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FLUID PHASE EQUILIBRIA · 2014 · IF 2.241

Solubilities of phosphoric acid, P,P′-1,4-phenylene P,P,P′,P′-tetraphenyl ester in the organic solvents

Guo-Min Yu,Li-Sheng Wang,Chao-Jun Du,Jian Sun

A phosphorous flame retardant of phosphoric acid , P , P ′-1,4-phenylene P , P , P ′, P ′-tetraphenyl ester (PAPTE) was synthesized by diphenyl chlorophosphate and hydroquinone . The structural features of PAPTE were investigated with mass spectra (MS), infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR) and high-performance liquid chromatograph (HPLC) methods. The thermal behavior of PAPTE was analyzed with differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA) instruments. A static analytic method was used to measure the solubilities of PAPTE in the several selected pure solvents, which are methanol, ethanol, acetone, ethyl acetate , acetonitrile , methyl acetate , toluene, ether, n -propanol, i -propanol, where the temperatures range is from 288.25 to 333.45   K. The experiments were also performed in the binary mixed solvents of acetone and methanol. Several thermodynamic models were used to correlate the experimental solubility data, such as Wilson, nonrandom two-liquid (NRTL), UNIQUAC equations. The solubility data of PAPTE in binary solvents were correlated with the modified Wilson model. The calculated results showed that those models can excellently reproduce the experimental data and the UNIQUAC equation reveals the better ability in correlation. Using the Scatchard–Hildebrand methodology, the activity coefficients, solubility parameter of the solute and the partial molar excess enthalpies at infinite dilution were calculated.

研究领域: 化学工程 · 材料科学
✓ 已验证 DOI 高影响因子
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Reactions · 2024 ·Vol. 5 ·期 4 ·812-822 · IF 2.2

Continuous Flow Optimisation of the Pudovik Reaction and Phospha-Brook Rearrangement Using DBN

Joseph Dean,Natalia Buckler Reinoso,Francesco Spiedo,Carola Romero Fernández,Bhaven Patel

Flow chemistry has shown significant versatility over the last two decades, offering advantages in efficiency, scalability, and sustainability. In this study, the continuous stirred tank reactor (CSTR) was used to optimise the synthesis of α-hydroxyphosphonates via the Pudovik reaction and their subsequent conversion to phosphates through the phospha-Brook rearrangement. The study highlights that using CSTRs allows for better control over reaction parameters, leading to reduced reaction times and improved yields compared to traditional batch methods. The optimised conditions successfully facilitated a range of organophosphates, including electron-rich and electron-poor derivatives, with high efficiency. Additionally, a one-pot tandem process combining the Pudovik reaction and the phospha-Brook rearrangement was developed, reducing reaction times to two hours while maintaining comparable yields. This work demonstrates the potential of CSTRs in flow chemistry for synthesising complex organophosphorus compounds, achieving higher reaction yields and shorter reaction times, highlighting the effectiveness of continuous flow methodologies.

研究领域: 有机化学 · 合成化学 · 流程优化
✓ 已验证 DOI 高影响因子
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POLYMER DEGRADATION AND STABILITY · 2024 · IF 6.3

A discovery for phosphorus valence and unsaturated bonds in polyphosphate/polyphosphonate: Promotion or inhibition for its flame-retardant mode of action in PET

