Method for preparing triethyl citrate through using nanometer intercalated hydrotalcite catalyst
A technology of triethyl citrate and hydrotalcite, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problems of environmental pollution of waste acid, difficulty in post-treatment, carbonization of organic matter, etc. The product has high purity, saves the removal of miscellaneous processes, and is not easy to run off.
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Embodiment 1
[0024] Embodiment 1: a kind of method that nanoscale intercalation hydrotalcite catalyst prepares triethyl citrate comprises the steps:
[0025] Step a, feeding: Add nano-scale intercalated hydrotalcite catalyst, citric acid, and excess ethanol into the container, and stir evenly; when feeding, the molar ratio of citric acid to ethanol is 1: (5-6); citric acid and nano-scale The mass ratio of the intercalated hydrotalcite catalyst is 1: (0.03~0.05);
[0026] Step b. Esterification reaction: heating in an oil bath to maintain the reaction temperature between 100-110°C; during the heating process, continuously add ethanol dropwise until the ethanol is excessive, and at the same time condense and reflux to collect and evaporate ethanol; the esterification reaction time is 16-20 hours ;
[0027] Step c, purification: After the esterification reaction is completed, filter the nano-scale intercalated hydrotalcite catalyst, extract the residual ethanol in the reaction vessel from th...
Embodiment 2
[0029] Embodiment 2: The difference between this embodiment and Embodiment 1 is that in this embodiment, the nano-scale intercalated hydrotalcite catalyst is a kind of magnesium-aluminum hydrotalcite and zinc-aluminum hydrotalcite intercalated with multiple acids, The chemical formula of the anion of the polyacid used is [XM 11 CoO 39 ] n- , where X=P or Si; M=W or Mo; n is the valence number, n=5-6.
Embodiment 3
[0030] Embodiment 3: a kind of nanoscale intercalation hydrotalcite catalyst prepares the method for triethyl citrate, comprises the steps:
[0031] Step a, feeding: Add nano-scale intercalation hydrotalcite catalyst, citric acid, and excess ethanol into the container, and stir evenly; when feeding, the molar ratio of citric acid to ethanol is 1:5; citric acid and nano-scale intercalation hydrotalcite The mass ratio of the catalyst is 1:0.03;
[0032] Step b. Esterification reaction: heating in an oil bath to maintain the reaction temperature between 100-105°C; during the heating process, continuously add ethanol dropwise until the ethanol is excessive, and at the same time condense and reflux to collect and evaporate ethanol; the esterification reaction time is 15-18 hours ;
[0033]Step c, purification: After the esterification reaction is completed, filter the nano-scale intercalated hydrotalcite catalyst, extract the residual ethanol in the reaction vessel from the filtra...
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