Method for synthesizing hafnium tetra-tert-butoxide

Method for synthesizing hafnium tetra-tert-butoxide

  • CN 102,351,891 A
  • Filed: 08/31/2011
  • Published: 02/15/2012
  • Est. Priority Date: 08/31/2011
  • Status: Active Grant
First Claim
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1. the synthesis method of four tert.-butoxy hafniums is characterized in that step is:

  • (1) under nitrogen atmosphere, the ratio in adding 100~

    400 ml n-hexanes in per 50 gram potassium tert.-butoxides adds potassium tert.-butoxide and normal hexane in the three-necked bottle, stir;

    (2) by hafnium tetrachloride;

    potassium tert.-butoxide is the mol ratio of 1;

    4.4 ~ 1;

    4.8, and hafnium tetrachloride is joined in the above-mentioned reaction system, and the temperature that keeps reaction system is between 20 to 60 ℃

    ;

    After adding hafnium tetrachloride, allow the temperature of reaction system remain between 40-65 ℃

    , under the condition of protection of inert gas stirring reaction 6-10 hour;

    (3) remove the solvent of reaction then under normal atmosphere, after the equal solvent normal hexane was all removed, the cut of 90-92 ℃

    /5 mmHg was collected in underpressure distillation, is four tert.-butoxy hafnium compounds.

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