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Method for preparing light-emitting crystal material [WS4Cu4(SCN)4Tb2(INA)4(HMPA)8]n with picric acid detecting function

A technology of luminescent crystals and picric acid, which is applied in the direction of luminescent materials, chemical instruments and methods, can solve the problems of expensive and complex equipment, and equipment can be moved at any time, and achieve the effects of high yield, easy access to raw materials, and simple synthetic routes

Inactive Publication Date: 2016-06-01
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the detection method of aromatic nitro explosives is mainly carried out by simulating the ability of dogs (electronic nose) and other complex instruments. These equipment are not only expensive and complicated, but also need to solve the problem that the equipment can be moved at any time when used in the field.

Method used

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  • Method for preparing light-emitting crystal material [WS4Cu4(SCN)4Tb2(INA)4(HMPA)8]n with picric acid detecting function
  • Method for preparing light-emitting crystal material [WS4Cu4(SCN)4Tb2(INA)4(HMPA)8]n with picric acid detecting function

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Experimental program
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Embodiment 1

[0016] Embodiment 1: The present invention has the luminescence crystal material [WS that detects picric acid 4 Cu 4 (SCN) 4 Tb 2 (INA) 4 (HMPA) 8 ] n The preparation method comprises the following steps:

[0017] The first step is to add tungstic acid into the ammonia solution and stir to obtain the ammonia solution of tungstic acid;

[0018] In the second step, hydrogen sulfide is introduced into the aqueous solution of ammonium tungstate prepared in the first step to react, and the compound tetrathioammonium tungstate is obtained through suction filtration and drying;

[0019] In the third step, 2 mmol of cuprous thiocyanate and 1 mmol of ammonium tetrathiotungstate were added to 5 ml of hexamethylphosphoric triamide solvent, and stirred for 20 minutes to obtain a clear solution;

[0020] In the fourth step, 2 mmol of isonicotinic acid was added to the solution prepared in the third step, stirred for 30 minutes until completely dissolved, and a red clear solution was...

Embodiment 2

[0023] Embodiment 2: The present invention has the luminescence crystal material [WS that detects picric acid 4 Cu 4 (SCN) 4 Tb 2 (INA) 4 (HMPA) 8 ] n The preparation method comprises the following steps:

[0024] The first step is to add tungstic acid into the ammonia solution and stir to obtain the ammonia solution of tungstic acid;

[0025] In the second step, hydrogen sulfide is introduced into the aqueous solution of ammonium tungstate prepared in the first step to react, and the compound tetrathioammonium tungstate is obtained through suction filtration and drying;

[0026] In the third step, 3 mmol of cuprous thiocyanate and 1 mmol of ammonium tetrathiotungstate were added to 5 ml of hexamethylphosphoric triamide solvent, and stirred for 20 minutes to obtain a clear solution;

[0027] In the fourth step, 3 mmol of isonicotinic acid was added to the solution prepared in the third step, and stirred for 30 minutes until completely dissolved to obtain a red clear sol...

Embodiment 3

[0030] Embodiment 3: The present invention has the luminescence crystal material [WS that detects picric acid 4 Cu 4 (SCN) 4 Tb 2 (INA) 4 (HMPA) 8 ] n The preparation method comprises the following steps:

[0031] The first step is to add tungstic acid into the ammonia solution and stir to obtain the ammonia solution of tungstic acid;

[0032] In the second step, hydrogen sulfide is introduced into the aqueous solution of ammonium tungstate prepared in the first step to react, and the compound tetrathioammonium tungstate is obtained through suction filtration and drying;

[0033] In the third step, 4 mmol of cuprous thiocyanate and 1 mmol of ammonium tetrathiotungstate were added to 5 ml of hexamethylphosphoric triamide solvent, and stirred for 20 minutes to obtain a clear solution;

[0034] In the fourth step, 4 mmol of isonicotinic acid was added to the solution prepared in the third step, and stirred for 30 minutes until completely dissolved to obtain a red clear sol...

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Abstract

The invention discloses a method for preparing a light-emitting crystal material [WS4Cu4(SCN)4Tb2(INA)4(HMPA)8]n with a picric acid detecting function. Hydrogen sulfide is introduced into an ammonia water solution of tungstic acid to react, and ammonium tetrathiotungstate is prepared through suction filtration and drying; ammonium tetrathiotungstate and cuprous thiocyanate are added into a hexamethylphosphoric triamide solvent to prepare a solution, isonicotinic acid is added into the prepared solution to be stirred and dissolved, and after a red clear solution is prepared, the pH of the solution is adjusted to range from 8 to 10; a solution of terbium trinitrate is added into the red clear solution, and the light-emitting crystal material [WS4Cu4(SCN)4Tb2(INA)4(HMPA)8]n is obtained through crystallization, filtration, washing and drying. The method has the advantage that the light-emitting crystal material [WS4Cu4(SCN)4Tb2(INA)4(HMPA)8]n capable of efficiently detecting picric acid is obtained.

Description

a technical field [0001] The invention relates to the preparation of aromatic nitro explosive detection materials, in particular to a luminescent crystal material [WS 4 Cu 4 (SCN) 4 Tb 2 (INA) 4 (HMPA) 8 ] n method of preparation. Two background technology [0002] Since the Second World War, aromatic nitro compounds have been widely used in military and industrial fields as a kind of high-energy explosives. The rapid and selective detection of aromatic nitro explosives has become one of the problems related to many fields such as homeland security, military applications, forensic investigation, and minefield analysis. And because these aromatic nitro explosives are one of the important environmental pollutants, the detection of aromatic nitro explosives in soil and groundwater is very important for burial tracking, underwater explosives and environmental monitoring near ammunition bases, etc. Therefore, it is very meaningful to study the detection of aromatic nitro ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09K11/06
CPCC08G83/008C09K11/06C09K2211/1466C09K2211/183C09K2211/188
Inventor 张金方刘宇航张弛
Owner JIANGNAN UNIV
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