Bo Xu,Meng Jia,Dong Wang,Siheng Zhao,Shouao Zhu,Lijun Qian

Four polyphosphate/polyphosphonate flame retardants (PAP, POP, PAP-UB and POP-UB) have been designed and synthesized to study the effects of phosphorus valence states and the presence of unsaturated carbon-carbon double bonds on self-cross-linking impacting flame-retardant modes of action. It was found that phosphorus valence states affect the proportion of flame-retardant activity between the gas phase and condensed phase. A phosphonate containing +3-valence phosphorus is primarily effective as a gas-phase flame-retardant, while the one containing +5-valence phosphorus mainly exerted an impact in the condensed phase. The introduction of an unsaturated bond enhances the carbon-forming effect promoted by polyphosphates/polyphosphonates in a degrading polymer matrix and increases the melt viscosity for blends at high temperature. The phosphorus-containing fragments which might have been released into the gas phase are locked in the condensed phase due to C C bonds cross-linking, thus forming more high-quality phosphorus-rich char layers. This effect balances the distribution of gas-phase and condense-phase flame-retardant effects and is especially obvious in PET/polyphosphonate blends containing +3-valence phosphorus, which originally plays mainly the role of a gas-phase flame retardant . PET blends containing unsaturated carbon-carbon double bonds display better carbon formation, flame-retardant activity and anti-dripping behavior than these do without this feature.

研究领域: 材料科学 · 化学
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HYDROMETALLURGY · 2016 · IF 2.29

Selective extraction and separation of Ce(IV) from thorium and trivalent rare earths in sulfate medium by an α-aminophosphonate extractant

Shengting Kuang,Zhifeng Zhang,Yanling Li,Guolong Wu,Haiqin Wei,Wuping Liao

A novel extractant, di (2-ethylhexyl) (2-((2-ethylhexyl) amino) propan-2-yl) phosphonate (DEHAPP, abbreviated as B ), was synthesized for the selective extraction of Ce(IV) in sulfate medium. The effect of contact time, the H 2 SO 4 concentration, the DEHAPP concentration and temperature on the Ce(IV) extraction were studied systematically. DEHAPP exhibits a good extraction ability towards Ce(IV) when compared with other neutral organophosphorus extractants such as Cyanex 923, Cyanex 925 and DEHEHP. The extraction equilibrium constants and thermodynamic parameters (Δ G , Δ H and Δ S ) were calculated. The extraction reaction of Ce(IV) is an endothermic process. The extracted complexes were determined to be H 2 SO 4 · B ( org ) and Ce(HSO 4 ) 2 SO 4 ·2 B ( org ) . A extraction process to selectively recover Ce(IV) from bastnaesite leaching was proposed, by which the purity of cerium product reached 99.5% with a yield of 90.7%.

CAS / MDL: 104-75-6
研究领域: 化学工程 · 材料科学
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Frontiers in Microbiology · 2024 · IF 4

Correlation of methane production with physiological traits in Trichodesmium IMS 101 grown with methylphosphonate at different temperatures

Chuze Zou,Xiangqi Yi,He Li,Mina Bizic,Ilana Berman-Frank,Kunshan Gao

The diazotrophic cyanobacterium Trichodesmium has been recognized as a potentially significant contributor to aerobic methane generation via several mechanisms including the utilization of methylphophonate (MPn) as a source of phosphorus. Currently, there is no information about how environmental factors regulate methane production by Trichodesmium. Here, we grew Trichodesmium IMS101 at five temperatures ranging from 16 to 31°C, and found that its methane production rates increased with rising temperatures to peak (1.028 ± 0.040 nmol CH4 μmol POC−1 day−1) at 27°C, and then declined. Its specific growth rate changed from 0.03 ± 0.01 d−1 to 0.34 ± 0.02 d−1, with the optimal growth temperature identified between 27 and 31°C. Within the tested temperature range the Q10 for the methane production rate was 4.6 ± 0.7, indicating a high sensitivity to thermal changes. In parallel, the methane production rates showed robust positive correlations with the assimilation rates of carbon, nitrogen, and phosphorus, resulting in the methane production quotients (molar ratio of carbon, nitrogen, or phosphorus assimilated to methane produced) of 227–494 for carbon, 40–128 for nitrogen, and 1.8–3.4 for phosphorus within the tested temperature range. Based on the experimental data, we estimated that the methane released from Trichodesmium can offset about 1% of its CO2 mitigation effects.

