Method for simultaneously preparing pyromellitic acid and terephthalic acid with coal serving as raw material

Method for simultaneously preparing pyromellitic acid and terephthalic acid with coal serving as raw material

  • CN 102,816,061 A
  • Filed: 09/05/2012
  • Published: 12/12/2012
  • Est. Priority Date: 09/05/2012
  • Status: Active Application
First Claim
Patent Images

1. one kind is that raw material prepares Pyromellitic Acid and method of terephthalic acid simultaneously with the coal, it is characterized in that,At first in autoclave, add Pottasium Hydroxide, coal sample and zero(ppm) water, oxygenation pressure to 1.0~

  • 10.0Mpa carries out alkali oxygen oxidizing reaction, the weight ratio 1;

    10 of Pottasium Hydroxide and coal sample~

    10;

    1 wherein, and temperature of reaction is 100 ℃



    400 ℃

    , the reaction times is 0.5 ~ 5h;

    The add-on of zero(ppm) water be Pottasium Hydroxide and coal sample gross weight 1%~

    300%;

    The reaction postcooling takes out oxygenated products, filters out undissolved residue, and filtrating is acidified to pH=2~

    5 with the vitriol oil;

    Filter and divide water outlet immiscible acid deposition;

    The filtrating of removing the water immiscible acid is acidified to pH=1~

    3 with the vitriol oil again, makes water-soluble acid free fully, and the solution after the processing extracts with butanone;

    Extraction liquid reclaims butanone through vacuum-evaporation;

    Enriched material obtains water-soluble acid again through vacuum-drying, and decarboxylation makes Pyromellitic Acid through selectivity in the blending agent of sulfuric acid, sal enixum and zero(ppm) water with water-soluble acid again;

    To produce remaining coal acid and catalyzer adding reaction kettle behind the Pyromellitic Acid, use CO 2Air in the displacement still is again with CO 2Charge into reaction kettle to 1.0~

    10.0Mpa and carry out the sour constant temperature isomerization reaction of coal, the temperature of reaction is 100 ℃



    400 ℃

    , and the reaction times is 1 ~ 5h, after reaction finishes;

    Take out reaction kettle, the water Quench is again with heat filtering after the reaction product heated and boiled, after filter residue is repeatedly washed;

    Oven dry is weighed, and filtrating is mixed with water lotion, and the cooling back adds the gac boiling decoloring with Hydrogen chloride adjustment pH value to 5~

    8;

    Heat filtering, filtrating cooling back is with Hydrogen chloride adjustment its pH=2~

    5, and terephthalic acid is separated out with precipitation forms;

    Filter, flushing promptly obtains the pure terephthalic acid after the oven dry.

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