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Green and environment-friendly ascorbyl palmitate and production method thereof

A technology of ascorbyl palmitate and a production method, applied in the field of ascorbyl palmitate and its production, can solve problems such as temperature rise, insufficient product purity, low production efficiency, etc., and achieves ensuring product quality, shortening technological process, and reducing raw materials. cost effect

Pending Publication Date: 2021-09-10
江西凯泰食品科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the acid chloride method requires a two-step reaction. The raw material thionyl chloride used is poisonous, harmful and highly corrosive. It requires harsh reaction conditions and a special reactor, and the reaction generates sulfur dioxide and hydrogen chloride, which is not suitable for industrial production; the lipase method is immature. , the enzyme cannot be reused, and the production cost is too high, which is still under discussion; the sulfuric acid method is a relatively mature production method, but the reaction time is long and the production efficiency is low, and a large amount of heat is released due to the dilution of concentrated sulfuric acid, which will cause a sharp temperature increase. Increased, increasing the risk of operation, while dilute sulfuric acid is troublesome for environmental protection
In addition to product purification in the prior art, most of the purification solvents are reclaimed by distillation. Unreacted palmitic acid has been enriched in the purification solvents. Applying mechanically leads to high palmitic acid content in the product ascorbyl palmitate, and waste residues are produced after solvent distillation. The waste residues are mainly For palmitic acid and ascorbyl palmitate, and other dark impurities, resulting in insufficient product purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 1000kg of reaction solvent DMF into the synthesis reaction kettle, add 150kg of palmitic acid into the kettle, control the temperature at 31°C, stir and dissolve until it dissolves; continue to add 100kg of ascorbic acid into the kettle, control the temperature at 31°C, stir and dissolve until Dissolve, add 10kg of reaction catalyst DDC, control the temperature at 31°C, and react for 4 hours; after the reaction, filter and separate the reaction catalyst DDC; vacuum-concentrate the filtered reaction solution to recover the reaction solvent DMF; Add 1600L of purification solvent (ethyl acetate) and 200L of water to the solution, heat up to 55°C, and dissolve until the solution is clear; leave to separate layers to obtain a water layer and a solvent layer; vacuum evaporate and crystallize the water layer to recover ascorbic acid, and dissolve the solvent layer Transfer to the crystallization kettle, lower the temperature for crystallization, and control the temperature ...

Embodiment 2

[0031] Put 1000kg of reaction solvent DMF into the synthesis reaction kettle, add 200kg of palmitic acid into the kettle, control the temperature at 32°C, stir and dissolve until it dissolves; continue to add 100kg of ascorbic acid into the kettle, control the temperature at 32°C, stir and dissolve until Dissolve, add 10kg of reaction catalyst DDC, control the temperature at 32°C, and react for 4 hours; after the reaction, filter and separate the reaction catalyst DDC; vacuum-concentrate the filtered reaction solution to recover the reaction solvent DMF; Add 1600L of purification solvent (ethyl acetate) and 200L of water to the solution, heat up to 55°C, and dissolve until the solution is clear; leave to separate layers to obtain a water layer and a solvent layer; vacuum evaporate and crystallize the water layer to recover ascorbic acid, and dissolve the solvent layer Transfer to the crystallization kettle, lower the temperature for crystallization, and control the temperature ...

Embodiment 3

[0033] Put 1000kg of reaction solvent DMF into the synthesis reaction kettle, add 150kg of palmitic acid into the kettle, control the temperature at 33°C, stir and dissolve until it dissolves; continue to add 100kg of ascorbic acid into the kettle, control the temperature at 33°C, stir and dissolve until Dissolve, add 15kg of reaction catalyst DDC, control the temperature at 33°C, and react for 4 hours; after the reaction, filter and separate the reaction catalyst DDC; vacuum-concentrate the filtered reaction solution to recover the reaction solvent DMF; Add 1600L of purification solvent (ethyl acetate) and 200L of water to the solution, heat up to 55°C, and dissolve until the solution is clear; leave to separate layers to obtain a water layer and a solvent layer; vacuum evaporate and crystallize the water layer to recover ascorbic acid, and dissolve the solvent layer Transfer to the crystallization kettle, lower the temperature for crystallization, and control the temperature ...

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PUM

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Abstract

The invention discloses green and environment-friendly ascorbyl palmitate and a production method thereof, and belongs to the field of chemical synthesis, and the green and environment-friendly ascorbyl palmitate is prepared by adopting ascorbic acid and palmitic acid as raw materials and carrying out esterification reaction in a reaction solvent DMF containing a DDC reaction catalyst. Meanwhile, unreacted raw materials of the reaction materials are sequentially separated and can continue to be returned to participate in the original reaction, and meanwhile, the purification solvent is used mechanically after being treated, so that the production process is simplified under the condition of ensuring the product purity, the raw material yield is greatly improved, and the environmental protection cost is reduced.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a green and environment-friendly ascorbyl palmitate and a production method thereof. Background technique [0002] Ascorbyl palmitate is a new type of multifunctional antioxidant, which has been assessed by the Food Additives Committee of the World Health Organization as a nutritious, non-toxic, efficient and safe food additive. Currently, there are three methods for the synthesis of ascorbyl palmitate. They are lipase method, sulfuric acid method and palmitoyl chloride method. Among them, the acid chloride method requires a two-step reaction. The raw material thionyl chloride used is poisonous, harmful and highly corrosive. It requires harsh reaction conditions and a special reactor, and the reaction generates sulfur dioxide and hydrogen chloride, which is not suitable for industrial production; the lipase method is immature. , the enzyme cannot be reused, and the production c...

Claims

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Application Information

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IPC IPC(8): C07D307/62
CPCC07D307/62
Inventor 李官华李成福
Owner 江西凯泰食品科技有限公司
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