into a hexaphenoxy cyclotriphosphazene synthesis liquid, stirring for 10 to 30 minutes at room temperature, standing, separating out a water phase, adding water, stirring at room temperature for 10-30 minutes, standing, separating out the water phase, adding a 5-10% hydrochloric acid solution, stirring at room temperature for 10-30 minutes, standing, separating out the water phase, adding water, stirring at room temperature for 10-30 minutes, standing, and separating out the water phase; finally steaming out chlorobenzene in the washed oil phase to obtain a hexaphenoxy cyclotriphosphazene crude product; and heating anddissolving the crude product with absolute ethyl alcohol, cooling to -10-0 DEG C, crystallizing for 4 to 8 hours, filtering, washing a filter cake with absolute ethyl alcohol twice, and drying at 90to 100 DEG C until the weight is constant so as to obtain the hexaphenoxy cyclotriphosphazene. According to the purification method disclosed by the invention, the yield of the hexaphenoxy cyclotriphosphazene is remarkably improved.
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Paragraph 0017-0019
(2020/10/30)
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- Phosphazene compound, composite containing phosphazene compound, flame retardant containing composite and application
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The invention relates to a phosphazene compound, a composite containing the phosphazene compound, a flame retardant containing the composite and application. The crystal form of the cyclotriphosphazene derivative flame retardant synthesized by using the method is most stable, and the cyclotriphosphazene derivative flame retardant is high in heat stability and high in flame retardant efficiency; moreover, when the crystal type cyclotriphosphazene derivative flame retardant synthesized by using the method is added into a material, such as engineering plastics, general-purpose plastics, a lithiumion battery electrolyte, a flame retardant fabric and flame retardant paper, a high flame retardant performance is achieved, the crystal form is stable, the flame retardant is resistant to drip, onlyan extremely small adding amount is needed, the flame retardant performance of the material can reach the V-0 standards, and other properties of the material are little affected.
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Paragraph 0221; 0224-0227
(2019/01/23)
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- ALLYL-PHENOXY-CYCLOPHOSPHAZENE COMPOUND, AND PRODUCTION METHOD THEREFOR
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An object of the present invention is to provide a mixture of cyclophosphazenes suitably substituted with phenoxy having a polymerizable functional group, such as allyl, on the phenyl ring and a production method for the mixture. The invention relates to a mixture of cyclophosphazene compounds that each contain a plurality of constituent units linked to each other, each constituent unit being represented by formula (I): wherein R1 and R2 are identical or different and represent C1-4 alkyl or the like, the mixture containing cyclophosphazene compounds in which 3, 4, and 5 constituent units represented by formula (I) are linked, wherein the cyclophosphazene compound containing 3 linked constituent units is cyclophosphazene compound (I-A) with a specific structure, compound (I-A) includes cyclophosphazene compounds (I-A2) and (I-A3) having a specific structure, and compounds (I-A2) and (I-A3) are present in an amount of 80 wt % or more in total in cyclophosphazene compound (I-A).
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Paragraph 0217
(2018/06/15)
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- Preparation method of hexaphenoxycyclotriphosphazene
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The invention discloses a preparation method of hexaphenoxycyclotriphosphazene. The preparation method comprises the following steps: (1) adding ammonium chloride, an inert solvent and a catalyst into a synthesis kettle, heating to 100-145 DEG C, uniformly putting phosphorus pentachloride into the synthesis kettle within 5-40 hours, and after the reaction is ended, carrying out filtrate concentration and cooling crystallization to obtain phosphonitrilic chloride trimer; (2) adding the inert solvent, phenol, alkali metal hydroxide and water into the synthesis kettle, heating to 100-145 DEG C, dropwise adding an inert solvent solution of phosphonitrilic chloride trimer after azeotropic separation of water, insulating and carrying out reflux reaction; and (3) adding a chloride-ion removing agent, continuously reacting for 3-6 hours at the temperature of 100-135 DEG C, then carrying out alkali washing, acid washing, water washing and steam distillation, and drying to obtain granular hexaphenoxycyclotriphosphazene with low chloride content. The preparation method disclosed by the invention has the advantages that the process is simple, the obtained product is low in chloride content and the stability is good in the use process.