研究领域: 微生物学 · 海洋生物学 · 环境科学
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Journal of Environmental Chemical Engineering · 2024 · IF 7.4

Aminophosphonate/sand nanocomposites for La(III) sorption: Application to REE concentrate

Ibrahim El-Tantawy El-Sayed,Xingmei Lu,Jiayu Xin,Azza A. Al-Ghamdi,Enas A. Imam,Hamada B. Hawash,Ahmed A. Galhoum,S. Wageh

Two α-aminophosphonate anlages (methyl- and phenyl-derivatives, MeAP and PhAP, respectively) were synthesized via an in-situ reaction. Moreover, their corresponding sand nanocomposites, MeAPNC and PhAPNC, respectively, were prepared using an eco-friendly, inexpensive and facile solid-state synthetic route. These materials were extensively characterized by CHNSP/O, XRD, FTIR, SEM-EDX, TEM, and PZC. Lanthanum sorption characteristics were investigated and compared through the study of pH dependence (optimal pH: 4.5), equilibration time (achieved at 120 and 90 min for α-APs and nanocomposites, respectively), and sorption isotherms. The Sips isotherm and pseudo-second-order (PSORE) kinetics were the optimal models for fitting the experimental data. Sorption isotherms showed that methyl-derivatives (≈1.29–1.359 mmol/g) were more effective than their corresponding phenyl-derivatives (≈0.941–0.986 mmol/g) due to steric hindrance, acid-base differences, and inductive effects. Sorbents showed appreciated stability with just a 4.5–10.5 % loss in performance over six reuse cycles using HCl (0.2 M). Notably, sand incorporation slightly increased capacity with half-organic-portion in composites, as well as enhanced kinetics and regeneration efficiency. La(III) sorption is spontaneous, exothermic, and increases randomness across all sorbents. Finally, the prepared sorbents have proven effective sorption for Nd(III) beside La(III) with high selectivity from acidic complex monazite liquor.

CAS / MDL: 75-05-8 623-27-8
研究领域: 材料科学 · 环境科学 · 化学工程
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Polymer Chemistry · 2013 ·Vol. 5 ·期 6 ·1857-1862 · IF 5.231

‘One pot’ synthesis of well-defined poly(aminophosphonate)s: time for the Kabachnik–Fields reaction on the stage of polymer chemistry

Yaling Zhang,Yuan Zhao,Bin Yang,Chongyu Zhu,Yen Wei,Lei Tao

A multicomponent reaction (MCR) has been carried out on the platform of controlled radical polymerization (CRP) to construct a ‘one pot’ MCR-CRP system for the facile preparation of well-defined functional polymers. In the current work, a novel ‘one pot’ system has been built through a combination of the Kabachnik–Fields (KF) reaction and reversible addition fragmentation chain transfer (RAFT) polymerization. Compared to a traditional stepwise method and polymer post-polymerization modification, this novel ‘one pot’ system exhibited distinct advantages to much more facilely and efficiently prepared well-defined poly(aminophosphonate)s (polyAPPs). A series of unique polyAPPs have also been successfully prepared through this KF–RAFT system, suggesting this novel method is a general and versatile approach to prepare well-defined organophosphorous polymers.

研究领域: 高分子化学 · 材料科学
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ACS Applied Engineering Materials · 2022 · IF 0

2D@0D Multidimensional Nanoparticles for Improving the Fire Safety of Epoxy Resin

