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Multi-metal hybrid compound formed by transplanting metal-Schiff base fragment on isopolymolybdate, preparation method and applications thereof

A technique for Schiff bases and compounds, applied in the field of polymetallic hybrid compounds and their preparation, can solve the problems of lack of expansion and the like

Inactive Publication Date: 2013-08-21
KUNMING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, the work combining the above two fields is far from extensive, there is only a small part of the work on the simultaneous combination of POM and metal-shiff-base, and the single crystal structure of such hybrid compounds has never been seen. to report

Method used

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  • Multi-metal hybrid compound formed by transplanting metal-Schiff base fragment on isopolymolybdate, preparation method and applications thereof
  • Multi-metal hybrid compound formed by transplanting metal-Schiff base fragment on isopolymolybdate, preparation method and applications thereof
  • Multi-metal hybrid compound formed by transplanting metal-Schiff base fragment on isopolymolybdate, preparation method and applications thereof

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preparation example Construction

[0023] The preparation method of the polymetallic hybrid compound formed by grafting metal-Schiff base fragments on the polymolyte of the present invention comprises the following steps:

[0024] A, take acidified sodium molybdate solution, will contain [Mn(salen)(H 2 O)] 2 (ClO 4 ) 2 ·H 2 O methanol solution is dropped into wherein, the sodium molybdate solution of described acidification, containing [Mn(salen)(H 2 O)] 2 (ClO 4 ) 2 ·H 2 The volume ratio of O methanol solution is 3~5:1;

[0025] B. Continue stirring at 55~65°C for 11~13h to obtain a brown clear solution;

[0026] C. After filtering, seal it with a film with very fine pores, and slowly volatilize the filtrate at room temperature. After 21 days, a flaky crystal product is obtained, rinsed with methanol, and dried in the air to obtain the transplanted metal-Schiff on the isopolymolyte. Multimetallic hybrid compounds formed by base fragments.

[0027] The acidified sodium molybdate solution described in...

experiment example 1

[0034] 20 ml of a solution containing 0.351 g (1.45 mmol) of sodium molybdate was introduced into a 100 ml Erlenmeyer flask and stirred vigorously, after which 3N hydrochloric acid was added dropwise to the above solution and stirred vigorously for 1 hour. Then, the new [Mn(salen)(H 2 O)] 2 (ClO 4 ) 2 ·H 2 O (0.88 g, 1 mmol) in methanol solution 5ml was added dropwise to the above solution. After stirring overnight in the Erlenmeyer flask at 60° C., a brown clear solution was obtained. After filtration, seal the filtrate with a membrane with very fine pores for slow evaporation. Flaky brown crystals were obtained after three weeks.

Embodiment 1

[0036] Preparation of acidified sodium molybdate solution: drop 3N HCL into 40ml of sodium molybdate solution with a sodium molybdate content of 0.07mmol / ml at a rate of 2 drops / s, the amount of instillation is 2ml, and the solution is 120 r / min Stir at a rotating speed for 50 min.

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Abstract

The present invention discloses a multi-metal hybrid compound formed by transplanting a metal-Schiff base fragment on an isopolymolybdate, a preparation method and applications thereof. The compound comprises an isopolymolybdate and a metal Schiff base fragment, has a molecular formula [NH4]2{[Mn(salen)(H2O)]2[Mo8O26(MoO4)2]}(H2en)2.9H2O, and is a triclinic system, wherein a space group is P-1, crystal cell parameters comprise that a is 10.507(2)angstrom, b is 13.708(3)angstrom, c is 14.701(3)angstrom, alpha is 108.94(3), beta is 110.16(3), gamma is 93.98(3), V is 1840.5(6)angstrom<3>, and Z is 2, and the crystal cell has a structure and a composition represented by a formula 1, and is represented by a Figure 2. The preparation method comprises: adding a [Mn(salen)(H2O)]2(ClO4)2.H2O-containing methanol solution in a dropwise manner, continuously stirring for 11-13 h at a temperature of 55-65 DEG C to obtain a brown clear solution, filtering, adopting a film with fine holes to carry out sealing storage, slowly evaporating the filtrate at a room temperature to obtain a sheet-like crystal product after 21 days, washing with methanol, and drying in air to obtain the multi-metal hybrid compound formed by transplanting the metal-Schiff base fragment on the isopolymolybdate, wherein the compound has characteristics of excellent stability and reusability, and can be used for catalytic degradation of pollutants in water in the photocatalysis field.

Description

technical field [0001] The invention belongs to the technical field of chemical material preparation, and in particular relates to a multimetal hybrid compound formed by grafting metal-Schiff base fragments on polymolyte, a preparation method and application thereof. Background technique [0002] Molecular-based polymetallic hybrid materials are an important branch of molecular science. In the past few decades, chemists have done a lot of work in selecting different organic or metal-organic fragments to modify polyanions, and there are also countless new properties. compounds have been reported. [0003] Among countless organic / inorganic metal compounds, metal-Schiff base type compounds are widely used in catalysis, biology and magnetic fields due to their rich structures and compositions, such as single-molecule magnets and single-chain magnets. Among the metal-Schiff base compounds, Mn-Schiff bases are the most important class of compounds due to their inherent paramagnet...

Claims

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Application Information

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IPC IPC(8): C07F13/00B01J31/34C02F1/32
Inventor 吴琼王海
Owner KUNMING UNIV
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