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Paragraph 0025; 0034; 0038; 00424; 0046; 0049; 0057
(2018/01/13)
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- Cyclotriphosphazene compound, preparing method thereof, electrolyte for lithium secodary battery, and lithium secodary battery including the same
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A cyclotriphosphazene compound in which at least one fluorine is substituted with a group represented by formula 1 below, a preparing method thereof, an electrolyte for a lithium secondary battery including the cyclotriphosphazene compound, and a lithium secondary battery including the electrolyte are provided. Formula 1 is *A-B-CN, where A is a heteroatom having an unshared electron pair, * represents a combined site of the fluorinated cyclotriphosphazene compound with phosphor (P), and B is a substituted or unsubstituted alkylene group having 1 to 5 carbon atoms.
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Paragraph 0128-0134
(2017/08/19)
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- N-P flameresistant material and preparation method thereof and application in textiles
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The invention discloses an N-P flameresistant material and a preparation method thereof and application in textiles. The chemical name of a flame retardant of the material is hexa(1-oxo-phospha-2,6,7-trioxabicyclo[2,2,2]octane-4-methylenedioxy)cyclotriphosphazene (HCPPA); the preparation method of the material comprises the steps of synthesizing hexachlorocyclotriphosphazene (HCPP) by reacting ammonium chloride with phosphorus pentachloride, wherein a catalyst is pyridine and ZnO; then synthesizing 1-oxo-phospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2,2,2]octane (PEPA) by reacting pentaerythritol with phosphorus oxychloride; finally synthesizing the HCPPA by reacting the HCPP with the PEPA. According to the preparation method, NaH is used as a catalyst, so that the synthesis reactions can be performed quickly, the reaction time is greatly shortened, and the product yield is improved. When the N-P flame retardant is used for retarding a flame of a cotton fabric, high limit oxygen index and char yield are achieved, and the wash durability is good.
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Paragraph 0046; 0047; 0048
(2016/10/08)
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- Method for synthesis of phosphazene hydrophobic polystyrene thin film with the synthesis device, three luen phenyl ring and method for preparing Phosphazenium
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The invention discloses a synthesizing method and a synthesizing device of phosphonitrilic chloride trimer as well as a preparation method of terphenyl cycloposphazene. The synthesizing method of the phosphonitrilic chloride trimer comprises the following steps: A1, adding powdered ammonium chloride and phosphorus pentachloride into a ceramic reaction kettle in a weight ratio of (900-1500):3000; A2, adding zinc chloride, heating and stirring to react, constantly dripping an acid-binding agent during stirring, wherein the weight ratio of zinc chloride to phosphorus pentachloride is (20-35):3000, the weight ratio of the acid-binding agent to the phosphorus pentachloride is (30-50):3000, the reacting temperature is 65-150 DEG C, and the reacting time is 1.5-2.5 hours; and A3, feeding to sublimation purifying equipment by adopting a closed screw rod, heating to 125-135 DEG C, and sublimating to obtain the phosphonitrilic chloride trimer.
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Paragraph 0028; 0032; 0033
(2018/02/04)
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- Structure and conformation of the medium-sized chlorophosphazene rings
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Medium-sized cyclic oligomeric phosphazenes [PCl2N]m (where m = 5-9) that were prepared from the reaction of PCl5 and NH4Cl in refluxing chlorobenzene have been isolated by a combination of sublimation/extraction and column chromatography from the predominant products [PCl2N]3 and [PCl2N]4. The medium-sized rings [PCl2N]m have been characterized by electrospray ionization-mass spectroscopy (ESI-MS), their 31P chemical shifts have been reassigned, and their T1 relaxation times have been obtained. Crystallographic data has been recollected for [PCl 2N]5, and the crystal structures of [PCl 2N]6, and [PCl2N]8 are reported. Halogen-bonding interactions were observed in all the crystal structures of cyclic [PCl2N]m (m = 3-5, 6, 8). The crystal structures of [P(OPh)2N]7 and [P(OPh)2N]8, which are derivatives of the respective [PCl2N]m, are also reported. Comparisons of the intermolecular forces and torsion angles of [PCl2N]8 and [P(OPh)2N]8 with those of three other octameric rings are described. The comparisons show that chlorophosphazenes should not be considered prototypical, in terms of solid-state structure, because of the strong influence of halogen bonding.
- Bowers, David J.,Wright, Brian D.,Scionti, Vincenzo,Schultz, Anthony,Panzner, Matthew J.,Twum, Eric B.,Li, Lin-Lin,Katzenmeyer, Bryan C.,Thome, Benjamin S.,Rinaldi, Peter L.,Wesdemiotis, Chrys,Youngs, Wiley J.,Tessier, Claire A.
