2010
DOI: 10.1007/s11743-009-1153-3
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Synthesis of High Purity Mono‐Alkyl Phosphate Using Cyclic Polyphosphoric Acid

Abstract: The uniform design method was used to study the synthesis of high purity mono-alkyl phosphate (MAP) by cyclic polyphosphoric acid. The main factors influencing the content of mono-alkyl phosphate were investigated. The experimental results were analyzed by regression, and the optimum conditions were found to be as follows: mass pentoxide/mass 85 wt% phosphoric acid/mass octanol = 14.2/5.62/48.5, reaction temperature: 115°C, reaction time: 8 h. Under the optimized conditions, a high purity mono-alkyl phosphate … Show more

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Cited by 8 publications
(6 citation statements)
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“…The 31 P NMR spectra were tested by silylating the samples with hexamethyldisilazane in CDCl 3 , unless otherwise stated. Hydrogen bromide–acetic acid solution was used for the titration of epoxide and an indicator method was used for the titration of acid content in PCO .…”
Section: Methodsmentioning
confidence: 99%
“…The 31 P NMR spectra were tested by silylating the samples with hexamethyldisilazane in CDCl 3 , unless otherwise stated. Hydrogen bromide–acetic acid solution was used for the titration of epoxide and an indicator method was used for the titration of acid content in PCO .…”
Section: Methodsmentioning
confidence: 99%
“…Chemical shifts were referred to the solvent peak (δ 7.26 for the residue peak of CDCl 3 and 4.79 for D 2 O). Hydrogen bromide/acetic acid solution was used for titratation of epoxide, and the indicator method was used for the titrations of P-PEG-P …”
Section: Methodsmentioning
confidence: 99%
“…The double indicator analysis method (Lin et al, ; Tian and Dong, ; Ye and Yan, ) was adopted to determine the content of MAP, DAP, and H 3 PO 4 in alkyl phosphates. Two samples of 0.5 g were placed in the two conical flasks of 250 mL, and n‐ propanol of 45 mL was added into the conical flask.…”
Section: Methodsmentioning
confidence: 99%
“…Until now, the preparation of alkyl phosphates has been mainly focused on low‐carbon alkyl phosphates (Clarke and Lyons, ; Davis, ; Du and Zhou, ; Hansell and Faulkner, ; He et al, ; Jiang, ; Lee, ; Li et al, ; Obata and Mukaiyama, ; Okabe et al, ; Okamato, ; Qiang et al, ; Ren et al, ; Thilo and Sauer, ; Wang, ; Wu et al, ; Xia et al, ; Ye and Yan, ), and little attention has been paid to the preparation of alkyl phosphates with alkyl chain length above 18, since the reactions between high‐carbon alcohols and phosphorylating reagents are difficult without solvents to obtain the high‐carbon alkyl phosphates. He et al () prepared octadecyl phosphates by means of removing water from azeotropic solvents, and Xu et al () adopted the method of adding solvent to synthesize the high‐carbon alkyl phosphates from C18 to C22.…”
Section: Introductionmentioning
confidence: 99%