Method for preparing glyphosate by catalyzing and oxidizing glyphosine in the presence of ultraviolet light source

Method for preparing glyphosate by catalyzing and oxidizing glyphosine in the presence of ultraviolet light source

  • CN 102,229,621 B
  • Filed: 05/07/2011
  • Issued: 10/02/2013
  • Est. Priority Date: 05/07/2011
  • Status: Active Grant
First Claim
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1. there is the method for preparing glyphosate by PMIDA catalytic oxidation down in a ultraviolet source, it is characterized in that present method comprises following steps:

  • A) with pmida98 and self-control load type active carbon catalyst mix in aqueous phase is injected with the reactor of ultraviolet source irradiation, the mass ratio of pmida98, self-control supported active Pd/carbon catalyst and water is (8-20);

    (1-4);

    (50-100), at pressure 0.5-1.2Mpa, temperature 50-90 ℃

    of logical oxygen rich gas oxidation down;

    B) self-control supported active Pd/carbon catalyst prepares by the following method in the step a);

    load M activity of such catalysts charcoal, be characterized as this active constituent that loads on activated-carbon catalyst for containing nano level noble metal M oxide compound, wherein M is titanium, be that benchmark calculates with the titanium, the weight ratio of gac and titanium is 110;

    (0.1~

    15), the specific surface area of raw material gac is 800~

    1500m/g, total hole volume is 0.5~

    1.5mL/g, adopt the preparation of following method;

    the raw material gac is added contain in the nano level M metallic compound aqueous solution in 90~

    150 ℃

    of dipping heat treated, dipping time is 18~

    25h;

    The charcoal material of dipping is drained temperature drying below 180 ℃

    ;

    Dry charcoal material is put into calcining furnace calcine under oxygen-free environment, calcining temperature is 200~

    500 ℃

    , and calcination time is 8~

    15h;

    C) react logical a certain amount of ammonia in the mixed solution that obtains after the end to step a), fully stir and make that system pH is 4-4.5;

    D) mixed solution filtration step c) gets ammonification liquid and activated-carbon catalyst, collects activated-carbon catalyst and applies mechanically to step a);

    E) drip the vitriol oil in the ammonification liquid that obtains to step d), the control rate of addition makes system temperature be no more than 40 ℃

    , stops to drip the vitriol oil when dropping to system pH for 1.0-1.8, filters by two-stage cooling sufficient crystallising, gets the solid glyphosate crystal;

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