Jove-Journal of Visualized Experiments
·
2017
·
IF 1.232
Junlian Wang,Meiying Xie,Xinyu Liu,Shengming Xu
We present the synthesis of (2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic acid as an example to demonstrate a method for the synthesis of high purity nonsymmetric dialkylphosphinic acid extractants. Low toxic sodium hypophosphite was chosen as the phosphorus source to react with olefin A (2,3-dimethyl-1-butene) to generate a monoalkylphosphinic acid intermediate. Amantadine was adopted to remove the dialkylphosphinic acid byproduct, as only the monoalkylphosphinic acid can react with amantadine to form an amantadine∙mono-alkylphosphinic acid salt, while the dialkylphosphinic acid cannot react with amantadine due to its large steric hindrance. The purified monoalkylphosphinic acid was then reacted with olefin B (diisobutylene) to yield nonsymmetric dialkylphosphinic acid (NSDAPA). The unreacted monoalkylphosphinic acid can be easily removed by a simple base-acid post-treatment and other organic impurities can be separated out through the precipitation of the cobalt salt. The structure of the (2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic acid was confirmed by 31P NMR, 1H NMR, ESI-MS, and FT-IR. The purity was determined by a potentiometric titration method, and the results indicate that the purity can exceed 96%.
研究领域:
有机化学
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分析化学
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DOI
PubMed
高影响因子
JOURNAL OF THE BRAZILIAN CHEMICAL SOCIETY
·
2023
·Vol. 34
·期 7
·1003-1012
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IF 1.4
Wang Junlian,Liu Hui,Xu Wen,Chang Ziyong,Wang Peilong,Wang Huajun
Designing highly efficient dialkylphosphinic acid extractant for zirconium/hafnium separation relies on systematic structure-property studies. In this paper, dialkylphosphinic acids with different substituents at β-C, γ-C and δ-C for zirconium and hafnium extraction and separation from H2SO4 media were investigated. The results show that substituents at β-C, γ-C and δ-C reduce the extraction ability of dialkylphosphinic acids for both zirconium and hafnium. The substituent effect at β-C is greater than that at γ-C and δ-C. The larger steric hindrance of the substituents (ethyl > methyl > H), the weaker extraction ability of the dialkylphosphinic acids. The zirconium and hafnium separation behavior is related to the extraction ability of dialkylphosphinic acids. Dialkylphosphinic acids with stronger extraction ability show better zirconium/hafnium separation performance at higher acidity of 2.0 mol L-1 H2SO4, while those with weaker extraction ability show better zirconium and hafnium separation performance at lower acidity of 0.25 mol L-1 H2SO4. The highest hafnium/zirconium separation factor (βHf/Zr) in the current study occurs with (2-ethylhexyl)(2,4,4-trimethylpentyl)phosphinic acid (USTB-1), which reaches 19.2.
研究领域:
化学工程
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材料科学
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DOI
高影响因子
JOURNAL OF RARE EARTHS
·
2022
·
IF 4.632
Junlian Wang,Guodong Xu,Wen Xu,Jianguo Cui,Yufu Chen,Ziyong Chang
The relationship between dialkylphosphinic acid structure and their loading capacity for HREEs and emulsification phenomena has rarely been studied. In this paper, we took Lu extraction as an example to study the effect of β , γ , δ -substituents of dialkylphosphinic acids on their loading capacity and anti-emulsification performance for HREEs. To discuss conveniently, the dialkylphosphinic acids were classified into two groups: β -substituent group (P208, INET-1, P218, USTB-1 and P227) and γ , δ -substituent group (P218, P2132 and Cyanex 272). For β -substituent group extractants, their loading capacities are in the order P208 (299.7 mg/L) ≈ INET-1 (299.5 mg/L) > P218 (270.8 mg/L) >> USTB-1 (163.1 mg/L) > P227 (151.4 mg/L), while their anti-emulsification/gelation performances are just in the opposite order P227 > USTB-1 > P218 > P208 ≈ INET-1 under the studied conditions. For γ , δ -substituent group extractants, their loading capacities are in the order P218 (270.8 mg/L) > P2132 (192.3 mg/L) > Cyanex 272 (131.7 mg/L), while the anti-emulsification performance of P218 is better than those of P2132 and Cyanex 272. The loading capacity data given in the parentheses are obtained through repeatedly extracting Lu from ∼4 × 10 −4 mol/L of Lu aqueous feed solution with initial pH of 2.40 by 0.01 mol/L extractant at phase ratio A/O of 1:1.
