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Preparation method of [Ni (Me3en) (acac)] BPh4

A solution and hexahydrate technology, which is applied in the field of preparation of [Ni]BPh4, can solve the problems of toxic safety, waste liquid treatment, many operation steps and high preparation cost, and achieves the effects of low cost, easy operation and simple device.

Pending Publication Date: 2022-08-02
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method has a long reaction time, many operation steps (involving twice normal pressure filtration and rotary steaming, etc.), and the preparation cost is high
More importantly, a large amount of organic solvents such as dichloromethane and petroleum ether are used in the preparation of the target product and its post-treatment process, which involves problems of toxicity, safety and waste liquid treatment.

Method used

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  • Preparation method of [Ni (Me3en) (acac)] BPh4

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 (aqueous one-pot method)

[0025] [Ni(Me 3 en)(acac)]BPh 4 Preparation process of solvent / thermochromic material:

[0026] Using pure water as the medium, according to the composition ratio of the complexes, take nickel nitrate hexahydrate (0.87g Ni(NO) 3 ) 2 ·6H 2 O), acetylacetone (0.75mL 4mol L -1 Hacac / ethanol solution), sodium carbonate (0.16g Na 2 CO 3 ), N,N,N'-trimethylethylenediamine (0.75mL 4mol L -1 Me 3 en / ethanol solution) and sodium tetraphenylborate (1.44g NaBPh 4 ) in the reaction flask, add 15 mL of pure water, stir and react for 30 min, filter with a glass sand core funnel, fully wash the product with pure water, drain it, and dry it in an oven at 80 °C. The obtained product is a red complex [Ni(Me 3 en)(acac)]BPh 4 , the yield is about 80%.

Embodiment 2

[0027] Example 2 (ethanol one-pot method)

[0028] The difference between Example 2 and Example 1 is that ethanol is used as the medium, and other operations are the same, and the yield of the obtained product is about 80%.

Embodiment 3

[0029] Example 3 (solid phase one-pot method)

[0030] The acetylacetone ethanol solution and the N,N,N'-trimethylethylenediamine ethanol solution in Examples 1, 2, and 3 are not limited to using ethanol as a solvent, and can also use water as a solvent, or directly use the stock solution.

[0031] The difference between Example 3 and Example 1 is that all the compounds were directly put into a mortar and pre-ground for 10 min, and other operations were the same, and the yield of the obtained product was about 80%.

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Abstract

The preparation method of the [Ni (Me3en) (acac)] BPh4 comprises the following steps: adding nickel nitrate hexahydrate, an acetylacetone solution, sodium carbonate, an N, N, N '-trimethyl ethylenediamine solution and sodium tetraphenylborate into a solvent, stirring, carrying out suction filtration, washing and drying to obtain a target product. The complex shows different colors in different solvents, changes are obvious and easy to recognize, and the complex has certain application value in the aspects of convenient detection, industrial production and the like. The three preparation methods are respectively a liquid phase reaction taking pure water as a medium, a liquid phase reaction taking ethanol as a medium and a solid phase reaction, and compared with a traditional method, the preparation method is convenient and rapid, easy to operate and lower in cost, does not use toxic and harmful organic reagents, and can be widely applied to preparation of the complex.

Description

technical field [0001] The invention relates to the field of color-changing materials, in particular to [Ni(Me 3 en)(acac)]BPh 4 preparation method. Background technique [0002] Color-changing materials usually refer to materials that can change color under external conditions, and can be divided into thermochromic materials, photochromic materials, electrochromic materials and solvochromic materials according to the stimulation mode. Color-changing materials are a kind of intelligent materials with memory function, which are widely used in various fields such as military, information processing, medical diagnosis, energy-saving materials, and anti-counterfeiting marks. [0003] Red [Ni(Me 3 en)(acac)]BPh 4 The complexes have solvent and thermochromic effects. It is mixed with materials such as SAP (saponite, saponite) or high molecular polymer Nafion (a perfluorosulfonic acid polymer) with a layered structure, and after proper treatment, an organic solvent identificat...

Claims

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Application Information

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IPC IPC(8): C07F15/04C09K9/02
CPCC07F15/045C09K9/02C09K2211/187
Inventor 任艳平董志强易波陈烨超陈欣
Owner XIAMEN UNIV
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