Method for extracting and purifying hydroxy-acetic acid by ester solvents
A technology of glycolic acid and ester solvents, which is applied in the field of ester solvent extraction and purification of glycolic acid and extraction of glycolic acid, can solve the problems of high viscosity, little industrial prospect, and difficult phase separation, and achieve easy recovery and reuse, high Theoretical and practical value, cost reduction effect
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Embodiment 1
[0017] Example 1: In a three-neck flask equipped with a stirrer, a thermometer and a condenser tube, add a solution of 92mL of 95% to 98% sulfuric acid and 60mL of water, start stirring, and heat the flask with an external oil bath. When it reaches 100°C, add 300mL of 50% hydroxyacetonitrile dropwise to produce a strong hydrolysis reaction, control the reaction temperature at 115-120°C, and boil and reflux for 6 hours to obtain a hydrolyzate. The conversion rate of hydroxyacetonitrile was determined to be 99.3%. Add 1g of activated carbon for decolorization, stop heating, filter while hot, and filter out the activated carbon. Adjust the pH value of the hydrolyzate to 0.5-2.0 by using ammonium bicarbonate or ammonia water in the filtrate. Cool to room temperature, and salt out. Filtrate and desalt to obtain a glycolic acid aqueous solution containing inorganic acids and salts, adjust and control the glycolic acid content in the hydrolyzed solution with water.
Embodiment 2
[0018] Embodiment 2: prepare glycolic acid aqueous solution according to embodiment 1, extraction hydrolyzate is water phase (W), pH value 0.5, glycolic acid content: 600g / L, ethyl acetate (O) is oil phase, adopts intermittent stirring extraction. In a three-neck flask equipped with a stirrer, a thermometer and a condenser tube, add 25mL of hydrolyzate and 25mL of ethyl acetate, control the extraction temperature, stir, and make the extractant ethyl acetate and glycolic acid mixed aqueous solution contact. Comparison: O / W=1, extraction temperature=10°C, extraction time=10min. After phase separation, the organic phase was distilled under reduced pressure at a heating temperature of 45°C to obtain white solid glycolic acid. Once extracted, the yield of glycolic acid was 6%.
Embodiment 3
[0019] Embodiment 3: Prepare glycolic acid aqueous solution according to embodiment 1, pH value is 1.0, glycolic acid content: 600g / L. Using the same device as in Example 2 for extraction, comparison: O / W=3, extraction temperature=35°C, extraction time=10min. After phase separation, the organic phase was distilled under reduced pressure at a heating temperature of 45°C to obtain white solid glycolic acid. Once extracted, the yield of glycolic acid was 24%.
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