Method for synthesizing triallyl phosphate

A technology of triallyl phosphate and synthesis method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problem of low yield, inability to achieve both purity and yield , the problem of low purity of triallyl phosphate

Active Publication Date: 2017-07-18
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problems of low purity and low yield of triallyl phosphate prepared in the prior art, and the incompatibility of both purity and yield, the present invention provides a synthetic method for triallyl phosphate. The present invention synthesizes The method is simple and easy to operate, and the prepared triallyl phosphate not only has a high yield, but also has a high purity, which solves the problem that the purity and the yield cannot be combined

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  • Method for synthesizing triallyl phosphate
  • Method for synthesizing triallyl phosphate
  • Method for synthesizing triallyl phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Under nitrogen protection, add 81.2g (1.4mol) allyl alcohol, 129.28g (1.28mol) triethylamine, and 200mL toluene into a 500mL four-neck flask. After stirring for 5 minutes, remove the nitrogen protection from the reaction flask, seal the bottle tightly, and place it in Low temperature and constant temperature reaction bath (Gongyi DFY-5), set to cool down.

[0023] Cool down to -34℃, first add 0.02g sodium ethoxide. The addition of sodium ethoxide can promote the reaction, make the reaction mild and stable, and provide a guarantee for obtaining high-purity and high-yield products, and then start adding 61.2g (0.4mol ) Phosphorus oxychloride controls the dropping rate so that the temperature of the reaction solution does not change significantly.

[0024] After dripping, it takes 7.5h, -34℃, stop refrigeration, continue stirring, and naturally heat up.

[0025] The temperature was raised to -2°C, and the reaction was stopped after 2 hours.

[0026] The reaction solution was filt...

Embodiment 2

[0028] Under the protection of nitrogen, add 20.3g (0.35mol) allyl alcohol, 25.28g (0.32mol) pyridine, and 50mL toluene into a 250mL four-neck flask. After stirring for 5min, remove the nitrogen protection from the reaction flask, tightly seal the mouth of the flask, and place it in a low temperature constant temperature. Reaction bath (Gongyi DFY-5), set to cool down.

[0029] The temperature was lowered to -34°C, and 15.3 g (0.1 mol) of phosphorus oxychloride was added dropwise to control the dropping rate so that the temperature of the reaction solution did not change significantly.

[0030] After dripping, it takes 3.5h, -36℃, stop refrigeration and heat up naturally.

[0031] The temperature was raised to 0°C and took 2.5 hours to stop the reaction.

[0032] The reaction solution was filtered to remove the white solid pyridine hydrochloride, and the filter cake was washed with a small amount of toluene. The filter cake pyridine hydrochloride is very easy to absorb water, liquefi...

Embodiment 3

[0034] Add 20.3g (0.35mol) allyl alcohol, 30.3g (0.3mol) triethylamine, and 40mL toluene into a 250mL four-necked flask under nitrogen protection. After stirring for 5min, remove the nitrogen protection from the reaction flask, tightly seal the mouth of the flask, and put it in Low temperature and constant temperature reaction bath (Gongyi DFY-5), set to cool down.

[0035] The temperature was lowered to -42°C, and 15.3g (0.1mol) of phosphorus oxychloride was started to be added dropwise to control the dropping rate so that the temperature of the reaction solution did not change significantly.

[0036] After dripping, it takes 5.4h, -42℃, stop refrigeration, and naturally heat up.

[0037] The temperature was raised to -2°C and it took 2.3 hours to stop the reaction.

[0038] The reaction solution was filtered to remove the white solid pyridine hydrochloride, and the filter cake was washed with a small amount of toluene. The filter cake pyridine hydrochloride is very easy to absorb w...

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Abstract

The invention provides a method for synthesizing triallyl phosphate, and belongs to the technical field of compound synthesis. The method comprises the following steps: adding allyl alcohol serving as a raw material and an acid-binding agent into a solvent under protection of nitrogen; then, adding phosphorus oxychloride to react; pumping and filtering the reacting liquid; washing, drying, decoloring and concentrating to obtain triallyl phosphate; controlling the reacting temperature to be less than negative 30 DEG C when the phosphorus oxychloride is dropwise added for 3.4-7.5 hours; and naturally heating to -2-zero DEG C, and stopping reaction. The synthesizing method is simple and easy to operate, and the prepared triallyl phosphate has high yield and high purity.

Description

Technical field [0001] The invention belongs to the technical field of compound synthesis and relates to a synthetic method of triallyl phosphate. The synthetic method of the invention is simple, the reaction is sufficient, the reaction process is stable, and the obtained triallyl phosphate has high yield and high purity. Background technique [0002] Triallyl phosphate is a new type of non-aqueous lithium ion battery electrolyte additive, which 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] At present, the synthesis of triallyl phosphate mainly has the following methods: [0004] 1. Under the protection of inert gas, use allyl alcohol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/113
CPCC07F9/113
Inventor 张民刘鹏梅银平
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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