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p. 8874 - 8886
(2014/12/09)
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- Halogenated hydroxy-aryloxy phosphazenes and epoxy oligomers based on them
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By partial substitution of the chlorine atoms in hexachlorocyclotriphosphazene for halophenols and subsequent reaction of the resulting halogenated phenoxy phosphazene and 2,2-di(4-hydroxyphenyl)propane monophenolate hydtoxy-aryloxy phosphazenes were synthesized with a molecular weight of 1100-1400 g mol-1. Epoxide oligomers (epoxy number of 6-8%), which are cured with the formation of non-combustible compositions [PV-0 class of resistance to combustion according to State Standard (GOST 28157-89)], were obtained by reaction of these compounds with epichlorohydrin. Introduction of 5-50 wt% halogenated epoxyphophazene oligomers in industrial resin ED-20 can significantly improve the fl ame resistance of compositions based on these compounds. Pleiades Publishing, Ltd., 2013.
- Terekhov,Filatov,Chistyakov,Borisov,Kireev
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p. 1600 - 1604
(2014/02/14)
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- Synthesis and characterization of glycine substituted cyclotriphosphazenide
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Glycine substituted adduct of (PNCI2)3 was synthesized and characterized on the basis of qualitative, quantitative, TLC, FTIR and mass spectral analysis. The chemical data assigned as (P 3N3)2H2(NH2CH 2COO)8NHCH2COO, having NHCH2COO- bridging between two (P3N3) rings along with other glycinic group linked to P atom of P3N3 rings.
- Singh, Santosh Kumar,Jadon
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p. 1489 - 1492
(2014/01/17)
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- Synthesis and structure of hexa-p-acetamidophenoxycyclotriphosphazene
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Hexa-p-acetamidophenoxycyclotriphosphazene was synthesized and examined by the 31P and 1H NMR spectroscopy and XRD analysis. Original Russian Text.
- Chistyakov, E. M.,Filatov, S. N.,Kireev, V. V.,Lysenko, K. A.,Buzin, M. I.,Chuev, V. P.
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p. 1065 - 1068,4
(2020/08/31)
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- X-ray crystal structures and DFT calculations of differently charged aminocyclophosphazenes
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Molecular structures of hexakis(amino)cyclotriphosphazene, N3P3(NH2)6, neutral and cationic forms of hexakis(ethylamino)cyclotriphosphazene, N3P3(NHC2H5)6,
- Vorontsov, Ivan I.,Tur, Dzidra R.,Papkov, Vladimir S.,Antipin, Mikhail Yu.
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- Probing the mechanism of the PCl5-initiated living cationic polymerization of the phosphoranimine Cl3P=NSiMe3 using model compound chemistry
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New insight into the mechanism of the ambient temperature PCl5-initiatedliving cationic chain growth polycondensation of the N-silylphosphorani mine Cl3P=NSiMe3 (1) to give poly(dichlorophosphazene), [N=PCl2]n,has been provided by studies of model compound chemistry. Investigations of the reactivity of Cl- salts ofthe proposed cationic intermediates [Cl3P=N=PCl3] + ([2] +) and [Cl3PdN-PCl2dNdPCl3] + ([6]+) toward Ph3P=NSiMe3 (3a) provided evidence that under the usual polymerization conditions that involve a high monomer to initiator ratio, propagation occurs at both chain ends. However, analogous studies of near stoichiometric processes suggested that propagation is faster at one chain end, particularly when the chains are short. In addition, experiments involving [Ph3P=N=PPh3][PCl6] ([9][PCl6]) and the N-silylphosphoranimines R3P-NSiMe 3 3a (R = Ph) and 3b (R = p-CF3C6H 4),showed that the [PCl6]- anion, which is formed in the early stages of the polymerization and has hitherto been assumed to be an innocent spectator counteranion, is actually reactive under the r eaction conditions and can initiate oligomerization and polymerization. Finally, the absence of reactions between phosphoranimines 3b or 1 with the Cl- salts of the cations [Ph3P=N-PCl2=N=PPh3]+ ([10a]+), [Ph3P=N-(PCl2=N) 2= PPh3]+ ([5]+), and [Ph3P=N-(PCl 2=N) 3-PPh3]+ ([8]+) with P-Cl bonds located internally but not at the chain ends have shown that chain branching reactions are unlikely to be significant during the polymerization. These results identify key factors that complicate the living PCl5-initiated chain growth polycondensation of 1 and potentially lead to a loss of control over molecular weight and broaden the molecular weight distributions, but also indicate that the polymer formed is essentially linear rather than branched.
