Process for preparing phenylacetic acid from impurity-containing phenylacetate solution without crystallization
A technology of phenylacetate and phenylacetic acid, which is applied in the preparation of carboxylate, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problem of low production efficiency of water recrystallization method, inconvenience in drying, storage and transportation, product Unstable quality and other problems, to achieve the effect of improving the production environment, easy to use, storage and transportation, and low cost
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Embodiment 1
[0024] Embodiment 1, a kind of process of preparing phenylacetic acid from devitrification-free phenylacetate solution containing impurities comprises the following steps:
[0025] (1) Dilution: Dilute the impurity-containing phenylacetate solution prepared by the alkaline hydrolysis process of phenylacetonitrile or the benzyl chloride carbonylation synthesis process with deionized water to a concentration not higher than 500g / l; the phenylacetate solution It is one or a mixed solution of sodium phenylacetate solution, potassium phenylacetate solution and ammonium phenylacetate solution;
[0026] (2) Decolorization: the diluted phenylacetate solution is adjusted to pH 8.5 with inorganic acid, the temperature is controlled at 10°C, and activated carbon is added to stir for 2.0 hours to decolorize, and then filtered; the inorganic acid is selected from sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid;
[0027] (3) Oxidation: adjust the pH value of the decoloriza...
Embodiment 2
[0032] Embodiment 2, a kind of process of preparing phenylacetic acid from devitrification-free phenylacetate solution containing impurities comprises the following steps:
[0033] (1) Dilution: Dilute the impurity-containing phenylacetate solution prepared by the alkaline hydrolysis process of phenylacetonitrile or the benzyl chloride carbonylation synthesis process with deionized water to a concentration not higher than 500g / l; the phenylacetate solution It is one or a mixed solution of sodium phenylacetate solution, potassium phenylacetate solution and ammonium phenylacetate solution;
[0034] (2) Decolorization: adjust the pH value of the diluted phenylacetate solution to 9.5 with inorganic acid, control the temperature at 60°C, add activated carbon and stir for 2.5 hours to decolorize, then filter; the inorganic acid is selected from sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid;
[0035] (3) Oxidation: adjust the pH value of the decolorized filtrate t...
Embodiment 3
[0040] Embodiment 3, a kind of process of preparing phenylacetic acid from devitrification-free phenylacetate solution containing impurities comprises the following steps:
[0041] (1) Dilution: Dilute the impurity-containing phenylacetate solution prepared by the alkaline hydrolysis process of phenylacetonitrile or the benzyl chloride carbonylation synthesis process with deionized water to a concentration not higher than 500g / l; the phenylacetate solution It is one or a mixed solution of sodium phenylacetate solution, potassium phenylacetate solution and ammonium phenylacetate solution;
[0042] (2) Decolorization: the diluted phenylacetate solution is adjusted to pH 9.0 with inorganic acid, the temperature is controlled at 30°C, and activated carbon is added to stir for 2.2 hours to decolorize, and then filtered; the inorganic acid is selected from sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid;
[0043](3) Oxidation: adjust the pH value of the decolorized...
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