Tetraethyl tetrafluo ammonium fluoroborate preparation method

Tetraethyl tetrafluo ammonium fluoroborate preparation method

  • CN 1,762,979 B
  • Filed: 09/26/2005
  • Issued: 10/10/2012
  • Est. Priority Date: 09/26/2005
  • Status: Active Grant
First Claim
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1. the preparation method of a tetraethyl-ammonium tetrafluoroborate is characterized in that:

  • (1) boric acid is refining;

    Industrial boric acid is dissolved in the deionized water that boils, filters then, filtrating is reduced to room temperature, crystallization;

    Filter, and wash, then filter cake is dissolved in the deionized water that boils again with deionized water;

    Cooling, crystallization, the triplicate recrystallization process obtains purity and is 99.8% refining boric acid;

    (2) preparation of fluoroboric acid;

    Take by weighing concentration and be 40% hydrofluoric acid and add in the reactor drum that gathers tetrafluoro material or band corrosion-proof lining that has stirring, condensation reflux unit and spiral coil cooling tube, add boric acid while stirring in batches, temperature of reaction is 30~

    40 ℃

    ;

    Finish after the boric acid;

    Continue to stir half a hour, at room temperature left standstill then 2 hours, filter, remove insolubles impurity;

    Promptly get the fluoborate aqueous solution of 33% ±

    1 concentration, hydrofluoric acid, boric acid consumption are 1;

    1 in molar ratio;

    (3) preparation of tetraethyl-ammonium tetrafluoroborate;

    The preparation of tetraethyl-ammonium tetrafluoroborate is in gathering tetrafluoro material reactor drum, to carry out, and 1;

    2 ratio adds tetraethyl-ammonium halide crystal and alcohol organic solvent at first by weight, in 10~

    50 ℃

    ;

    Slowly drip fluoborate aqueous solution, fluoborate aqueous solution and tetraethyl-ammonium halide crystalline consumption be by weight being 1;

    1, finish fluoroboric acid after;

    Continue reaction 2 hours, then, concentrating under reduced pressure;

    30~

    90 ℃

    of temperature controls, after reaction finished, the alcohol organic solvent of adding and tetraethyl-ammonium halide crystal equal weight stirred and carried out crystallization in 2 hours again;

    Crystallization liquid is through filtering;

    And use the alcohol organic solvent washing leaching cake, remove the mother liquor that has impurity, the wet-milling that obtains-tetraethyl-ammonium tetrafluoroborate crystal bullion;

    (4) the tetraethyl-ammonium tetrafluoroborate is refining;

    In having the container of condensation reflux unit, add ethanolic soln, add the tetraethyl-Tetrafluoroboric acid ammonium salt wet-milling through the alcohol solvent washing simultaneously, intensification is boiled;

    After treating that solid all dissolves;

    Be cooled to room temperature while stirring, and at room temperature carry out crystallization, filtration, and wash with the ethanolic soln under the room temperature;

    Twice of repeated recrystallization process;

    The crystal that obtains carries out drying in 40~

    80 ℃

    under vacuum condition, promptly get purified tetraethyl-ammonium tetrafluoroborate, wherein purified tetraethyl-ammonium tetrafluoroborate purity;

    >

    =99.5%;

    Water-content≤

    10ppm;

    Fe≤

    1.0ppm;

    Si≤

    3.0ppm;

    Na≤

    3.0ppm;

    K≤

    3.0ppm.

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