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Preparation method for alkali type copper fluoride

A copper fluoride, basic technology, applied in the direction of copper halide, etc., can solve the problems of complicated preparation steps, difficult separation and purification, harsh temperature, etc., and achieve the effect of simple separation and purification, cheap and easy-to-obtain raw materials, and mild reaction conditions

Active Publication Date: 2013-09-04
徐州宏阳新材料科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation steps of this method are complicated, the temperature is harsh (100-230°C), and the time is long (it takes several days). In addition, special anti-corrosion containers are required due to the use of highly toxic and dangerous hydrogen fluoride reagents; in addition, in the preparation process Cu 3 (OH) 2 f 4 Difficulty in separation and purification

Method used

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  • Preparation method for alkali type copper fluoride
  • Preparation method for alkali type copper fluoride
  • Preparation method for alkali type copper fluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Cu powder (64mg, 1mmol), 1-chloromethyl-4-fluoro-1,4-diazabicyclo[2.2.2]octane di(tetrafluoroborate) salt (Selectfluor, 354.3mg, 1mmol), Add it to a 200mL round bottom flask, and then add 10mL of acetonitrile / water (V:V=50:1) as a solvent. Then, magnetically stirred at room temperature for 1 h to obtain a light blue solution and a white precipitate. Filter to remove the white precipitate, concentrate the mother liquor, and precipitate 75 mg of basic copper fluoride, with a yield of 75%.

[0024] Characterization data of FCuOH: IR:ν3150(OH)cm -1 ; 19 F NMR (376MHz, CD 3 CN):δ-151.06ppm;ESI-MS:m / z:80[M-F] + .

Embodiment 2

[0026] Add Cu powder (64mg, 1mmol), 1-chloromethyl-4-fluoro-1,4-diazabicyclo[2.2.2]octane di(hexafluorophosphate) salt (470.6mg, 1mmol), into In a 200mL round bottom flask, add 10mL of acetonitrile / water (V:V=50:1) as a solvent. Then, magnetically stirred at room temperature for 1 h to obtain a light blue solution and a white precipitate. Filter to remove the white precipitate, concentrate the mother liquor, and precipitate 74 mg of basic copper fluoride, with a yield of 74%.

Embodiment 3

[0028] Cu powder (64mg, 1mmol), 1-chloromethyl-4-fluoro-1,4-diazabicyclo[2.2.2]octane di(trifluoromethanesulfonic acid) salt (478.8mg, 1mmol), Add it to a 200mL round bottom flask, and then add 10mL of acetonitrile / water (V:V=50:1) as a solvent. Then, magnetically stirred at room temperature for 1 h to obtain a light blue solution and a white precipitate. Filter to remove the white precipitate, concentrate the mother liquor, and precipitate 72 mg of basic copper fluoride, with a yield of 72%.

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Abstract

The invention provides a preparation method for alkali type copper fluoride, which is characterized in that copper powder, 1-Chloromethyl-4-fluoro-1 and 4 - dinitrogen mixed double loop (2.2.2) octane salt are mixed according to the molar ratio ranging from 1to 1 to 1to2, and then, under the action of a mixed solution of organic solution and water, carrying out reaction for 5 to 24 hours at a temperature of 20 DEG C to 100 DEG C, after that filtering and removing the white precipitate, so as to obtain the copper fluoride by concentrating the mother liquor. The synthetic method provided by the invention has the advantages that the raw material is low in cost and east to obtain, the operation is simple and safe, the synthetic step is short, and the depuration is simple.

Description

(1) Technical field [0001] The invention relates to a preparation method of basic copper fluoride, which belongs to the technical field of catalysts. (2) Background technology [0002] Copper-based catalysts have been widely used in both homogeneous and heterogeneous catalysis due to their high activity, high selectivity, low cost and low toxicity. In addition, many copper-containing reagents can be used in feed additives. For example, basic copper chloride is a good feed additive. High, less environmental pollution and other advantages. [0003] Although the preparation and application of basic copper chloride have been widely reported, there are few reports on the preparation and application of its analog basic copper fluoride. The main reason may be that there is no easy preparation method. Literature (Berzelius, J.J., Pogg. Ann., 1824, 1, 27; or Hayek, Z.; Inama, P.; Schatz, B., Monatschefte für Chemie, Bd., 1963, 94(5), 799) It is reported that basic copper fluoride...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G3/04
Inventor 刘运奎张文霞张剑徐振元
Owner 徐州宏阳新材料科技股份有限公司
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