研究领域:
化学工程
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材料科学
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DOI
高影响因子
JOURNAL OF THE ELECTROCHEMICAL SOCIETY
·
2021
·Vol. 168
·期 11
·116503
·
IF 4.316
Jiajie Zhou,Senhui Huang,Zhiqiao He,Shuang Song
A novel Ti/Sn-SbOx/PbO2-ODP electrode was constructed using a β-PbO2 layer modified with octadecyl phosphonic acid (ODP) through a co-electrodeposition method. Scanning electron microscopy with an energy dispersive spectrometer, X-ray diffraction and contact angle goniometry confirmed that ODP was successfully embedded into the β-PbO2 layer of Ti/Sn-SbOx/PbO2-ODP, increasing the water contact angle at the electrode surface from 75.9° to 133.9°. The Ti/Sn-SbOx/PbO2-ODP electrode exhibited excellent electrocatalytic oxidation of ciprofloxacin (CIP). The pseudo first-order rate constant for CIP removal was 3.92 h−1 at an electrolytic potential of 10 V, 2.6 times greater than that when using the unmodified electrode. Moreover, electrode stability was greatly improved after ODP modification. The Ti/Sn-SbOx/PbO2-ODP electrode had longer accelerated life (324 h) than the Ti/Sn-SbOx/PbO2 electrode (91 h). The enhanced electrocatalytic performance of Ti/Sn-SbOx/PbO2-ODP was attributed to improved utilization of hydroxyl radicals (•OH) resulting from higher oxygen evolution potential. Furthermore, the hydrophobic surface of Ti/Sn-SbOx/PbO2-ODP was beneficial for stronger adsorption of CIP, as evidenced by the initial surface concentration test.
研究领域:
材料科学
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环境工程
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电化学
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DOI
高影响因子
JOURNAL OF RARE EARTHS
·
2020
·
IF 3.104
Zhengyu Liu,Jiaming Wu,Xinyu Liu,Wen Wang,Ziwei Li,Ruijing Xu,Yue Ding,Junlian Wang
Rare earths (REs) and Co are critical strategic resources. Their recovery is crucial for ensuring that their supplies are adequate and for reducing environmental pollution. End-of-life NdFeB magnets are important secondary RE sources. The separation of Dy, Nd, and Co from NdFeB leachate using a relatively new extractant (2,3-dimethylbutyl) (2,4,4′-trimethylpentyl)phosphinic acid (INET-3), was investigated in this study. The separation parameters, such as equilibrium pH, phase ratio, INET-3 concentration, and number of counter-current extraction stages, were optimised. The results show that INET-3 can separate Dy, Nd, and Co efficiently. For the preferential extraction of Dy from synthetic iron-free NdFeB leachate, the optimum equilibrium pH is 2.60. Under this condition, separation of Dy from the leachate requires four counter-current extraction stages at A/O (volume ratio of aqueous to organic) = 1:2. This is demonstrated by a simulated four-stage counter-current extraction process. At equilibrium pH = 2.52 and A/O = 1:2, 98% of Dy is recovered with 95% purity. As to the subsequent separation of Nd from the leachate, nearly 100% is recovered with 99% purity through a simulated three-stage counter-current extraction process at equilibrium pH = 5.33 and A/O = 1:1. Approximately 95% of Co remains in the raffinate with 99.98% purity.
研究领域:
资源回收
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化学工程
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环境科学
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DOI
高影响因子
HYDROMETALLURGY
·
2015
·
IF 1.933
Junlian Wang,Guang Chen,Shengming Xu,Linyan Li
The extraction and separation of heavy rare earths is always one of the most challenging unit operations in hydrometallurgy . Research and development of novel efficient extractant is one way to solve this problem. Organophosphinic acid is a good potential extractant. A new method was established for the synthesis of nonsymmetric dialkylphosphinic acid (NSDAPA) (R′R″POOH, R′ ≠ R″), optimized the synthesizing conditions of the key intermediate mono-alkylphosphinic acid and successfully synthesized three novel extractants ( n -octyl)(2,4,4′-trimethylpentyl) phosphinic acid, ( n -octyl)(cyclohexyl)phosphinic acid and (2,3-dimethylbutyl) (2,4,4′-trimethylpentyl)phosphinic acid. The extraction ability of the novel extractants was investigated. The structure–property relationship and the separation performance for heavy rare earth couples Er/Y, Y/Ho, Yb/Tm and Lu/Yb were evaluated.
