16940-66-2Relevant articles and documents
A facile solvent-free method for NaBH4 and Na2B12H12 synthesis
He, Liqing,Fu, Yanda,Wu, Dong,Zhang, Dehui,Cheng, Hua,Lin, Huaijun,Li, Xiangnan,Xiong, Wei,Zhu, Qing,Deng, Yonghong,Shao, Huaiyu,Li, Hai-Wen,Zhao, Xingzhong,Lu, Zhouguang
, p. 16 - 21 (2018)
Sodium tetrahydroborate (NaBH4) and dodecahydro-closo-dodecaborate (Na2B12H12) are both important inorganic compounds presenting multiple applications. Nevertheless, multistep and complicated conditions are usually demanded for their synthesis. In order to simplify the synthesis processes, we design a novel and facile solvent-free method for synthesizing NaBH4 or Na2B12H12 from NaNH2 and B10H14. The product of either NaBH4 or Na2B12H12 is manipulable by simply adjusting the ratio of NaNH2 to B10H14. The reaction equations of synthesizing NaBH4 and Na2B12H12 are proposed and verified, and the reaction pathways are elucidated. The findings here supply new insight to synthesize metal dodecaborates using the strategy of equal electron body for the first time and may shed light on synthesis of small metal B-H compounds from large B-H clusters.
Synthesis of NaBH4 based on a solid-state reaction under Ar atmosphere
Zhang, Hanping,Zheng, Shiyou,Fang, Fang,Chen, Guorong,Sang, Ge,Sun, Dalin
, p. 352 - 355 (2009)
Sodium borohydride, NaBH4, was successfully synthesized via solid-state reaction under Ar instead of H2 atmosphere. A 4NaH-NaBO2-2SiO2 ternary mixture was first ball-milled and pressed into pellet, and then calc
Supersilylated tetraphosphene derivatives M2[t-Bu 3SiPPPPSi-t-Bu3] (M = Li, Na, Rb, Cs) and Ba[t-Bu 3SiPPPPSi-t-Bu3]: Reactivity and Cis-trans isomerization
Lorbach, Andreas,Nadj, Andor,Tuellmann, Sandor,Dornhaus, Franz,Schoedel, Frauke,Saenger, Inge,Margraf, Guenter,Bats, Jan W.,Bolte, Michael,Holthausen, Max C.,Wagner, Matthias,Lerner, Hans-Wolfram
, p. 1005 - 1017 (2009)
The tetraphosphenediides M2[t-Bu3SiPPPPSi-t-Bu 3] (M = Li, Na, K) were accessible by the reaction of P4 with the silanides M[Si-t-Bu3] (M = Li, Na, K), whereas M 2[t-Bu3SiPPPPSi-
A simple and efficient way to synthesize unsolvated sodium octahydrotriborate
Huang, Zhenguo,King, Graham,Chen, Xuenian,Hoy, Jason,Yisgedu, Teshome,Lingam, Hima K.,Shore, Sheldon G.,Woodward, Patrick M.,Zhao, Ji-Cheng
, p. 8185 - 8187 (2010)
A simple and efficient way to synthesize unsolvated sodium octahydrotriborate has been developed. This method avoids the use of dangerous starting materials and significantly simplifies the reaction setup, thus enabling convenient large-scale synthesis. The structure of the unsolvated compound has been determined through powder X-ray diffraction.
Structure and properties of NaBH4·2H2O and NaBH4
Filinchuk, Yaroslav,Hagemann, Hans
, p. 3127 - 3133 (2008)
NaBH4·2H2O and NaBH4 were studied by single-crystal Xray diffraction and vibrational spectroscopy. In NaBH 4·2H2O, the BH4- anion has a nearly ideal tetrahedral geometry and is bridged with two Na+ ions through the tetrahedral edges. The structure does not contain classical hydrogen bonds, but reveals strong dihydrogen bonds of 1.77-1.95 A. Crystal structures and vibrational spectra of NaBr·2H2O and NaBH 4·2H2O reveal many similarities. The unit cell volume of NaBH4·2H2O increases linearly with temperature between 200 and 313 K. At 313-315 K, the hydrate decomposes into NaBH4 and H2O, which react to release hydrogen. Wiley-VCH Verlag GmbH & Co. KGaA, 2008.
