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Preparation method of luminous crystal material for luminous enhanced aqueous phase detection of Bi < 3 + >

A luminescent crystal, luminescence enhancement technology, applied in luminescent materials, fluorescence/phosphorescence, material analysis by optical means, etc., to achieve the effect of simple and controllable synthesis route

Active Publication Date: 2022-06-28
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing detection Bi 3+ few luminescent materials, with sensitive luminescence-enhanced aqueous phase detection of Bi 3+ Luminescent crystal materials have not yet been reported

Method used

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  • Preparation method of luminous crystal material for luminous enhanced aqueous phase detection of Bi &lt; 3 + &gt;
  • Preparation method of luminous crystal material for luminous enhanced aqueous phase detection of Bi &lt; 3 + &gt;
  • Preparation method of luminous crystal material for luminous enhanced aqueous phase detection of Bi &lt; 3 + &gt;

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 0.1 mmol cadmium chloride, 0.1 mmol 1,4-naphthalenedicarboxylic acid and 0.025 mmol 9-bis(3-pyridine)ethylene-fluorene to 6 mL of water and acetonitrile (V:V=1:1) and stir to prepare mixture;

[0039] The prepared mixture was heated to 140°C for 72h in a closed reactor, slowly cooled to room temperature at a rate of 5°C / h, filtered, ultrasonically washed with a mixed solution of acetonitrile and water, and dried in an oven at 60°C for 5min , that is, [Cd(NDA)(3-L)(H 2 O)] n crystalline material. Calculated yield: 40%.

Embodiment 2

[0041] Add 0.1 mmol of cadmium chloride, 0.1 mmol of 1,4-naphthalenedicarboxylic acid and 0.05 mmol of 9-bis(3-pyridine)ethylene-fluorene into 6 mL of water and acetonitrile (V:V=1:1) and stir to prepare mixture;

[0042] The obtained mixed solution was heated to 140°C for 72h in a closed reaction kettle, slowly cooled to room temperature at a rate of 5°C / h, filtered, washed with acetonitrile and water mixed solution 50Hz ultrasonically for 10min, oven 60°C Dry for 5 min to obtain [Cd(NDA)(3-L)(H 2 O)] n crystalline material. Calculated yield: 60%.

Embodiment 3

[0044] Add 0.1 mmol of cadmium chloride, 0.1 mmol of 1,4-naphthalenedicarboxylic acid and 0.075 mmol of 9-bis(3-pyridine)ethylene-fluorene to 6 mL of water and acetonitrile (V:V=1:1) and stir to prepare mixture;

[0045] The obtained mixed solution was heated to 140°C for 72h in a closed reaction kettle, slowly cooled to room temperature at a rate of 5°C / h, filtered, washed with acetonitrile and water mixed solution 50Hz ultrasonically for 10min, oven 60°C Dry for 5 min to obtain [Cd(NDA)(3-L)(H 2 O)] n crystalline material. Calculated yield: 55%.

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Abstract

The invention provides a preparation method and a product of a luminescent crystal material [Cd (NDA) (3-L) (H2O)] n for luminescence-enhanced aqueous phase detection of Bi < 3 + >, cadmium chloride, 1, 4-naphthalic acid and 9-bis (3-pyridine) ethylene-fluorene are added into a mixed solution of water and acetonitrile, stirring is performed to prepare a mixed solution, the mixed solution is placed in a closed reaction kettle for heating reaction, then the temperature is slowly reduced to room temperature, and the luminescent crystal material [Cd (NDA) (3-L) (H2O)] n is obtained. And filtering, washing and drying the product to obtain the luminescent crystal material. The luminescent crystal material [Cd (NDA) (3-L) (H2O)] n for detecting Bi < 3 + > in a high-sensitivity luminescence enhanced water phase is obtained for the first time, the synthetic route is simple and easy to control and suitable for industrial production, and the highest yield of the prepared material [Cd (NDA) (3-L) (H2O)] n can reach 60%. The enhancement constant Ksv is equal to-5.3 * 10 < 4 > M <-1 >, and the detection limit is 1.87 * 10 <-5 > mM.

Description

technical field [0001] The invention belongs to the technical field of luminescence detection crystal materials, and in particular relates to a luminescence enhanced aqueous phase detection Bi 3+ The preparation method of the luminescent crystal material. Background technique [0002] The trivalent metal bismuth ion (Bi 3+ ) is widely used in the pharmaceutical industry, such as for the production of antibacterial agents, anti-HIV agents, anti-ulcer agents and radiotherapy agents. However, excess Bi 3+ It will pose a threat to human health and the ecological environment. Bi in soil 3+ If the concentration exceeds 0.416g / kg, it will affect the reproduction rate and number of earthworms, and then affect soil aeration and soil porosity. and Bi 3+ Has a long half-life and may accumulate in the kidneys leading to kidney disease. Therefore, exploring efficient detection of Bi 3+ material is extremely important. [0003] Existing detection Bi 3+ Few luminescent materials ...

Claims

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Application Information

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IPC IPC(8): C07F3/08C08G83/00C09K11/06G01N21/64
CPCC07F3/003C08G83/008C09K11/06G01N21/643C09K2211/188
Inventor 张金方李文静林卓
Owner JIANGNAN UNIV
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