研究领域:
冶金学
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化学工程
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DOI
高影响因子
Journal of Environmental Sciences
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2021
·
IF 5.565
Jiaqi Shi,Rui Han,Shuangchun Lu,Qingling Liu
A series of highly-hydrophobic MIL-53-Al (MIL = Materials of Institut Lavoisier) frameworks synthesized via decoration of the Al-OH groups by alkyl phosphonic acid were developed as adsorbents for removing acetone from humid gas streams. The newly prepared materials were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), N 2 adsorption-desorption and thermogravimetric analysis (TGA). Their adsorption behaviors toward acetone vapor under dry and wet conditions were studied subsequently. Results showed that alkyl phosphonic acid was successfully grafted into MIL-53-Al skeleton through coordinating interaction with Al 3+ generating MIL-53-Al@C x ( x = 12, 14, 18). The MIL-53-Al@C x exhibited similar crystal structure and thermal stability to parent MIL-53-Al. Furthermore, the modified materials showed significantly enhanced hydrophobicity . The water vapor uptake of MIL-53-Al@C 14 decreased by 72.55% at 75% relative humidity (RH). Dynamic adsorption experiments demonstrated that water vapor had almost no effect on the acetone adsorption performance of MIL-53-Al@C 14 . Under the condition of 90% RH, the acetone adsorption capacity of MIL-53-Al@C 14 was 102.98% higher than that of MIL-53-Al. Notably, MIL-53-Al@C 14 presented excellent adsorption reversibility and regeneration performance in 10 adsorption-desorption cycles. Taken together, the strategy of metal-OH group modification is an attractive way to improve the acetone adsorption performance over metal-organic frameworks (MOFs) under humid conditions. Besides, MIL-53-Al@C 14 would be deemed as a promising candidate for capturing acetone in high moisture environment.
研究领域:
材料化学
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环境科学
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吸附分离
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多孔材料
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配位化学
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DOI
高影响因子
International Journal of Industrial Chemistry
·
2020
·Vol. 11
·期 2
·133-145
·
IF 0
Mpelwa Musa,Tang Shanfa,Jin Lijun
Mineral scale deposit is one of the major problems incessantly faced in the oil and gas producing wells and surface facilities, and if not well-handled can cause an unsuccessful petroleum production. To eradicate scale deposits, scale inhibitors (SIs) are commonly deployed into industrial water systems. Because of effectiveness and long squeeze lifetimes, organic phosphonate SIs are extensively used for preventing mineral scale formation in industrial water systems. However, they usually exhibit lower Ca 2+ and Mg 2+ tolerances that restrict their applications in harsh conditions where high inhibitory dosages are needed. In this paper, a multifunctional aminoalkylenephosphonate-based antiscalant having higher Ca 2+ and Mg 2+ tolerances is studied. The antiscalant was synthesized, characterized (FTIR and NMR spectroscopies), and evaluated in accordance with the NACE Standard Method (TM0374) for preventing CaSO 4 and CaCO 3 formation in the petroleum industry. The effects of inhibitory dosages, water hardness, temperature, incubation period, and pH were studied. We further tested the performance of the antiscalant in simulated field waters. Experimental results show that the multifunctional aminoalkylenephosphonate-based antiscalant has better inhibitory properties as compared to conventional aminoalkylenephosphonate-based SIs. The incorporation of the sulfonate group into the molecule significantly improved the solubility of the antiscalant and hence its tolerances to Ca 2+ and Mg 2+ ions. Also, it bolstered thermal stability of the inhibitor. The results from simulated field conditions are promising. The synthesized antiscalant performed superbly than the conventionally aminomethylenephosphonate antiscalants where Ca 2+ and Mg 2+ concentrations are challenging.
研究领域:
化学工程
·
石油工程
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DOI
JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Zhihua Song,Shenghong Li,Yafeng Guan,Shuo Wang,Yinghao Wang,Gangqiang Yang,Xiaochen Zhang,Jinhua Li,Wenhao Song,Chuanming Zhou,Lingxin Chen
In this work, multilayer zirconia-coated silica (ZrO 2 /SiO 2 -n) microspheres were successfully produced by a straightforward hydrothermal procedure with a low concentration of Zr 4+ (5 mM) under low potential of hydrogen (pH) conditions (pH = =2). The obtained ZrO 2 /SiO 2 -n materials exhibited favorable characteristics for high-performance liquid chromatography (HPLC) separation, including high surface area and pore volume, good pore structure, narrow particle size, and pore size distribution. In addition, the zirconia coverage in the mesopores was confirmed by soaking the material in 1 M NaOH solution, with the particles showing strong resistance to the basic solution. The obtained ZrO 2 /SiO 2 -n stationary phases were packed into a fused-silica capillary tubing for the separation of alkaloids in hydrophilic interaction chromatography (HILIC) mode, and a column efficiency of 47,800 plates/m was obtained for berberine on a ZrO 2 /SiO 2 -6 micro column. The ZrO 2 /SiO 2 -6 microspheres were further modified by dodecylphosphonic acid (C 12 P-2-ZrO 2 /SiO 2 -6); the C 12 P-2-ZrO 2 /SiO 2 -6 material showed great potential for application in reversed-phase liquid chromatography (RPLC) mode. The C 12 P-2-ZrO 2 /SiO 2 -6 micro column showed a column efficiency of 55,000 plates/m for naphthalene and 51,300 plates/m for benzene.
