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Preparation method of polyacid based tubular monocrystal microreactor

A micro-reactor, tubular technology, applied in the field of polyacid-based tubular single-crystal micro-reactor preparation, can solve the problem of lack of crystal structure and the like

Inactive Publication Date: 2013-07-10
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

What is more relevant to the present invention is the report of these polyacid tubular materials, but the difference is that these tubular materials are polycrystalline, and their composition is determined by methods such as thermogravimetric analysis, infrared, and elemental analysis. crystal structure of

Method used

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  • Preparation method of polyacid based tubular monocrystal microreactor
  • Preparation method of polyacid based tubular monocrystal microreactor
  • Preparation method of polyacid based tubular monocrystal microreactor

Examples

Experimental program
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Effect test

Embodiment 1

[0020] A polyacid-based tubular single-crystal microreactor whose chemical composition is: Mn[Zn(im)] 2 {[Na(H 2 O)] 2 [Mn(H 2 O) 2 ][Zn(im) 2 ][P 4 Mo 6 o 31 h 6 ] 2} 8H 2 O.

[0021] Preparation method: Add molybdate and phosphorous acid in distilled water at a molar ratio of 5:1, and use hydrochloric acid (6 mol L －1 ) to adjust the pH of the mixture between 5 and stir for 20 minutes. Imidazole (im), manganese chloride, and zinc acetate were sequentially added to the mixture and stirred for 20 minutes. Then put it into a high-pressure reaction kettle, raise the temperature to 170°C, keep it warm for 60 hours, then lower it to room temperature at a speed of 1-10°C / min, and filter to obtain a polyacid-based tubular single crystal microreactor.

Embodiment 2

[0023] A polyacid-based tubular single-crystal microreactor whose chemical composition is: Mn[Zn(im)] 2 {[Na(H 2 O)] 2 [Mn(H 2 O) 2 ][Zn(im) 2 ][P 4 Mo 6 o 31 h 6 ] 2} 8H 2 O.

[0024] Preparation method: Add molybdate and phosphorous acid in distilled water at a molar ratio of 5:1, and use hydrochloric acid (6 mol L －1 ) to adjust the pH of the mixture to 3 and stir for 30 minutes. Imidazole (im), manganese chloride, and zinc acetate were sequentially added to the mixture and stirred for 30 minutes. Then put it into a high-pressure reaction kettle, raise the temperature to 160°C, keep it warm for 48 hours, then lower it to room temperature at a speed of 1-10°C / min, and filter to obtain a polyacid-based tubular single crystal microreactor.

Embodiment 3

[0026] A polyacid-based tubular single-crystal microreactor whose chemical composition is: Mn[Zn(im)] 2 {[Na(H 2 O)] 2 [Mn(H 2 O) 2 ][Zn(im) 2 ][P 4 Mo 6 o 31 h 6 ] 2} 8H 2 O.

[0027] Preparation method: add molybdate and phosphorous acid in distilled water at a molar ratio of 5:1, and use hydrochloric acid (6 mol L －1) to adjust the pH of the mixture at 6 and stir for 30 minutes. Imidazole (im), manganese chloride, and zinc acetate were sequentially added to the mixture and stirred for 30 minutes. Then put it into a high-pressure reaction kettle, raise the temperature to 180°C, keep it warm for 72 hours, then lower it to room temperature at a speed of 1-10°C / min, and filter to obtain a polyacid-based tubular single crystal microreactor.

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Abstract

The invention belongs to a chemical synthesis method, and in particular relates to a preparation method of a polyacid based tubular monocrystal microreactor. The polyacid based tubular monocrystal microreactor has a classical polyacid-organic skeleton structure of 4-connected diamond network topology, is a tubular crystalline material obtained by converting transition metal ions and a transition metal-organic unit bridged polyanionic cluster {Mo6O12(OH)3(HPO4)3(PO4)} into a polyacid based metal-organic skeleton at a proper pH value and a proper temperature, and has the chemical composition of Mn[Zn(im)]2{[Na(H2O)]2[Mn(H2O)2][Zn(im)2][P4Mo6O31H6]2}.8H2O, wherein im represents imidazole. The polyacid based tubular monocrystal microreactor overcomes the limit of the traditional polyacid based microtube material, is the first polyacid based monocrystal microtubule material with the precise chemical structure as well as has the redox activity. Therefore, the polyacid based tubular monocrystal microreactor can be served as a microtube reactor and can also be served as a reducing agent during the reaction process while the skeleton structure is unchanged. As a result, the preparation of the polyacid based tubular monocrystal microreactor has the important significance and great application prospect.

Description

[0001] technical field [0002] The invention belongs to chemical synthesis technology, in particular to a method for preparing a multi-acid base tubular single crystal microreactor. Background technique [0003] In general, microreactors can be fabricated from a variety of substrates, including silicon, quartz, metals, polymers, ceramics, and glass, depending to a large extent on the purpose of the reactor and the method of fabrication (Chem. Commun. , 2007, 443–467). No matter from academic or industrial point of view, the use of microreactors can greatly improve the efficiency of chemical reactions, which has aroused great interest of researchers. Although tubular entities exist widely in nature (Adv. Mater., 2007, 19, 858–861), artificially synthesized tubular structures attracted people’s attention after the discovery of carbon nanotubes (Nature, 1991, 354, 56–58 ). Since then, researchers have devoted a lot of effort to design and construct artificial nano / microporo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/08C30B29/10C30B29/66
Inventor 兰亚乾杜东英秦俊生苏忠民
Owner NORTHEAST NORMAL UNIVERSITY
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