Xiao-Lu Pu,Xi Luo,Jia-Hui Chen,Shao-Dong Xu,Song Gu,Yu-Zhong Wang,Li Chen

2D@0D multidimensional nanoparticles (WC@TDP) were first prepared by decorating WS2 2D nanosheets (WC) with titanium diphenylphosphonate (TDP) 0D nanoparticles, which were derived from the hybridization of diphenylphosphinic acid and TiO2. The chemical structure and micromorphology of the modified 2D nanosheet were confirmed, and TDP nanoparticles were tightly attached to the exfoliated WC nanosheets through noncovalent interactions. Afterward, WC@TDP was incorporated into the epoxy resin (EP), showing the improved dispersion and distribution in the thermosetting matrix. Because TDP exhibits catalytic charring activity and WC acts as a physical barrier, such EP/WC@TDP nanocomposites exhibited the enhanced fire safety, including flame retardation and smoke suppression during burning. The composite containing 8 wt % WC@TDP passed UL94 V-0 rating with a limiting oxygen index increased from 26.0 to 34.0 vol %. Compared with those of neat EP, the peak heat release rate, total heat release rate, and total smoke release of EP/8WC@TDP were reduced by 42%, 17%, and 38%, respectively, without sacrificing the mechanical properties of the nanocomposites.

研究领域: 材料科学 · 化学工程 · 高分子化学 · 火灾防护
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RSC Advances · 2025 ·Vol. 15 ·期 7 ·5042-5059 · IF 4.6

Simultaneous adsorption of sulfamethoxazole and neodymium from wastewater by a MXene-, α-aminophosphonate-, and sulfated fucan-based ternary composite based on anion-synergistic interactions

Irfan Ijaz,Aysha Bukhari,Ammara Nazir,Ezaz Gilani,Hina Zain,Attia Shaheen,Mohammed Rafi Shaik,Mujeeb Khan,Jilani P. Shaik

The simultaneous removal of antibiotics and heavy metal ions is of utmost importance because of their hazardous effects on the environment and humans. For the adsorption of sulfamethoxazole (SMX) and neodymium (Nd3+) in mono- and binary contaminant systems (SMX–Nd3+ and Nd3+–SMX), a novel composite was designed using sulfated fucan (FuS), MXenes, and α-aminophosphonates (AMPs) in this study. As far as we know, the concurrent adsorption of SMX and Nd3+ employing materials made of MXenes, FuS, and AMPs with this specific structure has not yet been reported. At 318 K, the FuS@MXene@AMP adsorbent demonstrated excellent adsorption capacities of 448.91 and 255.78 mg g−1 for SMX and Nd3+, respectively. The pseudo-first-order (PSO) kinetic model was the most appropriate for depicting the adsorption of SMX and Nd3+ among all the tested kinetic models. The adsorption of SMX and Nd3+ is better described by the Langmuir isotherm model with a higher value of adsorption capacity and R2. The simultaneous presence of Nd3+ and SMX promoted mutual sorption between the antibiotic and metal ions in the binary systems. The results of FTIR and XPS studies indicated that the removal mechanisms were primarily due to hydrogen bonding, complexation, electrostatic interaction, and π–π interaction.

研究领域: 环境科学 · 材料科学
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FLUID PHASE EQUILIBRIA · 2015 · IF 2.2

Solid–liquid equilibrium of diphenyl anilinophosphonate in the different organic solvents

Guo-Min Yu,Li-Sheng Wang,Lin-Kun Jiang,Jian Sun

A phosphorus flame retardant named diphenyl anilinophosphonate (DPAP) was synthesized using diphenyl chlorophosphate and aniline. Its structural features and purity were investigated by mass spectrometry (MS), infrared spectroscopy (IR), nuclear magnetic resonance (NMR) spectroscopy, and high-performance liquid chromatography (HPLC). The thermal properties of DPAP were evaluated using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). A static-analytic method was used to measure the solubilities of DPAP in acetonitrile, methanol, chloroform, ethanol, acetone, toluene, i -propanol, n -propanol, methyl acetate, ethyl acetate, 1,2-dichloroethane, and tetrahydrofuran from 293.15 to 333.15   K. Several thermodynamic models were used to correlate the experimental solubility data, such as the van’t Hoff equation, Buchowski–Ksiazczak ( λh ), Scatchard–Hildebrand, Wilson, nonrandom two-liquid (NRTL), and UNIQUAC. The calculated results showed that these models can reproduce the experimental data well, and that the NRTL equation gives the best correlation. The activity coefficients and solubility parameters of the solute were calculated using the Scatchard–Hildebrand methodology.

