Purifying process for high-quality glycolic acid
A glycolic acid, high-quality technology, applied in the separation/purification of carboxylic acid compounds, the preparation of carboxylate, the preparation of organic compounds, etc., to achieve the effects of improving production efficiency, overcoming complex processes, and high purification efficiency
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Embodiment 1
[0040] A purification process for high-quality glycolic acid:
[0041] (1) The low-purity glycolic acid mixed solution obtained by the hydrolysis of chloroacetic acid was reacted for 4 hours under a complex titanium catalyst, 170° C., and a vacuum of 10 mmHg to prepare glycolic acid oligomers;
[0042] (2) According to the molar ratio of glycolic acid and methanol corresponding to the glycolic acid oligomers as a feed ratio of 1:1.1, the alcoholysis reaction was carried out under a zinc oxide catalyst, 120° C., and 0.65 MPa for 6 hours to prepare a methyl glycolate mixture;
[0043](3) Utilizing the difference in boiling point of each component, the methyl glycolate is rectified and purified, and excess methanol is returned to participate in the alcoholysis reaction;
[0044] (4) According to the feed ratio of 1:1.2, a small amount of glycolic acid is added to the purified methyl glycolate and water as a catalyst, and a high-purity product with a purity of 99.6% is obtained th...
Embodiment 2
[0046] A purification process for high-quality glycolic acid:
[0047] (1) The low-purity glycolic acid mixed solution obtained by the hydrolysis of chloroacetic acid was reacted for 3 hours under a complex titanium catalyst, 185° C., and a vacuum degree of 20 mmHg to prepare glycolic acid oligomers;
[0048] (2) According to the molar ratio of glycolic acid and methanol corresponding to the polyglycolic acid oligomer as a feed ratio of 1:1.8, the alcoholysis reaction was carried out under a magnesium oxide catalyst, 135° C., and 0.96 MPa for 5 hours to prepare a methyl glycolate mixture;
[0049] (3) Utilizing the difference in boiling point of each component, the methyl glycolate is rectified and purified, and excess methanol is returned to participate in the alcoholysis reaction;
[0050] (4) According to the feed ratio of 1:3, a small amount of glycolic acid is added to the purified methyl glycolate and water as a catalyst, and a high-purity product with a purity of 99.6% ...
Embodiment 3
[0052] A purification process for high-quality glycolic acid:
[0053] (1) The low-purity glycolic acid mixed solution obtained by the hydrolysis of hydroxyacetonitrile was reacted for 2 hours under a complex titanium catalyst, 200° C., and a vacuum of 30 mmHg to prepare glycolic acid oligomers;
[0054] (2) According to the molar ratio of glycolic acid and methanol corresponding to the polyglycolic acid oligomer as a feed ratio of 1:2.5, the alcoholysis reaction was carried out at 150° C. and 1.8 MPa for 4 hours to prepare a methyl glycolate mixture;
[0055] (3) Utilizing the difference in boiling point of each component, the methyl glycolate is rectified and purified, and excess methanol is returned to participate in the alcoholysis reaction;
[0056] (4) According to the feed ratio of 1:5, a small amount of glycolic acid is added to the purified methyl glycolate and water as a catalyst, and a high-purity product with a purity of 99.7% is obtained through a vacuum hydrolysi...
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