A kind of preparation and purification method of trimethylolpropane fatty acid three ester

A kind of preparation and purification method of trimethylolpropane fatty acid three ester

  • CN 102,531,891 B
  • Filed: 01/04/2012
  • Issued: 01/20/2016
  • Est. Priority Date: 01/04/2012
  • Status: Active Grant
First Claim
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1. a preparation and purification method for trimethylolpropane fatty acid three ester, is characterized in that comprising following operation steps:

  • (1) synthesis of trimethylolpropane fatty acid three ester;

    with fatty acid methyl ester and TriMethylolPropane(TMP) for raw material, add basic catalyst, carry out transesterification reaction under vacuum, control the temperature of cooling water in reflux exchanger, the methyl alcohol that transesterify is generated is taken away by vacuum, TriMethylolPropane(TMP) condensing reflux, obtains transesterification reaction mixture;

    The time of described transesterification reaction is 60min, and temperature of reaction is 128 DEG C, and reaction pressure is 300Pa;

    (2) neutralization of reaction solution and washing;

    add phosphoric acid solution in step (1) gained transesterification reaction mixture, neutralization reaction removing basic catalyst;

    After reaction terminates, stratification, washes upper strata oil reservoir deionized water, then by standing separation, obtains oil reservoir and water layer;

    (3) purifying of trimethylolpropane fatty acid three ester;

    step (2) gained oil reservoir is dehydrated under vacuo, by the method for wiped film molecular distillation, gained heavy phase is the trimethylolpropane fatty acid three ester product of purifying, the fatty acid methyl ester of gained gently mutually for reclaiming;

    In step (1) described raw material, the mol ratio of fatty acid methyl ester and TriMethylolPropane(TMP) is 4;

    1;

    The mol ratio of described basic catalyst and TriMethylolPropane(TMP) is 0.10;

    1;

    Described basic catalyst is salt of wormwood;

    The temperature of the water coolant in described reflux exchanger is 30 DEG C;

    Described fatty acid methyl ester is palm oil fatty acid methyl esters;

    The addition of step (2) described phosphoric acid solution is 10% of transesterification reaction mixture weight, the absolute addition of phosphoric acid in and theoretical phosphoric acid amount needed for basic catalyst 90%;

    Described neutralization reaction temperature is 80 DEG C, and the reaction times is 30min;

    The time of described stratification is 40min;

    The deionized water that described deionized water washing adopts is 20% of upper strata oil reservoir weight, and described washing temperature is 80 DEG C, and washing time is 40min;

    The time of described standing separation is 60min;

    The temperature that step (3) described oil reservoir dehydrates under vacuo is 60 ~ 90 DEG C, and the time is 30min, and vacuum tightness is 2000Pa;

    The distillation temperature of described wiped film molecular distillation is 110 DEG C, and pressure is 1.0Pa.

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