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Mn4CaO4 core structure-containing water cracking catalyst and preparation method and application thereof

A heteronuclear, compound technology, applied in the field of biomimetic water splitting catalysts, can solve problems such as successful case reports

Active Publication Date: 2015-07-08
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, how to chemically synthesize and prepare a catalytic center similar to biological water splitting is an important scientific frontier, and it is also a very challenging scientific problem, and no successful cases have been reported yet.

Method used

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  • Mn4CaO4 core structure-containing water cracking catalyst and preparation method and application thereof
  • Mn4CaO4 core structure-containing water cracking catalyst and preparation method and application thereof
  • Mn4CaO4 core structure-containing water cracking catalyst and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Embodiment 1: compound 1 [Mn 4 CaO 4 ](C 5 h 9 o 2 ) 8 (C 5 h 9 o 2 h) 2 (C 5 h 5 N)

[0071] The preparation method is as follows:

[0072] The first step is the synthesis of compound 1 precursor: in the round bottom flask of 100ml, add tetrabutylamine permanganate (Bu n 4 NMnO 4 , 4mmol), manganese acetate (Mn(CH 3 CO 2 ) 2 , 1mmol), calcium acetate (Ca(CH 3 CO 2 ) 2 , 1mmol) and pivalic acid ((CH 3 ) 3 CCO 2 H, 40mmol) was continuously reacted in acetonitrile at 80°C for 25min, then stopped the reaction, filtered to remove a small amount of precipitate, and the obtained brown mother liquor was placed at 0°C for 1-2 weeks, and brown crystals were precipitated.

[0073] The second step is recrystallization. The crystals obtained in the first step were collected, dissolved in ethyl acetate, recrystallized by adding 2% pyridine (volume ratio), and brown crystals were precipitated after 1 to 2 weeks, rinsed with cyclohexane, dried in vacuo, and the...

Embodiment 2

[0080] Embodiment 2: compound 2 [Mn 4 CaO 4 ](C 5 h 9 o 2 ) 8 (C 5 h 9 o 2 h) 1 (C 5 h 5 N) 2

[0081] Weigh 0.100 g of compound 1, dissolve it in ethyl acetate, add 1% pyridine, place at room temperature, and after 3 weeks, black crystals are precipitated, rinsed with cyclohexane, dried in vacuo, and the yield is ~ 13% (according to the concentration of Ca ions moles).

[0082] Compound 2, structural formula [Mn 4 CaO 4 (R 1 CO 2 ) 8 ](L 1 )(L 2 )(L 3 ), where R 1 = tert-butyl; L 1 =L 2 = pyridine; L 3 = pivalic acid.

[0083] That is, the structural formula of compound 2 is [Mn 4 CaO 4 ](C 5 h 9 o 2 ) 8 (C 5 h 9 o 2 h) 1 (C 5 h 5 N) 2 . Molecular formula: C 55 h 92 N 2 o 22 CaMn 4 . Elemental analysis theoretical value: C, 47.42; H, 6.66; N, 2.01; experimental value: C, 47.74; H, 6.89; N, 1.69.

[0084] The single crystal of compound 2 is monoclinic, and the space group is P2 1 / c1, the cell parameters are α=90.00°, β=102.70...

Embodiment 3

[0088] Embodiment 3: compound 3 [Mn 4 CaO 4 ](C 5 h 9 o 2 ) 9 (C 5 h 9 o 2 h) 2 (C 9 h 7 N)

[0089] The first step is the synthesis of compound precursor: in the round bottom flask of 100ml, add tetrabutylammonate permanganate (Bu n 4 NMnO 4 , 4mmol), manganese acetate (Mn(CH 3 CO 2 ) 2 , 1mmol), calcium acetate (Ca(CH 3 CO 2 ) 2 , 1mmol) and pivalic acid ((CH 3 ) 3 CCO 2 H, 40mmol) continued to react in acetonitrile at 80°C for 25min, then stopped the reaction, filtered to remove a small amount of precipitate, obtained brown mother liquor was placed at 0°C for 1-2 weeks, and brown crystals were precipitated.

[0090]The second step is recrystallization: collect the crystals obtained in the first step, dissolve them with ethyl acetate, add 1% isoquinoline (volume ratio) for recrystallization, collect black crystals after 1 to 2 weeks, and rinse with cyclohexane , dried in vacuo with ~40% yield (based on moles of Ca ions).

[0091] Compound 3, the struc...

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Abstract

The present invention provides a preparation method and application of a Mn4CaO4 core structure-containing water cracking catalyst, a Mn4CaO4 core structure-containing cluster compound is compounded by cheap metal ions (Mn<2 +> and Ca<2 +> ions), a simple carboxylic ligand and a permanganate, the spatial structure is detected by single crystal X-ray diffraction, and physicochemical properties are characterized by electron spectroscopy, electrochemistry and electron paramagnetic nuclear magnetic resonance technology and the like. The cluster compound can catalyze the water cracking in the presence of an oxidant for release of oxygen, and also can catalyze the water cracking on the electrode surface, and electrons are released to the electrode surface to form a current.

Description

technical field [0001] The invention relates to a novel biomimetic water splitting catalyst. Specifically, the present invention relates to a method containing [Mn 4 CaO 4 ] Water-splitting catalyst with core structure, its preparation method and its application. Such compounds can be used as artificial catalysts to catalyze water splitting. Background technique [0002] Energy crisis and environmental pollution are two key problems restricting the sustainable development of human society. Since solar energy is inexhaustible, inexhaustible, clean and pollution-free; water is one of the most abundant substances on the earth, if solar energy can be used to efficiently and safely crack water, release oxygen, obtain electrons and protons, and then produce Electric energy or hydrogen energy can fundamentally solve the energy crisis and environmental pollution problems faced by human beings. Since water is a thermodynamically very stable chemical substance, a suitable water s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00B01J31/22C01B13/02C25B5/00C25B1/04
CPCC01B13/02C07F19/00C25B1/04C25B5/00B01J31/2239B01J2231/70B01J2531/0205B01J2531/0216B01J2531/22B01J2531/23Y02E60/36B01J31/22B01J2531/72C25B11/091C07F13/005
Inventor 张纯喜陈长辉
Owner INST OF CHEM CHINESE ACAD OF SCI
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