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Advanced preparation method of organic-transition metal hydride used as hydrogen storage materials

一种过渡金属、氢化物的技术，应用在钛有机化合物、有机化学、周期表第5/15族元素的化合物等方向，能够解决难以稳定分离、难分离、难分离和提纯等问题

Inactive Publication Date: 2009-09-09
HANWHA CHEMICAL CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Third, as a problem related to the separation and purification of the products, since the products are basically mixed with the catalyst, it is difficult to separate them from each other
However, since 2-alkanols having the above-mentioned characteristics contain too many hydrocarbon chains, various reaction by-products are produced, and thus there is a problem that it is difficult to further separate and purify them
[0013] Therefore, a typical hydrodehalogenation reaction using a hydrogen donor and a catalyst has limitations in that it is difficult to stably separate an organic-transition metal hydride complex and the product yield is low due to the above-mentioned problems.

Method used

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  • Advanced preparation method of organic-transition metal hydride used as hydrogen storage materials
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  • Advanced preparation method of organic-transition metal hydride used as hydrogen storage materials

Examples

Experimental program
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Effect test

preparation example 1

[0072] MAH Method I: Hydrodehalogenation Reaction

[0073] Under argon flow, 0.4 g (1.6 mmol) of phenoxytitanium trichloride (reactant II) was dissolved using 30 ml of toluene in a 100 ml two-neck round bottom flask container. Dissolve 0.184 g (4.85 mmol) of LiAlH in 70 ml of toluene in a 250 ml single necked round bottom flask vessel under argon flow 4(Reactant I). After reflux at 25° C. for 36 hours while slowly dropping reactant II into reactant I, the reaction was completed. The solvent was removed under an argon atmosphere by the Schlenk method, and only the phenoxytitanium aluminum hydride complexes (multiple target compounds A) were selectively extracted using 2-propanol as products (synthetic state (as -synthesis) Substance A). Next, 2-propanol was removed by the Schlenk method, whereby phenoxytitanium hydride (a target compound A) was obtained in a yield of 95%.

[0074] 1 H-NMR (CD 3 CN-d 3 )δ(ppm): 7.28(d, 1H), 6.95(t, 2H), 6.85(t, 2H), 7.62(s, 1H), 4.83(s, 1...

preparation example 2

[0078] MAH Method II: Hydrodehalogenation Reaction

[0079] Take the method similar to Preparation Example 1, the difference is to use 0.262g (4.85mmol) NaAlH 4 Instead of LiAlH used in Preparation Example 1 4 , obtained the phenoxytitanium aluminum hydride complex (a target compound A) with a yield of 96%.

[0080] 1 H-NMR (CD 3 CN-d3) δ (ppm): 7.28 (d, 1H), 6.95 (t, 2H), 6.85 (t, 2H), 7.60 (s, 1H), 4.81 (s, 1H), 4.24 (s, 1H) , -1.61(s, 1H), -2.29(s, 1H); ESI-MS (positive ion mode), m / z (relative intensity): [parent molecule] +171(9.9), 172(9.4), 173 (100), 174(23), 175(10.1); Anal. Calcd. for parent molecule: C, 41.6; H, 5.8. Measured: C, 41.9; H, 5.5%.

[0081] In order to check the kind of by-products prepared according to MAH method II and the preferred separation phenomenon of target compound A with high selectivity, from the XRD, 35 Cl-NMR and 27 As can be seen from the Al-NMR analysis results, NaCl and Al can be formed as the main by-products. In addition, it c...

Embodiment 1

[0083] LB Method I: Hydrogenation Reaction

[0084] Under argon flow, 0.4 g (2.3 mmol) of the phenoxyaluminum hydride complex (reactant IV) prepared according to Preparation 1 was dissolved in a 100 ml two-necked round-bottomed flask using 30 ml of tetrahydrofuran (THF). Under argon flow, 0.70 g (6.9 mmol) of triethylamine (reactant III) was dissolved in 70 ml of tetrahydrofuran (THF) in a 250 ml single necked round bottom flask vessel. After slowly dropping reactant IV into reactant III under reflux at 25° C. for 12 hours, the reaction was completed. The solvent was removed by the Schlenk method under an argon atmosphere, and only phenoxytitanium hydride (a target compound B) was selectively extracted from the as-synthesized substance B using 2-propanol. Next, 2-propanol was removed by the Schlenk method, whereby phenoxytitanium aluminum hydride complexes (various target compounds B) were obtained in a yield of 98%.

[0085] 1 H-NMR (CD 3 CN-d3) δ (ppm): 7.28 (d, 1H), 6.9...

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Abstract

The present invention relates to an advanced preparation method of organic-transition metal hydride used as hydrogen storage materials, the method including: preparing organic-transition metal-aluminum hydride complexes by reacting the organic-transition metal halide with metal aluminum hydride compounds; and preparing the organic-transition metal hydride by reacting the organic-transition metal aluminum hydride complexes with Lewis bases. Since the preparation method of the organic-transition metal hydride according to the present invention does not use catalysts, it has advantages that it does not cause problems due to poisoning and can prepare the organic-transition metal hydride at high yield under less stringent conditions. The hydrogen storage materials containing the organic-transition metal hydride prepared from the preparation method can safely and reversibly store a large amount of hydrogen.

Description

technical field [0001] The present invention relates to a method for producing an organic-transition metal hydride as a hydrogen storage material for absorbing and storing hydrogen and a hydrogen storage material containing the organic-transition metal hydride produced by the method. Background technique [0002] Examples of different hydrogen storage materials proposed by various research groups may include metal hydrides, chemical hydrides (including NaBH 4 、KBH 4 、LiBH 4 etc.), metal-organic framework (MOF), nanostructured materials (GNT, GNF, etc.), polymer-metal complexes, etc. However, these hydrogen storage materials have problems in that 1) their hydrogen storage capacity is smaller than the minimum hydrogen storage capacity reference value (6% by weight) required by the U.S. Department of Energy (DOE) for practical use of hydrogen storage materials, 2 ) reproducible degradation of hydrogen storage, 3) hydrogen adsorption and desorption conditions are very strict,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06C07F7/28B01J20/22
CPCC01B3/001C01B3/0015C07F5/069Y02E60/328Y02E60/327C01B3/0026Y02E60/32C01B3/00C07F7/28C07F9/00
Inventor 金钟植朴济城全孝镇尹熙复金东昱安贵龙金东钰任志淳车文铉
Owner HANWHA CHEMICAL CORPORATION
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