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Preparation method of triallyl phosphate

A technology of triallyl phosphate and allyl alcohol, which is applied in the field of preparation of triallyl phosphate, can solve the problems of failure to meet application requirements and low purity of triallyl phosphate, achieve short routes, high product purity, The effect of less toxic materials

Inactive Publication Date: 2013-12-25
SHENZHEN CAPCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

What's more serious is that this patent only separates the product by washing the reaction solution with ether, and the obtained triallyl phosphate has a very low purity, which contains a large amount of impurities such as ether and triethylamine hydrochloride, and the quality is far from reaching the level it was in Lithium-ion battery electrolyte additives and other application requirements

Method used

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preparation example Construction

[0023] The method for preparing high-purity triallyl phosphate of this embodiment includes the following steps:

[0024] 1. Under inert gas atmosphere, mix allyl alcohol, acid binding agent and ether solvent;

[0025] Wherein, the inert gas atmosphere is preferably nitrogen, and the materials are kept in a dry atmosphere during the mixing process;

[0026] Wherein, the ether solvent is selected from methyl tert-butyl ether, diethyl ether, tetrahydrofuran, 1,4-dioxane, n-propyl ether, n-butyl ether, ethylene glycol dimethyl ether and ethylene glycol diethyl ether One or more; from the viewpoint of solvent cost, safety and reaction yield, methyl tert-butyl ether is preferred.

[0027] Among them, the acid binding agent is preferably one or more of pyridine, triethylamine, potassium carbonate, sodium carbonate and quaternary ammonium base; in view of the reaction yield and the chemical toxicity of the acid binding agent, triethylamine is preferred.

[0028] Wherein, the molar ratio of the...

preparation Embodiment 1

[0042] Weigh 261g (4.5mol, 306ml) of propenol, 454g (4.5mol, 626ml) of triethylamine, and 1332g (1800ml) of methyl tert-butyl ether into a 3L three-necked flask.

[0043] Put the flask into an ice-water bath, pour nitrogen through it, and stir it mechanically to make it fully mixed. When the temperature of the mixed solution drops to 15°C, start to add 230g (1.5mol, 140ml) phosphorus oxychloride dropwise, and control the dropping rate to make the reaction liquid The temperature is kept within the room temperature range.

[0044] After the addition is complete, react at room temperature for 2 hours, filter to remove triethylamine hydrochloride, and then add about 200 ml of methyl tert-butyl ether to the residue in the flask for rinse, and the cleaning solution and the filtrate are combined.

[0045] The filtrate was heated in an oil bath at 70°C for atmospheric distillation to recover methyl tert-butyl ether.

[0046] The remaining filtrate was heated under a pressure of 1mbar and 130°...

preparation Embodiment 2

[0048] Weigh 261g (4.5mol, 306ml) of propenol, 454g (4.5mol, 626ml) of triethylamine, and 1284g of ether (1800ml) in a 3L three-necked flask.

[0049] Put the flask in an ice-water bath, ventilate nitrogen, and stir mechanically. When the temperature of the mixed solution drops to 10°C, start to add 230g (1.5mol, 140ml) of phosphorus oxychloride, and control the dropping rate to keep the temperature of the reaction solution at room temperature Within the range, a large amount of white solid is generated.

[0050] After the addition is complete, react at room temperature for 1 hour, filter to remove triethylamine hydrochloride, and then add about 200 ml of ether to the residue in the flask for rinse, and the cleaning solution and the filtrate are combined.

[0051] The filtrate was heated in an oil bath at 50°C for atmospheric distillation to recover ether.

[0052] The remaining filtrate was heated at a pressure of 1 mbar and 130°C in an oil bath for vacuum distillation. After the dis...

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Abstract

The invention relates to a preparation method of triallyl phosphate, which comprises the following steps that allyl alcohol, an acid-binding agent and an ether solvent are mixed in an inert gas atmosphere; phosphorus oxychloride is dropwise added to a mixed liquid in the inert gas atmosphere; then stirring and reaction are performed; a liquid obtained after the reaction is filtered; a filtrate obtained after filtering is subjected to atmospheric distillation and solvent recovery; the residual filtrate after the solvent recovery is subjected to rectification under vacuum; and a fraction of triallyl phosphate is collected. The method has the following advantages that 1, the method is simple in technology, short in route, cheap in material and very small in toxic property, and is suitable for industrial production; 2, the method is few in byproduct and high in yield; and 3, the purity of a rectified and purified product is high, and can reach 99.5%, and the method is particularly suitable for the fields of lithium ion battery electrolyte additives and the like.

Description

Technical field [0001] The invention relates to a method for synthesizing and purifying organic compounds, in particular to a method for preparing triallyl phosphate. Background technique [0002] Triallyl phosphate, a new type of non-aqueous lithium ion battery electrolyte additive, helps to form a stable and dense passivation film on the electrode surface, prevents further decomposition of solvent molecules, and can effectively improve the high temperature storage of lithium ion batteries And high temperature cycle performance. At the same time, triallyl phosphate is also an important polymer monomer, which can be used in industry as a halogen-free flame retardant. [0003] There are two methods for preparing triallyl phosphate currently reported: [0004] 1. Use phosphorus trichloride to react with allyl alcohol, pyridine as acid binding agent, and ether as solvent to obtain triallyl phosphite first, and then to obtain triallyl phosphate after oxidation. The disadvantage of thi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/113
Inventor 汪仕华陈群
Owner SHENZHEN CAPCHEM TECH CO LTD
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