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Green synthesis method of n-propyl phosphoric acid cyclic anhydride

A propylphosphoric acid cyclic anhydride, green synthesis technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of high reaction temperature and production and long reaction time, difficulty in obtaining raw materials, etc., to achieve the effect of reducing the pressure of environmental protection treatment, low production cost, and reducing the cost of environmental protection treatment

Pending Publication Date: 2022-07-08
HEILONGJIANG HAOYUN FINE CHEM
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Problems solved by technology

[0007] The purpose of the present invention is to solve the existing 1-propylphosphoric acid cyclic anhydride high reaction temperature, harsh conditions, difficult to deal with by-products, and the difficulty in obtaining some raw materials, resulting in limited production, long reaction time, and high cost technical problems

Method used

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  • Green synthesis method of n-propyl phosphoric acid cyclic anhydride

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Embodiment 1

[0031] Embodiment 1: the green synthesis method of a kind of n-propyl phosphoric acid cyclic anhydride of the present embodiment is carried out according to the following steps:

[0032] Step 1: Add 142.8g (2.1mol) sodium ethoxide to 600g toluene under stirring, then dropwise add 476g (2mol) toluene solution of diethyl phosphite (238g of toluene), dropwise add diethyl phosphite The temperature of the toluene solution is controlled to be below 50 °C, the temperature is raised to 50 °C after the dropwise addition is completed, and then 258.3 g (2.1 mol) of bromopropane are added dropwise to carry out the alkylation reaction. The temperature of the chemical reaction was 80°C and the time was 8h. According to gas chromatography analysis, diethyl phosphite in the system was less than 0.5wt%, 320g of water was added and left to stand for stratification to obtain an aqueous layer of sodium bromide solution and an oil layer, and the oil layer was desolubilized. and vacuum distillation...

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Abstract

The invention relates to a green synthesis method of n-propyl phosphoric acid cyclic anhydride. The invention belongs to the field of polymer synthesis. The invention aims to solve the technical problems of production limitation, long reaction time and high cost caused by high reaction temperature, harsh conditions, difficulty in byproduct treatment and difficulty in obtaining part of raw materials in the existing 1-propyl phosphoric acid cyclic anhydride. The method comprises the following steps: 1, adding sodium ethoxide, a toluene solution of diethyl phosphite and bromopropane into a solvent, adding water after the reaction is completed, standing for layering, and carrying out desolvation and reduced pressure distillation on an oil layer to obtain 1-propyl diethyl phosphate; 2, hydrobromic acid is added into 1-propyl diethyl phosphate for a hydrolysis reaction, and propyl phosphoric acid is obtained; and 3, adding acetic anhydride into propyl phosphoric acid, and carrying out a dehydration reaction to obtain n-propyl phosphoric anhydride. According to the method, efficient removal of the byproduct sodium bromide can be completed through simple treatment, the raw materials are simple and easy to obtain, the price is low, the synthesis steps are simple, the production cost is low, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, in particular to a green synthesis method of n-propylphosphoric acid cyclic anhydride. Background technique [0002] n-Propylphosphoric acid cyclic anhydride is a colorless or light yellow viscous liquid, which is an important condensation reagent. It is mainly used as a coupling agent for amide or ester condensation reaction, because of its high activity, compared with conventional condensation reagents, it has the advantages of high reaction yield, low toxicity and convenient post-processing. The application is more and more extensive, and there is a trend to gradually replace DCC, DIC and EDC. In recent years, it has been reported in the literature that adding a certain amount of n-propyl phosphoric acid cyclic anhydride to the lithium battery electrolyte can significantly improve the SEI film-forming performance of lithium battery electrodes. Effectively prolong the cycle life of lithium ba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6571
CPCC07F9/657181Y02E60/10
Inventor 张琳左殿发刘广才袁福龙任吉秋于欣李成军余威
Owner HEILONGJIANG HAOYUN FINE CHEM
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