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Metal-string material connected with aromatic dibasic acid and method for preparing same

A technology of aromatic dicarboxylic acid and metal strings, applied in organic chemistry, nickel organic compounds, etc., can solve the problem of limited length of dipyridylamine trinuclear nickel metal strings

Inactive Publication Date: 2009-12-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the limited length of existing dipyridinamine trinuclear nickel metal strings, and aims to provide materials and preparation methods for realizing one-dimensional dipyridylamine nickel metal strings using aromatic dicarboxylic acid linkers

Method used

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  • Metal-string material connected with aromatic dibasic acid and method for preparing same

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Experimental program
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Effect test

Embodiment 1

[0026] Solution mixing reaction synthesis [Ni 3 (dpa) 4 (1,2-nbdc)] material.

[0027] 1. Synthesis of tri-nuclear nickel metal string [Ni 3 (dpa) 4 Cl 2 ]:

[0028] Take 7.6g of anhydrous nickel chloride, 20g of naphthalene, and 13.6g of dipyridylamine (Hdpa) in a 100ml Erlenmeyer flask, add a stirrer, control the heating temperature at about 180°C, heat for 4h, and add 8.8g of it dropwise within 10 minutes Dissolve potassium tert-butoxide in 15ml of n-butanol, purple or black products appear, heat for 4 hours, stop heating and cool to about 80°C, add 50ml of n-hexane in three batches to remove naphthalene, and extract three times with 100ml of dichloromethane Product, remove dichloromethane with rotary evaporator, recrystallize with dichloromethane / n-hexane;

[0029] 2. Three-core nickel metal string [Ni 3 (dpa) 4 (ClO 4 ) 2 ]preparation:

[0030] Take 0.05 mole [Ni 3 (dpa) 4 Cl 2 ] was dissolved in 1000ml of dichloromethane, and 0.1 mole of Ag(ClO 4 ) was dis...

Embodiment 2

[0035] [Ni] was synthesized by solution layered diffusion method 3 (dpa) 4 (1,2-nbdc)] material

[0036] Using a 20cm long, 0.8cm diameter thin tube experiment, 6ml concentration of 5.0mmol / l 3-nitrosodium hydrogen phthalate aqueous solution is placed at the bottom of the test tube, 6ml concentration of 5.0mmol / l [Ni 3 (dpa) 4 (ClO 4 ) 2 ] The methanol solution was slowly placed on the 3-nitrosodium hydrogen phthalate aqueous solution, and suitable crystals grew after 45 days, and the crystals were analyzed by single crystal X-ray diffraction to confirm that the material had a one-dimensional structure.

Embodiment 3

[0038] [Ni 3 (dpa) 4 (1,3-bdc)] material synthesis.

[0039] Weigh 25.0g of isophthalic acid, 12.0g of NaOH, add 200ml of water, stir until completely dissolved, the solution is clear, filter, evaporate the solution to dryness at 90°C, and bake in an oven at 120°C for 2h to obtain isophthalic acid Disodium salt 31.1g. Weigh 10.0g (0.047mol) of isophthalic acid disodium salt and dissolve it in 1000ml water, weigh 50.0g [Ni 3 (dpa) 4 (ClO 4 ) 2 ] (0.047mol) was dissolved in 1000ml of acetone, mixed the above two solutions appeared precipitation, stirring reaction 2h. The product was washed with water and acetone respectively, and baked in an oven at 120°C for 2 hours. The product was confirmed by mass spectrometry (FAB). The product is insoluble in dimethylformamide, dimethylsulfoxide, dichloromethane, chloroform, tetrahydrofuran, acetonitrile, methanol and ethanol. Yield 42.4g, about 88% yield. Through infrared (IR) analysis, the product is at 1700cm -1 There is no a...

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Abstract

The invention provides a nickel metal-string material of aromatic dibasic acid bipyridine amine, which has a chemical formula of [Ni3C40H32N12X]. The material is characterized in that: the material consists of a nickel trinuclear skeleton [Ni3(dpa)4] and a connexon X, wherein the dpa is a univalent anion of bipyridine amine, and X is a bivalent anion of aromatic dicarboxylic acid; and the material comprises six types which are [Ni3(dpa)4(1,2-nbdc)], [Ni3(dpa)4(1,3-bdc)], [Ni3(dpa)4(1,3-hbdc)], [Ni3(dpa)4(1,3-abdc)], [Ni3(dpa)4(1,4-bdc)], or [Ni3(dpa)4(1,4-nbdc)]. The material is prepared by the solution mixing method or solution layering diffusion method of the [Ni3(dpa)4(ClO4)2] and a salt of aromatic dibasic acid. The material can be extended in one dimension, the synthetic yield is high, and the synthetic process is easy and convenient.

Description

technical field [0001] The invention relates to the manufacture of new molecular wire materials, in particular to the field of expanding the manufacture of polypyridylamine trinuclear nickel metal string materials. Background technique [0002] Metal string materials can be used as molecular wires, which are a new class of molecular devices. The polypyridylamine metal chain is a compound in which more than two metals are connected in a linear arrangement by polypyridylamine. At present, the number of metal atoms that can be connected by polypyridine amines of different lengths is 3-9. With the increase of the number of metal atoms, the production yield is getting lower and lower, and the synthesis yield of metal strings containing nine metal atoms is less than 0.1%. , so it is very difficult to prepare long metal chains through long polypyridylamines, and it is difficult to have practical value. However, connecting ligands or linkers with different lengths and different fu...

Claims

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Application Information

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IPC IPC(8): C07F15/04C07D213/74
Inventor 张静朱龙观
Owner ZHEJIANG UNIV