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Preparation method of tetrakis (acetyl nitrile) silver tetrafluoroborate

A technology of silver tetrafluoroborate and acetonitrile is applied in the preparation of carboxylic acid nitrile, the preparation of organic compounds, chemical instruments and methods, etc., and can solve the problems of many impurities, high post-processing cost, and many steps.

Active Publication Date: 2022-07-29
JIANGSU SINOCOMPOUND CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In the above-mentioned preparation methods of silver tetrakis(acetonitrile)tetrafluoroborate, there are many steps and many impurities produced by the reaction, resulting in high post-processing cost, and the prepared silver tetrakis(acetonitrile)tetrafluoroborate is not easy to store, which is extremely difficult to store. It is easy to turn black and deteriorate, which is not conducive to large-scale industrial production

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  • Preparation method of tetrakis (acetyl nitrile) silver tetrafluoroborate

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[0035] The invention provides a preparation method of tetrakis (acetonitrile) silver tetrafluoroborate, comprising the following steps:

[0036] Silver nitrate and acetonitrile are mixed and dissolved to prepare a first reaction solution;

[0037] The first reaction solution is mixed and reacted with ammonium fluoroborate to prepare the tetrakis(acetonitrile)silver tetrafluoroborate.

[0038] In one specific example, the ratio of the silver nitrate to acetonitrile is 50g:(300~550)mL. Specifically, the ratio (g:mL) of silver nitrate to acetonitrile includes but is not limited to: 50g:300mL, 50g:350mL, 50g:400mL, 50g:450mL, 50g:500mL, 50g:550mL. Further, the ratio of described silver nitrate and acetonitrile is 50g:(300~400)mL.

[0039] In one specific example, the molar ratio of the silver nitrate to the ammonium fluoroborate is 1:(1.2~1.4). Specifically, the molar ratio of silver nitrate to ammonium fluoroborate includes but is not limited to: 1:1.2, 1:1.25, 1:1.3, 1:1.35, ...

Embodiment 1

[0050] The present embodiment is a preparation method of tetrakis (acetonitrile) silver tetrafluoroborate, and the steps are as follows:

[0051] (1) Add 62.6g silver nitrate into a 500mL single-neck flask, add 300mL acetonitrile and stir to dissolve;

[0052] (2) Add ammonium fluoroborate (silver nitrate: ammonium fluoroborate molar ratio = 1:1.2) and continue to stir the reaction, the water bath is heated to 60 °C, and the reaction is performed for 4 hours;

[0053] (3) After the solution after the reaction is filtered twice with a filter membrane (pore size is 0.2 μm), the filtrate is rotary-evaporated at a temperature of 50 °C, and the filtrate is rotary-evaporated to about the theoretical product weight. In a viscous state, some silver nitrate remains;

[0054] (4) Dissolve the product of step (3) in a saturated solution of 300 mL of ammonium fluoroborate-acetonitrile, and a white precipitate (ammonium nitrate) is produced. Add 10 g of ammonium fluoroborate to the mixed ...

Embodiment 2

[0056] The present embodiment is a kind of preparation method of tetrakis (acetonitrile) silver tetrafluoroborate, and the main difference with embodiment 1 is: increase the feeding amount of acetonitrile and ammonium fluoroborate, wherein the feeding amount of acetonitrile is 400mL, silver nitrate: fluorine The molar ratio of ammonium borate=1:1.4; prolong the reaction time to 6h.

[0057] Specific steps are as follows:

[0058] (1) Add 62.6g silver nitrate into a 500mL single-neck flask, add 400mL acetonitrile and stir to dissolve;

[0059] (2) Add ammonium fluoroborate (silver nitrate: ammonium fluoroborate molar ratio = 1:1.4) and continue to stir the reaction, the water bath is heated to 60 ℃, and the reaction is performed for 6 hours;

[0060] (3) After the solution after the reaction is filtered twice with a filter membrane (pore size is 0.2 μm), the filtrate is rotary-evaporated at a rotary evaporation temperature of 50°C, and the filtrate is rotary-evaporated to abou...

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Abstract

The invention relates to a preparation method of tetrakis (acetyl nitrile) silver tetrafluoroborate, which comprises the following steps: mixing and dissolving silver nitrate and acetonitrile to prepare a first reaction solution; and mixing the first reaction solution with ammonium fluoroborate for reaction to prepare the tetrakis (acetylacetonitrile) silver tetrafluoroborate. According to the preparation method of tetrakis (acetylacetonitrile) silver tetrafluoroborate provided by the invention, proper silver salt and fluoroborate are selected as raw materials, and acetonitrile, which is one of the reaction raw materials, is directly used as a reaction solvent, so that the tetrakis (acetylacetonitrile) silver tetrafluoroborate prepared by the method has few impurities, and the tetrakis (acetylacetonitrile) silver tetrafluoroborate has excellent storage stability through test verification; deterioration is avoided after long-time storage. Meanwhile, the preparation method also realizes maximization of reaction atom economy, meets the requirements of sustainable development of the modern society, is simple to operate and low in production cost, and has a great industrial application prospect.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of tetrakis(acetonitrile) silver tetrafluoroborate. Background technique [0002] Silver, as one of transition metals, is abundant in nature. The physical and chemical properties of silver are relatively stable, the thermal conductivity and electrical conductivity are good, soft, ductile, and the reflectivity is extremely high, reaching more than 99%. It is widely used, especially in the field of metal complexes. It plays an important role. Since Ag(I) is a well-coordinated ion with organic ligands, it can form complexes with unique structures, and its unique structure is also the reason why silver ligand compounds are one of the important intermediates. [0003] Metal-butyronitrile complexes were among the first coordination compounds to be thoroughly studied by synthetic chemists and spectroscopists. Nonaqueous solvated transition metal cations...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/03
CPCC07C253/30C07C255/03
Inventor 马家豪袁庆庆倪自林
Owner JIANGSU SINOCOMPOUND CATALYST
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