Preparation method of silver tetrafluoroborate

A technology of silver tetrafluoroborate and tetrafluoroborate, applied in tetrafluoroboric acid, boron halide compounds, etc., can solve problems such as high production cost, easy decomposition, contact with air, etc., and achieve production safety guarantees and mild reaction conditions. , the effect of low equipment requirements

Active Publication Date: 2022-01-21
SUZHOU SINOCOMPOUND TECH
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

This method of synthesizing silver fluoride and boron trifluoride gas in nitromethane not only has low yield, but also the main problem is safety and cost in large-scale production
[0004] First of all, the chemical properties of the precursors silver fluoride and boron trifluoride are unstable, highly toxic, easy to decompose when exposed to air or light, and even have the risk of explosion, especially in large-scale production, which is very easy to cause leakage, so the safety problem...

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  • Preparation method of silver tetrafluoroborate

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[0029] One embodiment of the present invention provides a method for preparing silver tetrafluoroborate, comprising the following steps: mixing and reacting a fluoroboric acid source and a silver salt in a reaction medium to obtain silver tetrafluoroborate.

[0030] Wherein, the fluoroboric acid source is selected from at least one of tetrafluoroborate and tetrafluoroboric acid; the reaction medium is a mixed solvent of the first organic solvent and water, or water, and the first organic solvent is selected from ether, nitromethane and at least one of toluene.

[0031] The present invention uses the above-mentioned fluoroboric acid source and silver salt as raw materials, and uses a specific type of mixed solvent of the first organic solvent and water as the reaction medium, so that the fluoroboric acid source and silver salt can be mixed to form a macroscopically homogeneous solution for ionization. Exchange and metathesis reaction occurs, and finally form silver tetrafluorob...

Embodiment 1

[0056] Dissolve 16.98 g of silver nitrate solid in 150 mL of ether to obtain an ether solution of silver nitrate.

[0057] Dissolve 10.58 g of ammonium tetrafluoroborate solid (molar ratio of silver nitrate to ammonium tetrafluoroborate: 1:1.01) in 25 mL of deionized water to obtain ammonium tetrafluoroborate aqueous solution.

[0058] Ammonium tetrafluoroborate aqueous solution was added dropwise to silver nitrate ether solution at room temperature, and stirred for 3 h until the reaction was completed. Filter the solid-liquid mixture obtained by the reaction, wash the filter cake with anhydrous diethyl ether, collect the filtrate, and spin-steam the obtained filtrate at room temperature for 1 h under weak light to remove ether, then continue to heat up to 90 ° C and spin-steam for 0.5 h to remove residual water, and obtain a white Crystal, that is, silver tetrafluoroborate crude product.

[0059] Dissolve the obtained silver tetrafluoroborate crude product in 30 mL of anhydr...

Embodiment 2

[0063] Dissolve 16.98 g of silver nitrate solid in 150 mL of water to obtain a silver nitrate solution.

[0064] Dissolve 10.58 g of ammonium tetrafluoroborate solid (molar ratio of silver nitrate to ammonium tetrafluoroborate: 1:1.01) in 25 mL of deionized water to obtain ammonium tetrafluoroborate aqueous solution.

[0065] Add the ammonium fluoroborate solution dropwise to the silver nitrate solution at room temperature in the dark, and stir for 0.5 h until the reaction is complete. Filter the solid-liquid mixture obtained from the reaction, wash the filter cake with 5 mL of deionized water, collect the filtrate and rotate it at 55 °C and -0.1 MPa pressure for 1 h under dark conditions, then at the same pressure at 75 °C for 1 h, and finally 90 °C for 1 h to remove the residual water by rotary evaporation to obtain white silver tetrafluoroborate crude product.

[0066] Dissolve the obtained silver tetrafluoroborate crude product in 30 mL of anhydrous ether, filter to remov...

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Abstract

The invention relates to a preparation method of silver tetrafluoroborate, which comprises the steps of mixing and reacting a fluoboric acid source and silver salt in a reaction medium to obtain the silver tetrafluoroborate, wherein the fluoboric acid source is selected from at least one of tetrafluoroborate and tetrafluoroboric acid; and the reaction medium is a mixed solvent of a first organic solvent and water or water, and the first organic solvent is selected from at least one of diethyl ether, nitromethane and methylbenzene. The preparation method is wide in raw material applicability, the raw materials are low in toxicity and easy to obtain, the problem that the toxicity is too high when silver fluoride and boron trifluoride serve as reaction raw materials is solved, the reaction can be carried out at the room temperature, the reaction condition is mild, the reaction is easy to operate, the needed time is short, the requirement for equipment is low, and the production safety problem is guaranteed.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of silver tetrafluoroborate. Background technique [0002] Silver tetrafluoroborate (AgBF 4 ) is a noble metal salt used to replace halide ions or ligands with a non-coordinating anion fluoroborate, and has a wide range of applications in metalorganic chemistry. However, the poor tolerance and harsh synthesis process of silver tetrafluoroborate limit its large-scale production. [0003] At present, the industrial production of silver fluoroborate adopts the silver fluoride method, that is, boron trifluoride gas is continuously injected into the silver fluoride / nitromethane dispersion, and the temperature is kept at 60°C until the solid silver fluoride is almost dissolved. , stop the introduction of boron trifluoride, and then pass through inert gas to purge and remove excess boron trifluoride to obtain a solution of silver fluoroborate in nitrome...

Claims

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Application Information

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IPC IPC(8): C01B35/06
CPCC01B35/063
Inventor 刘相禹倪自林张佳琪
Owner SUZHOU SINOCOMPOUND TECH
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