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Preparation method of crystal material [WS4Cu4(CN)2(TPP) (2, 3, 5, 6-4-tetra-pyridyl pyrazine)] with high detection sensitivity for TNP (2, 4, 6-trinitrophenol)

A crystal material, ws4cu4 technology, applied in the direction of polycrystalline material growth, crystal growth, chemical instruments and methods, etc., can solve the problem of rare crystal materials, and achieve easy control, good optical stability, and sensitive fluorescence detection performance. Effect

Inactive Publication Date: 2018-04-13
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] There are many examples of crystal materials synthesized by solvothermal method, but in situ reaction is added to the solvent method to obtain new final ligands from raw materials and combine with other raw materials to obtain crystalline materials.

Method used

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  • Preparation method of crystal material [WS4Cu4(CN)2(TPP) (2, 3, 5, 6-4-tetra-pyridyl pyrazine)] with high detection sensitivity for TNP (2, 4, 6-trinitrophenol)
  • Preparation method of crystal material [WS4Cu4(CN)2(TPP) (2, 3, 5, 6-4-tetra-pyridyl pyrazine)] with high detection sensitivity for TNP (2, 4, 6-trinitrophenol)
  • Preparation method of crystal material [WS4Cu4(CN)2(TPP) (2, 3, 5, 6-4-tetra-pyridyl pyrazine)] with high detection sensitivity for TNP (2, 4, 6-trinitrophenol)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: A kind of crystal material [WS of highly sensitive detection TNP of the present invention 4 Cu 4 (CN) 2 (TPP)] preparation method, comprises the following steps:

[0021] In the first step, 0.1 mmol of ammonium tetrathiotungstate, 0.3 mmol of ammonium thiocyanate, 0.3 mmol of cuprous cyanide, 0.2 mmol of 4-(pyridin-4-yl)methyleneamino-1, 2,4-triazole was added to a mixed solvent of 1 ml of acetonitrile and 3 ml of N,N-dimethylformamide and stirred to obtain a homogeneous suspension;

[0022] In the second step, transfer the homogeneously stirred suspension in the first step into a reaction kettle, heat it to 90 degrees in an airtight manner for three days, then slowly lower it to room temperature at a rate of 2 degrees per hour, filter it with suction, wash and dry it get [WS 4 Cu 4 (CN) 2 (TPP)] crystalline material.

[0023] Fluorescence quenching test: the prepared crystal material [WS 4 Cu 4 (CN) 2 (TPP)] (1 mg) was dispersed in 2.5 ml of N,N...

Embodiment 2

[0024] Embodiment 2: A kind of crystal material [WS of highly sensitive detection TNP of the present invention 4 Cu 4 (CN) 2 (TPP)] preparation method, comprises the following steps:

[0025] In the first step, 0.1 mmol of ammonium tetrathiotungstate, 0.4 mmol of ammonium thiocyanate, 0.4 mmol of cuprous cyanide, 0.4 mmol of 4-(pyridin-4-yl)methyleneamino-1, 2,4-triazole was added to a mixed solvent of 1 ml of acetonitrile and 3 ml of N,N-dimethylformamide and stirred to obtain a suspension;

[0026] In the second step, transfer the homogeneously stirred suspension in the first step into a reaction kettle, heat it to 90 degrees in an airtight manner for three days, then slowly lower it to room temperature at a rate of 2 degrees per hour, filter it with suction, wash and dry it get [WS 4 Cu 4 (CN) 2 (TPP)] crystalline material.

[0027] Fluorescence quenching test: the prepared crystal material [WS 4 Cu 4 (CN) 2 (TPP)] (1 mg) was dispersed in 2.5 ml of N,N-dimethylfor...

Embodiment 3

[0028] Embodiment 3: A kind of crystal material [WS of highly sensitive detection TNP of the present invention 4 Cu 4 (EN) 2 (TPP)] preparation method, comprises the following steps:

[0029] In the first step, 0.1 mmol of ammonium tetrathiotungstate, 0.3 mmol of ammonium thiocyanate, 0.3 mmol of cuprous cyanide, 0.2 mmol of 4-(pyridin-4-yl)methyleneamino-1, 2,4-triazole was added to a mixed solvent of 1 ml of acetonitrile and 4 ml of N,N-dimethylformamide and stirred to obtain a suspension;

[0030] In the second step, transfer the homogeneously stirred suspension in the first step into a reaction kettle, heat it in an airtight manner to 85 degrees for three days, and then slowly lower it to room temperature at a rate of 2 degrees per hour, filter it with suction, wash and dry it get [WS 4 Cu 4 (EN) 2 (TPP)] crystalline material.

[0031] Fluorescence quenching test: the prepared crystal material [WS 4 Cu 4 (EN) 2 (TPP)] (1 mg) was dispersed in 2.5 ml of N,N-dimethy...

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Abstract

The invention discloses a preparation method of a crystal material [WS4Cu4(CN)2(TPP) (2, 3, 5, 6-4-tetra-pyridyl pyrazine)] with high detection sensitivity for TNP (2, 4, 6-trinitrophenol). The preparation method comprises the following steps: adding ammonium tetrathiotungstate, ammonium thiocyanate, cuprous cyanide and 4-(4-pyridyl) methylene amino-1, 2, 4-triazole into a mixed solvent acetonitrile and N, N-dimethylformamide at a certain ratio and stirring the mixture, so as to obtain a uniform turbid liquid; transferring the uniformly stirred turbid liquid into a reaction kettle for airtightheating to a certain temperature for a few days, slowly reducing the temperature to a room temperature, performing suction filtration, washing and drying, so as to obtain the crystal material [WS4Cu4(CN)2(TPP)]. The preparation method has the advantage that the crystal material [WS4Cu4(CN)2(TPP)] with high detection sensitivity for the TNP is obtained.

Description

a technical field [0001] The present invention relates to the preparation of crystal materials with fluorescence detection performance, in particular to a crystal material [WS 4 Cu 4 (CN) 2 (TPP)] (TPP=2,3,5,6-tetra-4-pyridylpyrazine) preparation method. Two background technology [0002] In recent years, chemical explosives have been widely used in terrorist attacks against some countries, posing a serious threat to people's daily life. Chemical explosives are mostly compounds containing nitro or nitroaromatic rings, such as nitrobenzene (NB), 2,4,6-trinitrotoluene (TNT), 1,3,5-trinitrobenzene (TNB ), 2,4,6-trinitrophenol (TNP), 2,4-dinitrotoluene (2,4-DNT), p-nitrotoluene (4-NT), etc. It is worth noting that these aromatic nitro compounds also widely exist in pesticides, dyes, fireworks, and medicines, which will pollute groundwater and soil and cause harm to human health during the production process. Therefore, the rapid and sensitive detection of aromatic nitro com...

Claims

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Application Information

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IPC IPC(8): C30B7/14C30B29/54
CPCC30B7/14C30B29/54
Inventor 张金方冯姣阳吴俊洁
Owner JIANGNAN UNIV
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