CAS / MDL: 62-53-3 121-44-8
研究领域: 化学 · 材料科学
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SENSORS AND ACTUATORS B-CHEMICAL · 2021 · IF 7.46

Hydrogen bonds-induced room-temperature detection of DMMP based on polypyrrole-reduced graphene oxide hybrids

Zhimin Yang,Yaqing Zhang,Shang Gao,Liang Zhao,Teng Fei,Sen Liu,Tong Zhang

The development of fast-response, high sensitivity and selectivity gas sensors for monitoring of organophosphorus is essential, where two dimensional graphene-based materials possessing exceptionsal carrier mobility are considered as promising candidates for room-temperature organophosphorus detection. However, it is challenging to fabrication of graphene-based gas sensors for detection of organophosphorus with excellent sensing performances. Herein, we develope a self-redox strategy to synthesize polypyrrole decorated-reduced graphene oxide hybrids (PPy-rGO) by redox reactions between pyrrole and GO during hydrothermal treatment process. This self-redox strategy results in the formation of perfact interfical strucutre between PPy and rGO through the π-π interactions without the impurity from the conventional oxidation/reducing agents. Most importantly, such PPy-rGO hybrids can be used as novel sensing materials for detection of dimethyl methylphosphonate (DMMP) at room temperature. Specially, the response of PPy-rGO-based sensor towards 100 ppm DMMP can reach 12.9 %, which is 3-fold higher than that pristine rGO-based sensor. Meanwhile, PPy-rGO-based sensor exhibits short response time/recovery time (43 s/75 s), low detection limit (5 ppm), excellent repeatability, and high selectivity. By combination of FT-IR and N 2 sorption isotherms, the enhanced DMMP sensing performances of PPy-rGO hybrids are concluded as following two aspects. Firstly, the formation of hydrogen bonds between PPy-rGO hybrids and DMMP molecules regulates the adsorption/desorption of DMMP. Secondly, increasing BET surface area by introduction of PPy into rGO matrix is beneficial to DMMP diffusion among the sensing materials. Our work would offer a new strategy for rational development of graphene-based materials for detection of organophosphorus at room temperature.

研究领域: 材料科学 · 化学传感器 · 环境监测
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POLYMERS FOR ADVANCED TECHNOLOGIES · 2019 ·Vol. 30 ·期 5 ·1269-1278 · IF 2.162

Microfluidic fabrication of polysiloxane/dimethyl methylphosphonate flame-retardant microcapsule and its application in silicone foams

Fu-Ru Kang,Jun Deng,Dong-Sheng Jiao,Li-Qun He,Wei-Feng Wang,Zhi-Chao Liu

A novel and versatile route for fabricating flame-retardant microcapsules via microfluidics technology is reported. The flame-retardant microcapsules were prepared with a dimethyl methylphosphonate (DMMP) core and an ultraviolet-curable (UV-curable) polysiloxane shell. Furthermore, a UV-curable polysiloxane was synthesized. The synthesis mechanism of UV-curable polysiloxane and the curing mechanism of flame-retardant microcapsules were analyzed. To verify that DMMP was encapsulated in the microcapsules, X-ray fluorescence was used before and after microencapsulation. The resulting microcapsules were well monodispersed and exhibited a good spherical shape with a smooth surface. In addition, the size of the microcapsules decreased dramatically with an increasing flow-rate ratio of the middle-/inner-phase or outer-phase flow rate. The thermal stability of the microcapsules was worse than shell materials but superior to DMMP. Silicone foams (SiFs) with microcapsules prepared using a dehydrogenation method achieved a relatively higher limiting oxygen-index value than the pure SiF, which indicated that the microcapsules could enhance the flame retardation of SiFs effectively. Because of the polysiloxane shell, the microcapsules had good compatibility with SiFs, and the influence of microcapsules on the mechanical properties of SiFs was unremarkable.

研究领域: 材料科学 · 化学工程
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