A kind of preparation method of tannic acid ether stearate
A technology of stearic acid ester and tannic acid ether, applied in the field of preparation of tannic acid ether stearic acid, can solve the problem that the excellent properties of tannic acid cannot be efficiently utilized, affect the yield, and cannot be directly used for food Medium problems with oil or makeup
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[0022] Concrete preparation method steps are as follows:
[0023] (1) Synthesis of intermediate product of chlorotannic acid ethyl ether
[0024] Mix 20ml of paraldehyde with 2g of tannic acid, put it in an ice-salt bath at 0°C to cool, wait until the temperature drops to about 0°C, pass in dry hydrogen chloride gas, control the flow rate of hydrogen chloride gas, and react at 0°C for 4~ 6h, stop the flow of hydrogen chloride gas, let it stand still, take the upper layer liquid, dry it with anhydrous calcium chloride, separate it, distill it under reduced pressure, collect the intermediate product of chlorotannic acid ethyl ether, and obtain 10-15ml.
[0025] (2) Synthesis of tannic acid ether stearate
[0026] Dissolve sodium stearate in 20ml anhydrous organic solvent, add phase transfer catalyst FeCl 3 And polyethylene glycol-400 (PEG-400) mixture at a temperature of 20 ~ 30 ℃, slowly dropwise add the chlorotannic acid ethyl ether prepared above. Raise the temperature to ...
Embodiment 1
[0041]Mix 20ml of paraldehyde with 2g of tannic acid, cool in an ice-salt bath at 0°C, and when the temperature drops to about 0°C, pass in dry hydrogen chloride gas, control the flow rate of hydrogen chloride gas, and react at 0°C for 6 hours. Stop flowing the hydrogen chloride gas, let it stand still, take the upper layer liquid, dry it with anhydrous calcium chloride, separate it, and distill it under reduced pressure to collect the intermediate product of chlorotannic acid ethyl ether to obtain 14ml.
[0042] Dissolve 4.22g sodium stearate in 20ml toluene, add phase transfer catalyst FeCl 3 - PEG-400 (0.045g FeCl 3 Mix with 0.344ml polyethylene glycol-400), at a temperature of 30°C, slowly add the above-prepared chlorotannic acid ethyl ether dropwise. Raise the temperature to 100°C, reflux for 6h, cool to room temperature, and filter with suction to obtain a crude product.
[0043] The crude product was washed with ether, the filter residue was collected, ether and tolue...
Embodiment 2
[0045] Mix 20ml of paraldehyde with 2g of tannic acid, cool in an ice-salt bath at 0°C, wait until the temperature drops to about 0°C, pass in dry hydrogen chloride gas, control the flow rate of hydrogen chloride gas, and react at 0°C for 4 hours, Stop the flow of hydrogen chloride gas, let it stand still, take the upper layer, dry it with anhydrous calcium chloride, separate it, and distill it under reduced pressure to collect the intermediate product of chlorotannic acid ethyl ether to obtain 13ml.
[0046] Dissolve 4.22g sodium stearate in 20ml dioxane, add phase transfer catalyst FeCl 3 - PEG-400 (0.045gFeCl 3 Mix with 0.344ml polyethylene glycol-400), at a temperature of 30°C, slowly add the above-prepared chlorotannic acid ethyl ether dropwise. Raise the temperature to 70°C, reflux for 6h, cool to room temperature, and filter with suction to obtain a crude product. The crude product was washed with ether, the filter residue was collected, the ether and dioxane were eva...
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