Melt phosphates

The manufacture of these glassy polyphosphates or melt phosphates occurs as follows ... 

Melt phosphates A product with a P2O5 content of ca. 21% is obtained by melting apatite with magnesium compounds and silica. These fertilizers are mainly manufactured in Eastern Asia (capacity in Japan and Korea 670 10 t/a). 

Titrimetric determination The mannitol or glycerol acid-base titration procedure is applied to the dissolved sodium carbonate melt for the determination of milligram amounts of B2O3. A blank prepared from a glass that does not contain boric oxide should be subjected to the same procedure. There are certain interferences the effect of fluoride is eliminated by adding calcium carbonate to the fusion mixture lead and zinc can be filtered off after dissolution of the melt phosphate is precipitated by addition of iron(ni) chloride. The influence of some interference from such elements as aluminum or titanium can be eliminated by adding ethylenediaminetetraacetic acid (EDTA). 

The so-called oxynitride glasses can be obtained by melting phosphate salts in an atmosphere of ammonia, or alternatively by melting a nitride such as Mg3N2 with sodium metaphosphate. 

Figure 6.10.2 The effect of the initial PO/ RE mole ratio on precipitation of rare earth phosphates from NaCI-2CsCI based melts. Phosphate added as Na PO, temperature 550° C, time of experiments = 4h...

A bicychc pentaerythritol phosphate, CN-1197, has more recently been introduced by Great Lakes Chemical for use in thermosets, preferably in combination with melamine or ammonium polyphosphate (89). It is a high melting soHd befleved to have the following stmcture [5301-78-0] (87) ... 

Garbodiimide Formation. Carbodiimide formation has commercial significance in the manufacture of Hquid MDI. Heating of MDI in the presence of catalytic amounts of phosphine oxides or alkyl phosphates leads to partial conversion of isocyanate into carbodiimide (95). The carbodiimide (39) species reacts with excess isocyanate to form a 2 + 2cycloaddition product. The presence of this product in MDI leads to a melting point depression and thus a mixture which is Hquid at room temperature. 

Flame retardants (qv) are incorporated into the formulations in amounts necessary to satisfy existing requirements. Reactive-type diols, such as A/ A/-bis(2-hydroxyethyl)aminomethylphosphonate (Fyrol 6), are preferred, but nonreactive phosphates (Fyrol CEF, Fyrol PCF) are also used. Often, the necessary results are achieved using mineral fillers, such as alumina trihydrate or melamine. Melamine melts away from the flame and forms both a nonflammable gaseous environment and a molten barrier that helps to isolate the combustible polyurethane foam from the flame. Alumina trihydrate releases water of hydration to cool the flame, forming a noncombustible inorganic protective char at the flame front. Flame-resistant upholstery fabric or liners are also used (27). 

The salts containing polymeric anions in die solid state melt retain die anion stiiicture, e.g. and on melting, while die phosphates in which die... 

Dried with Linde type 5A molecular sieves or Na2S04 and fractionally distd at reduced pressure. Alternatively, it was refluxed with, and distd from, BaO. Also purified by fractional crystn from the melt and distd from zinc dust. Converted to its phosphate (m 135°) or picrate (m 223°), which were purified by crystn and the free base recovered and distd. [Packer, Vaughn and Wong J Am Chem Soc 80 905 1958.] The procedure for purifying via the picrate comprises the addition of quinoline to picric acid dissolved in the minimum volume of 95% EtOH to yield yellow crystals which are washed with EtOH and air dried before recrystn from acetonitrile. The crystals are dissolved in dimethyl sulfoxide (previously dried over 4A molecular sieves) and passed through a basic alumina column, on which picric acid is adsorbed. The free base in the effluent is extracted with n-pentane and distd under vacuum. Traces of solvent are removed by vapour phase chromatography. [Mooman and Anton J Phys Chem 80 2243 1976.]... 

In a typical process adiponitrile is formed by the interaction of adipic acid and gaseous ammonia in the presence of a boron phosphate catalyst at 305-350°C. The adiponitrile is purified and then subjected to continuous hydrogenation at 130°C and 4000 Ibf/in (28 MPa) pressure in the presence of excess ammonia and a cobalt catalyst. By-products such as hexamethyleneimine are formed but the quantity produced is minimized by the use of excess ammonia. Pure hexamethylenediamine (boiling point 90-92°C at 14mmHg pressure, melting point 39°C) is obtained by distillation, Hexamethylenediamine is also prepared commercially from butadience. The butadiene feedstock is of relatively low cost but it does use substantial quantities of hydrogen cyanide. The process developed by Du Pont may be given schematically as ... 

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