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Keller,P.C.
, p. 1231 (1969)
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ANIONIC ZIRCONIUM AND HAFNIUM BOROHYDRIDE COMPLEXES
Makhaev, V. D.,Borisov, A. P.,Boiko, G. N.,Tarasov, B. P.
, (1990)
Zirconium and hafnium tetrachlorides react with NaBH4 in dimethoxyethane (DME) to give .These compounds react with Bu4NBH4 and Ph4PBH4 to give (R4E).Bidentate and tridentate BH4(1-) occur in (1-) according to IR spectr
Preparation of sodium borohydride by the reaction of MgH2 with dehydrated borax through ball milling at room temperature
Li,Morigazaki,Liu,Suda
, p. 232 - 236 (2003)
A convenient method was developed to synthesize NaBH4 by the reaction of MgH2 with Na2B4O7 through ball milling at room temperature. In order to improve the sodium borohydride yield, Na compounds were added to compensate the Na insufficiency in reactants when MgH2 instead of NaH was used as the reducing agent. It was found that Na2CO3 addition was better than NaOH or Na2O2 addition in increasing the borohydride yield.
Tris(dithiolene) complexes of neodymium and cerium: Mononuclear species, chains, and honeycomb networks
Roger, Mathieu,Arliguie, Therese,Thuery, Pierre,Fourmigue, Marc,Ephritikhine, Michel
, p. 584 - 593 (2005)
Reactions of Ln(BH4)3(THF)3 (Ln = Nd, Ce) and M2dddt (M = Na, K; dddt = 5,6-dihydro-1,4-dithiine-2,3- dithiolate) in THF or pyridine gave, after addition of 18c6 (18-crown-6), several crystalline compounds which all contain the tris(dithiolene) Ln(dddt)3 unit. Crystals of [Na(18c6)(py)2] 2[Na(18c6)(py)][Nd(dddt)3(py)]·3py (1·3py) are built up from discrete mononuclear cationic and anionic species whereas crystals of {[Na(18c6)(py)2]0.5[Na(18c6)(py) 1.5][Na1.5Nd(dddt)3]}∞ (2) are composed of discrete [Na(18c6)(py)x]+ cations and polymeric anionic two-dimensional layers in which the Nd(dddt)3 units are linked to three neighbors by sodium atoms to form a honeycomb network. Analysis of the temperature dependence of the molar magnetic susceptibility of 2 shows that χMT decreases from 1.63 cm3 K mol -1 at 300 K down to 0.6 cm3 K mol-1 at 5 K, due to the crystal-field splitting of the 4I9/2 free-ion state. Complexes {[Na3(18c6)1.5Nd(dddt) 3(THF)]·3THF}∞ (3·3THF) and {[K 3(18c6)1.5Nd(dddt)3(py)]·3py} ∞ (4·3py) exhibit neutral polymeric layers with the Nd(dddt)3 units linked by M2(18c6) fragments. In the cerium compound {[Na2(18c6)Na(py)2Ce(dddt) 3(py)]·3py}∞ (5·3py), each Ce(dddt)3 unit is linked to two neighbors only by Na 2(18c6) moieties, giving infinite zigzag chains.
Hough, W. V.,Edwards, L. J.,McElroy, A. D.