研究领域:
材料科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Colloid and Interface Science Communications
·
2021
·
IF 4.914
Runzhi Wei,Zheng Liu,Wenchang Wei,Sheng Wang,Yi-ju Lv,Guo-Cheng Han
Two nano metal-organic frameworks (NMOFs), [Cu(2,6-dmy-3,5-pyda) 4 ] n (namely Cu-MOFs) and {[Zn(2,6-dmy-3,5-pyda) 2 (4,4′-bipy) (H 2 O)]•H 2 O} n (namely Zn-MOFs) with the unsaturated metal sites were hydrophobically modified by octadecylphosphonic acid (OPA) to prepare MOFs/OPA hydrophobic composites, which were added as hydrophobic additives to the epoxy (EP) coating to prepare Cu-MOFs/OPA/EP and Zn-MOFs/OPA/EP anticorrosion coating. The corrosion protection behavior of these coatings was examined in 3.5 wt% NaCl solution by using EIS, the capacitive arc of the coating modified with Cu-MOFs/OPA and Zn-MOFs/OPA was larger than EP, and R p increases from 1.283 × 10 7 to 6.111 × 10 8 and 7.415 × 10 8 , respectively. The two anticorrosion coatings showed higher impedance modulus values in low frequency region. All the study results proved that both Cu-MOFs/OPA and Zn-MOFs/OPA composite materials with the EP coating provided a very strong barrier and shielding effect, and have the ability to enhance the anticorrosive performance of the epoxy coating
研究领域:
材料科学
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腐蚀科学
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表面工程
·
化学
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产品关联
DOI
高影响因子
Analytical Methods
·
2018
·Vol. 10
·期 46
·5516-5523
·
IF 2.073
Qing Wang,Jiaxin Lian,Zhongdan Hua,Ying Yang,Ying Li,Xiuwen Hao,Yaxin Cao,Xianqi Zeng
A novel magnetic solid-phase extraction (MSPE) sorbent, magnetic multiwalled carbon nanotube-octadecylphosphonic acid modified zirconia (mMWCNT–ZrO2–C18) composite, was fabricated via a simple solvothermal reduction method to extract polycyclic aromatic hydrocarbons (PAHs) from edible oils, coupling with high performance liquid chromatography analysis. The hydrophobic ZrO2–C18 nanoparticles were introduced to enhance the extraction capability. Factors influencing the extraction efficiency, i.e. the type and volume of desorption solvent, amount of the sorbent, and adsorption and desorption time, were systematically investigated. Under the optimal conditions, calibration curves were linear (R2 > 0.9937) over the concentration range from 0.20 to 200 ng g−1. The limits of detection (S/N = 3) and limits of quantification (S/N = 10) achieved were in the range of 0.06–0.55 and 0.20–1.83 ng g−1, respectively. The intra- and inter-day relative standard deviations were less than 7.21%. A comparative study indicated that higher recoveries were obtained by using mMWCNT–ZrO2–C18 compared to when using bare mMWCNTs. The results indicated that the mMWCNT–ZrO2–C18 nanomaterial was endowed with great adsorption capability and had significant potential in the preconcentration of PAHs from edible oil samples.
研究领域:
分析化学
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环境科学
·
纳米技术
·
食品科学
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产品关联
DOI
高影响因子
HYDROMETALLURGY
·
2023
·
IF 4.7
Xintong Li,Yongna Guo,Xin Ma,Chao Zhang,Jia Yang,Shuai Wang
Herein, a series of α -hydroxyalkyl phosphinic acids were designed and first introduced in Mn 2+ extraction and Mn 2+ -Mg 2+ separation. The extraction tests indicate that the α -hydroxy-2-ethylhexyl phosphinic acid ( α -H-2-EHA) possesses superior extraction ability compared to di-2-ethylhexyl phosphinic acid (P204) for Mn 2+ and Mg 2+ , and the partition coefficient ( β ) is 28.2 at a saponification ratio of 30%. The results of quantum chemical calculation, FT-IR spectrum and slope analysis method reveal that the α -H-2-EHA can form stable four-membered ring structure with metal ions during the extraction process through P–OH and P O bonds. Furthermore, the HOMO composition results suggest that α -OH might also promote the interaction between extractant and metal ions. Finally, a three-stage countercurrent extraction—washing—stripping process was proposed and Mn 2+ can be enriched from 11.2 g/L to 36.6 g/L, with Mg 2+ decreased from 30.3 g/L to 0.6 g/L, which provides an efficient strategy for the preparation of high-purity manganese.
研究领域:
化学工程
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分析化学
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材料科学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）