In the study, the epoxidation process
of soybean oil by microflow
system (MFS) was investigated. With formic acid as oxygen carrier
and EDTA-2Na as stabilizer, the optimal result (epoxidized soybean
oil (ESO) with an epoxy number (EN) of 7.3) was obtained in such conditions:
temperature 75 °C, H2SO4 concentration
3%, EDTA-2Na dosage 3%, residence time 6.7 min, ratio of formic acid
to hydrogen peroxide 1:1, and H2O2 to double
bond molar ratio 8:1.
During
the lactide producing process, volatile impurities, such
as lactic acid and its dimer, are simultaneously distilled out with
lactide. To remove these impurities, many post-treatments were needed.
Herein, we present a novel approach to obtain high purity lactide
by adding high-boiling-point alcohols to immobilize these volatile
impurities. A series of high-boiling-point alcohols were screened
and pentaerythritol was found to be the best immobilization reagent.
When the molar ratio of lactic acid’s carboxylic group and
pentaerythritol’s hydroxyl group was 15:1, lactide with 99%
GC purity was directly distilled out and no traces of lactic acid
and its dimer were detected. The results of HPLC-MS revealed that
the distillation residues were esters of pentaerythritol with lactic
acid or its oligomer. This indicated that volatile impurities were
immobilized in distillation residues. The distillation residues were
reused for 4 runs, and the purities of lactide were all over 98%.
Key indicatorsSingle-crystal X-ray study T = 293 K Mean (C-C) = 0.004 Å R factor = 0.061 wR factor = 0.192 Data-to-parameter ratio = 14.1 For details of how these key indicators were automatically derived from the article, see
Key indicators: single-crystal X-ray study; T = 298 K; mean (C-C) = 0.003 Å; R factor = 0.046; wR factor = 0.130; data-to-parameter ratio = 14.6.In the molecule of the title compound, C 9 H 8 ClNO 4 , an intramolecular C-HÁ Á ÁO hydrogen bond results in the formation of a planar five-membered ring, which is nearly coplanar with the adjacent six-membered ring, the rings being oriented at a dihedral angle of 4.40 (3) . In the crystal structure, intermolecular C-HÁ Á ÁO hydrogen bonds link the molecules.
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ExperimentalCrystal data
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