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Preparation method of crystal material {[NH4][TbCu(ina)4(CN)].2DMF}n with function of selectively adsorbing organic dye

A technology of crystal materials and organic dyes, which is applied in the growth of polycrystalline materials, adsorption of water/sewage treatment, crystal growth, etc., can solve the problems of application limitations and limited adsorption capacity of adsorbents, and achieve good adsorption performance, easy control, and synthesis The effect of a simple route

Inactive Publication Date: 2016-08-31
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the research on these new materials is still in its infancy, and its adsorption capacity as an adsorbent is still very limited, its application is greatly limited.

Method used

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  • Preparation method of crystal material {[NH4][TbCu(ina)4(CN)].2DMF}n with function of selectively adsorbing organic dye
  • Preparation method of crystal material {[NH4][TbCu(ina)4(CN)].2DMF}n with function of selectively adsorbing organic dye

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Embodiment 1

[0018] Embodiment 1: The present invention has the crystalline material {[NH 4 ][TbCu(ina) 4 (CN)]·2DMF} n The preparation method comprises the following steps:

[0019] The first step is to add tungstic acid into the ammonia solution and stir to obtain the ammonia solution of tungstic acid;

[0020] 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;

[0021] In the third step, 0.4mmol ammonium tetrathiotungstate and 1.2mmol cuprous cyanide were added to 4ml N,N'-dimethylformamide and stirred for 20 minutes to obtain an orange-red clear solution;

[0022] In the fourth step, 1.2 mmol of isonicotinic acid is added to the solution prepared in the third step, stirred, and ammonia water is added dropwise until it is completely dissolved to obtain a dark red solution and filtered;

[0023] In the fif...

Embodiment 2

[0025] Embodiment 2: the present invention has the crystalline material {[NH 4 ][TbCu(ina) 4 (CN)]·2DMF} n The preparation method comprises the following steps:

[0026] The first step is to add tungstic acid into the ammonia solution and stir to obtain the ammonia solution of tungstic acid;

[0027] 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;

[0028] In the third step, 0.4mmol ammonium tetrathiotungstate and 1.6mmol cuprous cyanide were added to 4ml N,N'-dimethylformamide and stirred for 20 minutes to obtain an orange-red clear solution;

[0029] In the fourth step, 2.4 mmol of isonicotinic acid is added to the solution prepared in the third step, stirred, and ammonia water is added dropwise until it is completely dissolved to obtain a dark red solution, which is then filtered;

[0030]...

Embodiment 3

[0032] Embodiment 3: the present invention has the crystalline material {[NH 4 ][TbCu(ina) 4 (CN)]·2DMF} n The preparation method comprises the following steps:

[0033] The first step is to add tungstic acid into the ammonia solution and stir to obtain the ammonia solution of tungstic acid;

[0034] 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;

[0035] In the third step, 0.4mmol ammonium tetrathiotungstate and 1.2mmol cuprous cyanide were added to 4ml N,N'-dimethylformamide and stirred for 20 minutes to obtain an orange-red clear solution;

[0036] In the fourth step, 2.4 mmol of isonicotinic acid is added to the solution prepared in the third step, stirred, and ammonia water is added dropwise until it is completely dissolved to obtain a dark red solution, which is then filtered;

[0037]...

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Abstract

The invention discloses a preparation method of a crystal material {[NH4][TbCu(ina)4(CN)].2DMF}n with the function of selectively adsorbing organic dye. The method comprises the steps that hydrogen sulfide is introduced into an ammonia solution of tungstic acid for a reaction, and suction filtration and drying are carried out to obtain ammonium tetrathiotungstate; the ammonium tetrathiotungstate and cuprous cyanide are added into N,N'-dimethyl formamide and stirred to obtain an orange red solution; isonicotinic acid is added into the obtained orange red solution, stirring is performed, ammonium hydroxide is dropwise added, the mixture is filtered after being completely dissolved, an acetonitrile solution containing terbium nitrate is added to the upper layer of filtrate, crystallization, filtration, washing and drying are performed, and therefore the crystal material {[NH4][TbCu(ina)4(CN)].2DMF}n is obtained. The preparation method has the advantage that the crystal material {[NH4][TbCu(ina)4(CN)].2DMF}n with the function of selectively adsorbing the organic dye is obtained.

Description

A technical field [0001] The present invention relates to the preparation of adsorption materials, in particular to a crystal material {[NH 4 ][TbCu(ina) 4 (CN)]·2DMF} n method of preparation. Two background technology [0002] In recent years, dyes have been widely used in industrial products such as papermaking, plastics, textiles, rubber, coatings, etc., bringing colorful colors to people's lives and generating huge economic benefits, but also producing a large amount of dye wastewater discharged to the environment water, causing serious harm to the environment and human health. Therefore, how to solve the dyes in wastewater has become a major problem faced by various countries in the world. So far, many methods on dye removal have been reported, such as using activated carbon, filtration, photocatalysis, adsorption and so on. Among these methods, activated carbon and filtration are only effective for those low-concentration wastewaters, so it is difficult for them t...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30C30B29/54C30B7/14C02F1/28C02F101/30
CPCB01J20/223C02F1/285C02F2101/308C30B7/14C30B29/54
Inventor 张金方龚林培吴俊洁冯姣阳张弛
Owner JIANGNAN UNIV
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