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Osmium double-teeth diamine complex with effect of catalyzing dehydrogenation activity of ammonia borane and preparation method thereof

A technology for catalyzing ammonia borane and bidentate diamine, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, organic chemistry, etc. Difficulties and other problems, to achieve the effect of mild reaction conditions, low energy consumption, and simple steps

Inactive Publication Date: 2018-11-09
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, although ammonia borane has various advantages as a potential hydrogen storage material, there are still problems such as high hydrogen release temperature during the hydrogen release process, the generation of impurity gases, volume expansion, and difficult regeneration during the hydrogen release process.

Method used

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  • Osmium double-teeth diamine complex with effect of catalyzing dehydrogenation activity of ammonia borane and preparation method thereof
  • Osmium double-teeth diamine complex with effect of catalyzing dehydrogenation activity of ammonia borane and preparation method thereof
  • Osmium double-teeth diamine complex with effect of catalyzing dehydrogenation activity of ammonia borane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh o-phenylenediamine (22mg, 0.20mmol) and OsCl 2 (PPh 3 ) 3 (178mg, 0.17mmol) into 25mL reaction bottle with magnetic sub, under N 2 Under protection, 15 mL of dichloromethane solvent was added, and the reaction was stirred at 20-25° C. for 2 h, and the solution changed from dark green to brown-red. After the reaction was completed, the reaction solution was concentrated, and 20 mL of anhydrous n-hexane was added to form a light yellow precipitate, which was the crude product of o-phenylenediamine-substituted osmium nitrogen complex. The crude product was washed with n-hexane (4 times, 40 mL), filtered and dried to obtain the purified osmium nitrogen complex light yellow solid with a yield of 136 mg and a yield of 90%.

[0026] The results of NMR analysis were 1 H NMR (600MHz, CDCl 3 )δ: 7.4 (broad s, 12H, PPh 3 ), 7.2(t, J=7.2Hz, 6H, PPh 3 ), 7.1(t, J=7.2Hz, 12H, PPh 3 ),7.0(broad s,2H,Ar),6.8(broad s,2H,Ar),5.0(broad s,4H,NH 2 ). 13 C{ 1 H}NMR (151MHz, C...

Embodiment 2

[0029] Weigh 3-methyl-o-phenylenediamine (24mg, 0.20mmol) and OsCl 2 (PPh 3 ) 3 (178mg, 0.17mmol) into 25mL reaction bottle with magnetic sub, under N 2 Under protection, 15 mL of dichloromethane solvent was added, and the reaction was stirred at 20-25° C. for 2 h, and the solution changed from dark green to brown-red. After the reaction was completed, the reaction solution was concentrated, and 20 mL of anhydrous n-hexane was added to form a yellow precipitate, which was the crude product of 3-methyl-o-phenylenediamine substituted osmium nitrogen complex. The crude product was washed with n-hexane (4 times, 40 mL), filtered and dried to obtain the purified osmium nitrogen complex yellow solid, with a yield of 133 mg and a yield of 86%.

[0030] The results of NMR analysis were 1 H NMR (600MHz, CDCl 3 )δ:7.5(q,J=8.8Hz,12H,PPh 3 ), 7.2(t, J=4.4Hz, 6H, PPh 3 ), 7.1(t, J=7.5Hz, 12H, PPh 3 ),6.9(t,J=7.5Hz,1H,Ar),6.8(d,J=3.6Hz,1H,Ar),6.6(d,J=4.5Hz,1H,Ar),5.0(broad s,2H ,NH...

Embodiment 3

[0033] Weigh 3-bromo-o-phenylenediamine (38mg, 0.2mmol) and OsCl 2 (PPh 3 ) 3 (178mg, 0.17mmol) into 25mL reaction bottle with magnetic sub, under N 2 Under protection, 15 mL of dichloromethane solvent was added, and the reaction was stirred at 20-25° C. for 2 h, and the solution changed from dark green to brown-red. After the reaction was completed, the reaction liquid was concentrated, and 20 mL of anhydrous n-hexane was added to form a yellow precipitate, which was the crude product of osmium nitrogen complex substituted by 3-bromo-o-phenylenediamine. The crude product was washed with n-hexane (4 times, 40 mL), filtered and dried to obtain the purified osmium nitrogen complex yellow solid, with a yield of 129 mg and a yield of 78%.

[0034] The results of NMR analysis were 1 H NMR (600MHz, CDCl 3 )δ:7.4(broad s,12H,PPh 3 ),7.3(broad s,1H,Ar),7.2(broad s,PPh 3 ), 7.1 (broad s, 12H, PPh 3 ), 6.9(t, J=6.3Hz, 1H, Ar), 6.8(d, J=7.2Hz, 1H, Ar), 5.1(broad s, 2H, NH 2 ), 4...

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Abstract

The invention discloses an osmium double-teeth diamine complex with the effect of catalyzing the dehydrogenation activity of ammonia borane and a preparation method thereof, and belongs to the technical field of inorganic synthesis and catalysis. The preparation method comprises the following step that a series of osmium-nitrogen complexes can be generated by room-temperature reaction of OsCl2(PPh3)3 and o-phenylenediamine double-teeth diamine active ligand in an organic solvent. The preparation method has the beneficial effects of mild condition, simple product separation and high yield. Whenbeing applied to catalysis of dehydrogenation reaction of ammonia borane, the osmium double-teeth diamine complex has high-efficiency catalytic reaction activity.

Description

technical field [0001] The invention relates to an osmium bidentate diamine complex with catalytic ammonia borane dehydrogenation activity and a preparation method thereof, belonging to the technical field of inorganic synthesis and catalysis. Background technique [0002] In recent years, with the increasing energy and environmental problems, it is imminent to develop a sustainable and clean energy system to replace the existing energy carrier. Hydrogen energy has become the preferred new energy due to its many advantages such as large reserves, wide distribution, high combustion value, and zero pollution to the environment. However, safe and efficient hydrogen storage and transportation methods are the key to the large-scale application of hydrogen energy. Chemical hydrogen storage has the advantages of high hydrogen storage density and good safety, and has received extensive attention in recent years. Among them, ammonia borane (NH 3 BH 3 , AB) has become the most pot...

Claims

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Application Information

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IPC IPC(8): C07F15/00C01B3/02B01J31/18B01J31/24
CPCB01J31/1815B01J31/2404B01J2531/825C01B3/02C07F15/0026
Inventor 赵茜怡梁媛窦婷张絜陈学年
Owner HENAN NORMAL UNIV
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