Processing method of 13C urea

Processing method of 13C urea

  • CN 106,631,905 A
  • Filed: 12/29/2016
  • Published: 05/10/2017
  • Est. Priority Date: 12/29/2016
  • Status: Active Application
First Claim
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1. a kind of13C urea processing methods, it is characterised in that:

  • Comprise the following steps:

    Synthesis:

    S1. sulphur 100-120 parts are added in reactor;

    S2. vavuum pump is opened, by reaction kettle for vacuumizing, vacuum is 0.8-0.97;

    S3. alcohols 900-1300 parts are added in reactor;

    S4. hydrogen sulfide gas 7-12 parts, 15-22 parts nitrogen and 180-240 parts ammonia are passed through into reactor or sulfuration is passed throughHydrogen 7-12 parts and 180-240 part ammonias;

    S5. add in reactor13CO gas 40-60 parts, while heating to reactor, improve temperature to 70-90 DEG C,Reaction 0.5-2 hours, reaction terminates;

    S6. stop heating response kettle, be cooled to 20-40 DEG C;

    Distillation:

    S7. the reactant that Jing steps S6 are obtained is sent in distillation still, is heated to 20-40 DEG C, carry out vacuum distillation, consolidateState mixture;

    It is refined:

    S8. the solid mixt for Jing steps S7 being obtained is sent into reactor, adds water, activated carbon, heating-up temperature to 58-75DEG C, stirring mixing 100-150 minutes, decompression suction filtration obtains supernatant liquid;

    S9. the supernatant liquid that Jing steps S8 obtained is sent into reactor, is vacuumized, and vacuum is 0.8-0.97, heating responseKettle to temperature is 55-65 DEG C, heats 30-45 minutes, evaporation section moisture;

    Recrystallization:

    S10. close heating system, open cooling system, chilled liquid temperature to subzero 12-2 DEG C, cool time 2-5 hour,13C urea crystallizations;

    It is dried:

    The crystal of the urea that S11. Jing steps S10 are obtained is separated with mother liquor by way of suction filtration, and urea crystal is putIn putting vacuum dryer, it is vacuum dried under conditions of vacuum 0.8-0.97, temperature 55-65 DEG C, is obtained qualified'"'"'s13C urea.

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