Solubilities of Some Phosphaspirocyclic Compounds in Selected Solvents

Abstract

The solubilities of 3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane-3,9- dioxide from (303.15 to 311.35) K in dichloromethane and from (298.15 to 357.65) K in acetic acid, 3,9-dihydroxy-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane-3,9-dioxide from (309.35 to 331.55) K in acetonitrile and from (295.75 to 319.15) K in acetone, 2,4,8,10-tetraoxa-3,9-dioxide-3,9-diphosphaspiro[5.5]undecane-3,9-melamine salt from (293.15 to 343.15) K in water, and 3,9-(bis-2,2‘-carboxyetheyl)-3,9-dioxo-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5] undecane from (332.15 to 342.15) K in ethyl acetate were determined using a gravimetric method. The estimated uncertainty of all the solubility values based on error analysis and repeated observations was within 2.5 %.

Synthesis, characteristic of a novel flame retardant containing phosphorus and its application in poly(ethylene‐co‐vinyl acetate)

“…After the reaction, the appearance of the absorption peak at 104−1126 cm −1 for P-O-C group of SPDPC and the disappearance of the chemical shifts at 3.32 ppm for the hydroxyl group of PER was observed respectively by FTIR ( Figure 1) and 1 H NMR (Figure 2(a)). The FTIR analysis of SPDPC in detail is as follows: 534-589 (P-Cl), 1206 (P = O), 1477 (CH 2 ), and was in accordance with the reported literature [26]. Meanwhile, the 1 H NMR and 31 P NMR spectrum of SPDPC shown in Figure 2 further demonstrated the structure of SPDPC: the chemical shifts at 4.21-4.24 ppm (Figure 2(a)) resulted from the eight hydrogens of the spirocycle; the only one chemical shift at −6.2 ppm for the P in the spirocycle was observed in Figure 2(b) Moreover, the reactant DOPO-HQ was characterized by 1 H NMR (Figure 3(a)) and 31 P NMR (Figure 3(b)) spectrum.…”

Synthesis of a phosphorus‐ and nitrogen‐containing flame retardant and evaluation of its application in waterborne polyurethane

“…Pentaerythritol diphosphonate dichloride (PDD) was synthesized according to Wang et al . First, 20.0 g of pentaerythritol and 80 mL of POCl 3 were put into a 250 mL round‐bottom flask with a tail gas treatment device, stirred and heated to 80 °C, and refluxed for 1 h. It was then slowly heated up to 105 °C and refluxed for 12 h until no HCl gas was released.…”

“…Pentaerythritol diphosphonate ester (PDE) was synthesized according to Wang et al . First, 14.8 g of PDD was suspended in 100 mL of acetonitrile, and the suspension was put into a 250 mL round‐bottom flask with a tail gas treatment device, and stirred and heated up to 105 °C.…”

A Novel Spirocyclic Halogen-Free Flame Retardant: Synthesis and Flammability Characteristics in Epoxy Resin Composites

“…Synthesis of ISCP. As shown in Scheme 1, the intermediate SPDPC was synthesized by esterification reaction of PER and POCl 3 according to previous literature [5]. Afterwards, dichloromethane (50 mL), imidazole (1.64 g, 0.024 mol) and SPDPC (2.97 g, 0.01 mol) were mixed in a 250 mL three-neck flask equipped with a mechanical stirrer, a thermometer, a reflux condenser and HCl absorption device.…”