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Method for preparing phosphorylethanolamine compound

A technology of phosphoethanolamine and compounds, which is applied in the field of biochemistry, can solve the problems of lower yield, lower product quality, and more wastes, and achieve the effects of simple, safe and reasonable process, short production cycle, and wide source of raw materials

Inactive Publication Date: 2012-07-04
HENAN INST OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] A large amount of solvent is required in the two-step reaction of preparing phosphoethanolamine: in the first step reaction, while ethanolamine phosphate is precipitated in the organic solvent, inorganic ions such as lead and other heavy metals in the reaction system are also precipitated together with the precipitation, resulting in impurities The enrichment of these impurities then enters the subsequent reaction, and cannot be directly removed in the second step reaction, which reduces the quality of the product. In order to improve the quality, it is necessary to use activated carbon for further purification treatment, which increases the cost and the amount of three wastes. At the same time The yield is reduced; the impurities in the organic solvent used in the second step reaction are also enriched in the final product, which further reduces the quality of the product
In addition, due to the use of a large amount of organic solvents in production, the production environment is poor, there are many wastes, and the cost is high

Method used

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  • Method for preparing phosphorylethanolamine compound
  • Method for preparing phosphorylethanolamine compound

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Experimental program
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Embodiment 1

[0030] Add 50kg of water into the 100L reactor, heat up to 80°C, add 14.2kg of 100% phosphorus pentoxide, then add 12.2kg of 100% ethanolamine, remove water for 2 hours at a vacuum degree of -0.098kPa, and then heat up to 100°C, 120°C, 140°C, 160°C, 180°C, 200°C respectively at a vacuum degree of -0.098kPa or above to remove water for 2 hours, then crush the agglomerates and then dry at 160°C at a vacuum degree of -0.098kPa or above After 2 hours, 27.1 kg of white solid powder of monoethanolamine phosphate was obtained, with a melting point of 236.6-237.6° C., a yield of 96%, and a purity of ≥99.3%.

Embodiment 2

[0032] Add 85% phosphoric acid (H 3 PO 4 ) aqueous solution 500kg, add 265kg (61.05) of 100% ethanolamine at room temperature, raise the temperature to 80°C, remove water for 2 hours at a vacuum degree above -0.098kPa, then raise the temperature to 100°C, 120°C, 140°C, 160°C, 180°C ℃, 200 ℃, vacuum dewatering at a vacuum degree of -0.098kPa or above for 2 hours, the agglomerates were crushed, and then dried at 160 ℃ at a vacuum degree of -0.098kPa or above for 2 hours to obtain 593kg of white solid powder of monoethanolamine phosphate, melting point 239.8 ~242°C, yield 97%, purity 99.5%.

Embodiment 3

[0034] Add 61.4kg of 50% phosphorus oxychloride toluene solution into a 100L reactor, then add 12.2kg of 100% ethanolamine, keep at 80°C for 2 hours at a vacuum degree of -0.098kPa, and then raise the temperature to 100°C, 120°C , 140°C, 160°C, and 180°C were kept at a vacuum degree of -0.098kPa or more for 2 hours respectively, and the tail gas was condensed to obtain an aqueous solution of hydrogen chloride. Monoethanolamine hydrochloride white solid powder 32.3kg, melting point 247.5-248.9°C, yield 91%, purity ≥ 99.0%.

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Abstract

The invention relates to a method for preparing a phosphorylethanolamine compound, which belongs to the technical field of biochemistry. The method comprises the following steps of: adding ethanolamine or ethanolamine solution into one of phosphorus pentoxide, the solution of phosphoric acid, phosphorus oxychloride or the solution of phosphorus oxychloride at a certain reaction temperature to form a reaction mixture; heating the reaction mixture for vacuum-drying by using a direct program to form phosphorylethanolamine or phosphorylethanolamine hydrochloride; and dissolving the reaction product into water in a certain amount and then adding ethanolamine or the ethanolamine solution, wherein the mass ratio of the reaction product to the water in the certain amount is 1:1-100. As the water serves as a solvent, the method of the invention ensures high yield, vast raw material sources, low production cost, simple, safe and rational process, short production cycle and high purity of the prepared product, and avoids wastewater, waste gases and waste residues.

Description

technical field [0001] The invention relates to a method for preparing phosphoethanolamine compounds, belonging to the technical field of biochemistry. Background technique [0002] According to the structure, phosphoethanolamine is divided into monoethanolamine phosphate (CAS: 1071-23-4), diethanolamine phosphate (CAS: 6094-81-1) and triethanolamine phosphate (CAS: 29901-63-1). Among them, monoethanolamine phosphate is also called 2-aminoethanol dihydrogen phosphate, 2-aminoethanol phosphate, ethanolamine phosphate, o-phosphoethanolamine, phosphoric acid, 2-aminoethyl ester, phosphoric acid aminoethanol, phosphorylcholine, 2-ammonia Ethyl dihydrogen phosphate, cholamine phosphoric acid, 2-hydroxyethylamine phosphoric acid, etc. [0003] Phosphoethanolamine compounds are widely used in biotechnology, medicine and other fields, and can also be used as feed additives and special lubricants. The disclosed synthesis method and process of phosphoethanolamine compounds mainly us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/09
Inventor 胡海燕李玉川常景玲
Owner HENAN INST OF SCI & TECH
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