Cryptomelane-type K(2-x)CoyNizMn(8-y-z)O16 nanowire and preparation method thereof

A technology of hidden potassium-manganese type and nanowires, which is applied in the field of molecular sieves, can solve the problems of many miscellaneous items, poor structural stability and controllability, etc., and achieve single phase, strong structural stability and controllability, and crystallinity high effect

Active Publication Date: 2014-05-07
JIANGSU JICUI ANTAI CHUANGMING ADVANCED ENERGY MATERIALS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that in the structure of doped manganese oxide octahedral molecular sieve prepared by hydrothermal method in the prior art, the doping atoms do not replace the position of manganese in the crystal lattice, there are many miscellaneous items, and the structure is stable. and poor controllability, thus providing a hidden potassium manganese type K in the form of a single compound 2-x co y Ni z mn 8-y-z o 16 Nanowire and its preparation method

Method used

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  • Cryptomelane-type K(2-x)CoyNizMn(8-y-z)O16 nanowire and preparation method thereof
  • Cryptomelane-type K(2-x)CoyNizMn(8-y-z)O16 nanowire and preparation method thereof
  • Cryptomelane-type K(2-x)CoyNizMn(8-y-z)O16 nanowire and preparation method thereof

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Embodiment 1

[0036] Cryptopotassium manganese type K described in this embodiment 2-x co y Ni z mn 8-y-z o 16 In the nanowire, z=0, the atomic ratio of K, Co, and Mn is 0.62:2.44:5.56, x=1.38, y=2.44, that is, the molecular formula is K 0.62 co 2.44 mn 5.56 o 16 , which is prepared by the following steps:

[0037] (1) Add 10mmol of potassium permanganate, 18mmol of cobalt nitrate and 12mmol of manganese nitrate into 85ml of water, stir to mix evenly, and obtain a mixed solution;

[0038] (2) Transfer the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene liner of 100ml, seal it and put it in a constant temperature box, and conduct a heating reaction at 220°C and 2Mpa for 24 hours.

[0039] After the reaction, the product was cooled and centrifuged to obtain a yellow-brown solid, which was washed alternately with water and ethanol for 5 times, and vacuum-dried at 70°C for 10 hours to obtain the cryptopotassium manganese type K 0.62 co 2.44 mn 5.5...

Embodiment 2

[0045] Cryptopotassium manganese type K described in this embodiment 2-x co y Ni z mn 8-y-z o 16 In the nanowire, z=0, the atomic ratio of K, Co, and Mn is 0.62:1.2:6.8, x=1.38, y=1.2, that is, the molecular formula is K 0.62 co 1.2 mn 6.8 o 16 , which is prepared by the following steps:

[0046] (1) Add 10mmol of potassium permanganate, 6mmol of cobalt acetate and 24mmol of manganese sulfate into 85ml of water, and stir magnetically for 30min to obtain a mixed solution;

[0047] (2) Transfer the mixed solution into a 100ml polytetrafluoroethylene-carbon fiber composite material reactor, seal the high-pressure reactor, put it into a closed microwave reaction system, turn on the microwave power supply, and rapidly heat the reaction system to within 12 minutes. 150°C, reacted at 150°C and 3Mpa for 10 hours, then took it out, cooled and centrifuged to obtain a yellow-brown solid, washed it alternately with water and ethanol for 3 times, and dried it in vacuum at 120°C for...

Embodiment 3

[0049] Cryptopotassium manganese type K described in this embodiment 2-x co y Ni z mn 8-y-z o 16 In the nanowire, z=0, the atomic ratio of K, Co, and Mn is 0.62:4.8:3.2, x=1.38, y=4.8, that is, the molecular formula is K 0.62 co 4.8 mn 3.2 o 16 , which is prepared by the following steps:

[0050] (1) Add 10mmol of potassium permanganate, 24mmol of cobalt nitrate and 6mmol of manganese nitrate into 85ml of water, and magnetically stir for 30min to obtain a mixed solution;

[0051] (2) Transfer the mixed solution into a 100ml polytetrafluoroethylene-carbon fiber composite material reactor, seal the high-pressure reactor, put it into a closed microwave reaction system, turn on the microwave power supply, and rapidly heat the reaction system to within 12 minutes. 220°C, reacted at 220°C and 2.5Mpa for 15 hours, then took it out, cooled and centrifuged to obtain a yellow-brown solid, washed it alternately with water and ethanol for 3 times, and dried it in vacuum at 90°C fo...

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Abstract

The invention relates to a cryptomelane-type K(2-x)CoyNizMn(8-y-z)O16 nanowire, which is prepared by the following steps: mixing and dissolving potassium permanganate, a soluble bivalent cobalt salt and/or soluble bivalent nickel salt into water according to a proper molar ratio to obtain a mixed solution; carrying out heating reaction inside a sealed container under the conditions that the temperature is 150-220 DG C and the pressure is 2-3MPa for 10-24 hours. The data display that the cryptomelane-type K(2-x)CoyNizMn(8-y-z)O16 nanowire is a single compound, and belongs to a tetragonal system. In the cryptomelane-type K(2-x)CoyNizMn(8-y-z)O16 nanowire disclosed by the invention, the structure is stabilized after lattice positions of a part of manganese ions are substituted by cobalt ions and/or nickel ions. Meanwhile, the physical and chemical properties such as catalytic activity, gas adsorption property and the like are improved by the synergistic effects of a few of elements of cobalt, nickel and manganese. Thus, the application prospects of the nanowire in the fields such as catalysis, sensing, a lithium ion battery, a solid fuel battery and the like are expanded.

Description

technical field [0001] The present invention relates to a kind of hidden potassium manganese type K 2-x co y Ni z mn 8-y-z o 16 Nanowires and a preparation method thereof belong to the technical field of molecular sieves. Background technique [0002] Manganese oxide octahedral molecular sieve (OMS-2) has high porosity and a variety of pore structures. It is a new type of microporous material similar to zeolite. Its crystal structure has 2x2 shared sides of octahedral MnO 6 The chains are connected by the oxygen atoms at the vertices of the octahedron to form a one-dimensional channel with a size of about 0.46nm×0.46nm. Due to the presence of manganese ions in various valence states (Mn 2+ , Mn 3+ , Mn 4+ ), and a large number of open interlayer and pore structures, so it shows good redox activity, and also has mild surface acidity and alkalinity and excellent ion exchange performance, so OMS-2 can be widely used in separation, gas transmission sensor, energy storage...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/62C30B29/22C30B7/10C01G53/00B82Y30/00B82Y40/00
Inventor 闫东伟武英况春江周少雄
Owner JIANGSU JICUI ANTAI CHUANGMING ADVANCED ENERGY MATERIALS RES INST CO LTD
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