- Blackstone, Vivienne,Lough, Alan J.,Murray, Martin,Manners, Ian
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p. 3658 - 3667
(2009/09/24)
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- Process For Producing Phosphonitrilic Acid Ester
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A process for producing a cyclic and/or linear phosphonitrilic acid ester from a cyclic and/or linear phosphonitrile dichloride is provided, wherein the reaction time is shorter and the content of monochloro phosphazenes is very small. When phosphonitrile dichloride is reacted with a metal arylolate and/or a metal alcoholate in the presence of a reaction solvent, a metal arylolate and/or a metal alcoholate composed of at least two different metals having different ionization energies is used and also a specific compound is used as a catalyst.
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Page/Page column 14
(2008/06/13)
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- Synthesis and characterization of some transition metal complexes of trimeric and tetrameric aminocyclophosphazenes
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Reactions of aminocyclotri-and aminocyclotetra-phosphazenes, viz., N3P3L6 and N4P4L8 (L = -HN(sec- C4H9) -NHC6H11, - HNC8H17, -NC5H10 and -NC4H8O) with hydrated Cu(II), Co(II), Ni(II) and Fe(III) chlorides have been studied. CuCl2.2H2O give only [(N3P3L6H or N4P4L8H)CuCl3] whereas with CoCl2.6H2O, a mixture of two products, namely, [(N3P3L6H or N4P4L8H)CoCl3] and [(N3P3L6H or N4P4L8H)]2[CoCl4] are recovered. FeCl3.6H2O and NiCl2.6H2O give only ionic products of the type [(N3P3L6)H)][FeCl4] and [(N3P3L6H)]2[NiCl4]. A few reactions of N2P3L6 (L=-HN(sec-C4H9). -HNC6H13 and -HNC8H17) with Mo(CO)6 have also been carried out. In these reactions [(N3P3L6)Mo(CO)3] derivatives are obtained. The complexes have been characterized by analytical data, conductivity, magnetic and IR measurements.
- Shrimal,Srivastava,Pandey,Agrawal
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p. 528 - 533
(2007/10/03)
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- A new route to the phosphazene polymerization precursors, Cl3P=NSiMe3 and (NPCl2)3
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An improved synthesis of the phosphazene polymerization precursors, hexachlorocyclotriphosphazene, (NPCl2)3 (1), and Cl3P=NSiMe3 (2) is reported. The addition of PCl5 to N(SiMe3)3 in methylene chloride at 40 °C produced a mixture of phosphazenes which contained 76% of 1. However, the addition of N(SiMe3)3 to PCl5 in methylene chloride at 0 °C, followed by the addition of hexane, provided 2 in 40% yield. The mechanism of the reaction is discussed.
- Allcock, Harry R.,Crane, Chester A.,Morrissey, Christopher T.,Olshavsky, Michael A.
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p. 280 - 283
(2008/10/08)
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- Phosphazenes on diatomaceous earths in water adsorption
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Hexachlorocyclotriphosphazene (T) and poly-bis-(trifluoroethoxy) phosphazene (A) deposited separately on wide-pore kieselguhr supports result in composite adsorbents of an increased adsorption capacity for water vapour per unit surface area. Deposition alters the adsorption behaviour of T and A themselves due to high dispersion and conformation changes of polymer chains within the pores in comparison with the initial solid state.
- Gocheva, E.,Vassileva, P.,Lakov, L.,Peshev, O.
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- Reactions of Alkali-metal Azides with some Organophosphorus(V) Compounds
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The reactions of Li or Na with some organophosphorus(V) compounds containing chloro-groups, including PCl5(py) (py = pyridine) and catechyl derivates of PCl5, have been investigated by I31IP n.m.r. spectroscopy.Several new azido-species have been
- Dillon, Keith B.,Platt, Andrew W. G.,Waddington, Thomas C.
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p. 2292 - 2295
(2007/10/02)
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- Optimized Synthesis and Mechanism of Formation of 2,4-Dichloro-1,3-bis(dichlorophosphoryl)-2,4-dioxocyclodiphosph(v)azane from Phosphoryl Chloride and Ammonium Chloride
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Detailed investigation of the reaction between Cl and an excess of POCl3 has established a procedure for isolation of the main product, the novel title cyclodiphosph(v)azane, and permitted the identification of three other reaction products, namely, pyrophosphoryl chloride, hexachlorocyclotriphosph(v)azane, and PPP-trichloro-N-dichlorophosphorylmonophosph(v)azane.A reaction mechanism is proposed which accounts for the formation of all four products.
- Jaeger, Roger De,Taylor, David R.
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p. 851 - 853
(2007/10/02)
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