P-coumaric acid and o-phenanthroline mixed samarium complex, preparation method and application thereof

A technology of hydroxyphenylacrylic acid and carboxyl hydroxyphenylacrylic acid, which is applied in the field of rare earth metal complex materials, can solve the problems of difficult purification and separation of samples, high risk, high temperature, etc., and achieve high yield, overcome high temperature and high pressure, and mild conditions.

Inactive Publication Date: 2010-09-08
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the current synthesis methods of samarium metal carboxylic acid ligand complexes are all hydrothermal or solvothermal synthesis methods. The above synthesis methods all have high temperature, high risk, low yield, and difficult purification and separation of samples. defect

Method used

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  • P-coumaric acid and o-phenanthroline mixed samarium complex, preparation method and application thereof
  • P-coumaric acid and o-phenanthroline mixed samarium complex, preparation method and application thereof
  • P-coumaric acid and o-phenanthroline mixed samarium complex, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 0.1mmol Sm(NO 3 ) 3 ·6H 2 O is placed at the bottom of the test tube and dissolved with 5 mL of distilled water to form reaction solution A; 15 ml of a mixed solution C of methanol and water at a volume ratio of 1:1 is added in the middle; 0.05 mmol of HL and 0.05 mmol of phen are dissolved in 5 mL of methanol, and 2,6-dimethyl Base pyridine 0.017mL to obtain reaction solution B, placed in the upper layer of the test tube. After sealing and standing for 25 days, a yellow blocky single crystal appeared at the junction of the solution interface on the test tube wall. The crystals were washed successively with distilled water, ethanol and ether, and dried in vacuum, with a yield of about 50%.

[0026] The main infrared absorption peaks are: 3184s(br), 2816w, 1636s, 1607s, 1565s, 1512s, 1417vs, 1347w, 1287m, 1248s, 1168s, 1141w, 1101w, 1047w, 981m, 939w, 872w, 863m, 836s, 806w, 765w, 729m, 703w, 637w, 625w, 566w, 454w, 529m, 517w, 416w.

Embodiment 2

[0027] The preparation of embodiment 2 complexes

[0028] 0.2mmol Sm(ClO 4 ) 3 ·6H 2 O is placed at the bottom of the test tube and dissolved with 5 mL of distilled water; 20 mL of a mixed solution of methanol and water at a volume ratio of 1:1.2 is added in the middle; 0.08 mmol of HL and 0.08 mmol of phen are dissolved in 5 mL of methanol, and 0.023 mL of 2,6-lutidine is added The reaction solution B was obtained and placed on the upper layer of the test tube. After being sealed and left standing for 28 days, yellow massive single crystals appeared at the junction of the solution interface on the test tube wall. The crystals were washed successively with distilled water, ethanol and ether, and dried in vacuum. The yield was about 55%.

[0029] The main infrared absorption peaks are: 3184s(br), 2816w, 1636s, 1607s, 1565s, 1512s, 1417vs, 1347w, 1287m, 1248s, 1168s, 1141w, 1101w, 1047w, 981m, 939w, 872w, 863m, 836s, 806w, 765w, 729m, 703w, 637w, 625w, 566w, 454w, 529m, 517...

Embodiment 3

[0030] The preparation of embodiment 3 complexes

[0031] 0.24mmol Sm(SO 4 ) 3 ·8H 2 O is placed at the bottom of the test tube and dissolved with 4 mL of distilled water to form reaction solution A; 16 ml of a mixed solution C of methanol and water at a volume ratio of 1:1.1 is added in the middle; 0.10 mmol of HL and 0.10 mmol of phen are dissolved in 4 mL of methanol, and 2,6-dimethyl Base pyridine 0.02mL to obtain reaction solution B, placed in the upper layer of the test tube. After sealing and standing for 33 days, a yellow blocky single crystal appeared at the junction of the solution interface on the test tube wall. The crystals were washed successively with distilled water, ethanol and ether, and dried in vacuum, with a yield of about 57%.

[0032] The main infrared absorption peaks are: 3184s(br), 2816w, 1636s, 1607s, 1565s, 1512s, 1417vs, 1347w, 1287m, 1248s, 1168s, 1141w, 1101w, 1047w, 981m, 939w, 872w, 863m, 836s, 806w, 765w, 729m, 703w, 637w, 625w, 566w, 454...

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Abstract

The invention relates to a p-coumaric acid and o-phenanthroline mixed samarium complex, a preparation method and an application thereof. The chemical formula of the complex is as follows: [[Sm(L)3(phen)]2(dmpy)(CH3OH)2(H2O)2] infinity, wherein L is a carboxyl anion ligand of p-coumaric acid, phen is o-phenanthroline, and dmpy is 2,6-dimethyl pyridine. The complex is prepared with a test tube stratification diffusion method. The method overcomes the technical defects of high pressure and high temperature, high risk, low yield, difficult separation and purification and poor repeatability in the traditional hydrothermal/solvothermal synthesis method of rare earth samarium carboxylic acid complex. The synthesis method disclosed by the invention is carried out at the normal temperature and pressure, and has the advantages of moderate condition, high yield and good reproducibility. The fluorescence spectrum data of the crystal specimen of the complex shows that the complex can emit stable solid-state fluorescence, and the complex can be used as the fluorescent material in the material science field.

Description

technical field [0001] The invention belongs to the field of rare earth metal complex materials, and specifically relates to a samarium complex compounded with p-hydroxyphenylacrylic acid and o-phenanthroline and its preparation method and application. The complex has a dual-nuclear structure, and its fluorescent properties make it a fluorescent The material can be widely used. Background technique [0002] In recent years, carboxylic acid complexes of rare earths have received great attention because of their novel structural characteristics and superior optical, electrical, magnetic and catalytic properties (such as: high luminous intensity, good monochromaticity, long lifetime of excited states, etc.). It has been synthesized and studied a lot, and has become one of the current research hotspots in organometallic chemistry. Carboxylic acid ligands with rich coordination modes have always received great attention in the construction of coordination compounds. In particul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C09K11/06
Inventor 周立明方少明刘春森户敏高丽君孙光辉郭良起马松涛张强
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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