FIELD: chemistry.
SUBSTANCE: invention relates to a method for processing of high-boiling by-products of trimethylolpropane production process by condensation of n-butyraldehide with formaldehyde. Di-TMP with a purity of 98 wt % or higher is recovered by successive crystallisation of bottom products of raw TMP vacuum distillation, first using ethyl acetate at a mass ratio of 1:1-1.5, then using acetone at a mass ratio of 1:2-5. Formal-rich and oily di-TMP combined residue, unsuitable for the recovery of 98 wt % or higher di-TMP, is converted into TMP and di-TMP esters by esterification process, using C1-C18 carboxylic acid or a mixture of acids in the presence of 0.05-20.0 wt % of acid catalyst at a temperature of 70-250°C. The resulting esters are separated from the traces of carboxylic acid and acid catalyst. The produced in the process water, formaldehyde and methanol are removed from the reaction mix as their azeotropes with hydrocarbons or as a vapour phase.
EFFECT: improved efficiency and completeness of processing of high-boiling by-products, remaining in the bottoms of raw TMP vacuum distillation; as a result, produced a number of sought after industrial substances, reducing thereby the total amount of process waste.
3 cl, 2 tbl, 15 ex
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Authors
Dates
2017-04-12—Published
2016-03-10—Filed