, p. 1828 - 1829 (1958)
Sodium borohydride formation when Mg reacts with hydrous sodium borates under hydrogen
Liu, Bin Hong,Li, Zhou Peng,Zhu, Jing Ke
, p. L16-L20 (2009)
In this work, we explored the possibility of NaBH4 synthesis when Mg reacted with hydrous sodium borates under hydrogen. It was found that Mg could react with the water in molten hydrous borates to form MgO and release hydrogen, which can be us
Challenges in the synthetic routes to Mn(BH4)2: Insight into intermediate compounds
Tumanov, Nikolay A.,Safin, Damir A.,Richter, Bo,?odziana, Zbigniew,Jensen, Torben R.,Garcia, Yann,Filinchuk, Yaroslav
, p. 6571 - 6580 (2015)
We have studied the reaction of MnCl2 with MBH4 (M = Li+, Na+, K+) in Et2O. Crystal structures of two new intermediates, named [{M(Et2O)2}Mn2(BH4)5] (M = Li+, Na+), were elucidated by X-ray diffraction. Mn(BH4)2 in a mixture with LiBH4 or NaBH4 forms upon the solvent removal in a vacuum. [{M(Et2O)2}Mn2(BH4)5] contains 2D layers formed by Mn and BH4 groups, linked through the alkali metal atoms coordinated to Et2O. The loss of the solvent molecules leads to the segregation of the partially amorphous or nanocrystalline LiBH4/NaBH4 and a creation of the 3D framework of the crystalline Mn(BH4)2. While using LiBH4 led to Mn(BH4)2 contaminated with LiCl, presumably due to an efficient trapping of the latter salt by the [Mn(BH4)2-Et2O] system, the reaction with NaBH4 produced chlorine-free Mn(BH4)2 accompanied with NaBH4. Using KBH4 led to the formation of K2Mn(BH4)4 as a second phase. Two pyridine-containing solvomorphs, [Mn(py)3(BH4)2] and [Mn(py)4(BH4)2]·2py, were isolated in pure form. However, Mn(BH4)2 partly decomposes upon removal of pyridine molecules. This journal is
Hydroboration Reaction and Mechanism of Carboxylic Acids using NaNH2(BH3)2, a Hydroboration Reagent with Reducing Capability between NaBH4and LiAlH4
Wang, Jin,Ju, Ming-Yue,Wang, Xinghua,Ma, Yan-Na,Wei, Donghui,Chen, Xuenian
supporting information, p. 5305 - 5316 (2021/04/12)
Hydroboration reactions of carboxylic acids using sodium aminodiboranate (NaNH2[BH3]2, NaADBH) to form primary alcohols were systematically investigated, and the reduction mechanism was elucidated experimentally and computationally. The transfer of hydride ions from B atoms to C atoms, the key step in the mechanism, was theoretically illustrated and supported by experimental results. The intermediates of NH2B2H5, PhCH= CHCOOBH2NH2BH3-, PhCH= CHCH2OBO, and the byproducts of BH4-, NH2BH2, and NH2BH3- were identified and characterized by 11B and 1H NMR. The reducing capacity of NaADBH was found between that of NaBH4 and LiAlH4. We have thus found that NaADBH is a promising reducing agent for hydroboration because of its stability and easy handling. These reactions exhibit excellent yields and good selectivity, therefore providing alternative synthetic approaches for the conversion of carboxylic acids to primary alcohols with a wide range of functional group tolerance.
Realizing facile regeneration of spent NaBH4 with Mg-Al alloy
Zhong, Hao,Ouyang, Liuzhang,Zeng, Meiqin,Liu, Jiangwen,Wang, Hui,Shao, Huaiyu,Felderhoff, Michael,Zhu, Min
supporting information, p. 10723 - 10728 (2019/05/06)
The regeneration of sodium borohydride (NaBH4) is crucial to form a closed cycle after it either supplies hydrogen energy via a hydrolysis process or provides energy through electron transfer at the anode of direct borohydride fuel cells (DBFCs). In both of these cases, the spent fuels are NaB(OH)4 from NaBO2 aqueous solution. However, the current regeneration process from (NaB(OH)4)·xH2O to form NaBH4 by reduction reaction and calcination at high temperature with metal hydrides as reducing agents is very expensive. In this work, we developed a simple regeneration process via ball milling with Mg-Al alloys as the reducing agent for NaB(OH)4 under an argon atmosphere. Under optimized conditions, a high yield of about 72% of NaBH4 could be obtained. Mechanistic study showed that all the hydrogen atoms from NaB(OH)4 remain in NaBH4 and no additional hydrogen sources are needed for the reduction process. The inexpensive Mg-Al alloy works as a reducing agent transforming the H+ to H- in NaBH4. This approach demonstrates a ~20-fold cost reduction compared with the method using metal hydrides. This opens the door to the commercial implementation of simple ball milling processes for the regeneration of spent NaBH4 from NaB(OH)4 with cheap reducing agents.