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Synthetic method of triallyl phosphate

A technology of triallyl phosphate ester 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 that purity and yield cannot be achieved at the same time, and the yield is low. , the problem of low purity of triallyl phosphate

Active Publication Date: 2019-04-16
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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  • Synthetic method of triallyl phosphate
  • Synthetic method of triallyl phosphate
  • Synthetic method of triallyl phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 81.2g (1.4mol) of allyl alcohol, 129.28g (1.28mol) of triethylamine, and 200mL of toluene into a 500mL four-necked flask under nitrogen protection. After stirring for 5 minutes, remove the nitrogen protection from the reaction flask, tightly seal the bottle mouth, and place Low temperature and constant temperature reaction bath (Gongyi DFY-5), set to cool down.

[0022] Cool down to -34°C, first add 0.02g sodium ethylate, the addition of sodium ethylate can promote the reaction, make the reaction mild and stable, and provide guarantee for obtaining high-purity, high-yield products, and then start to drop 61.2g (0.4mol ) phosphorus oxychloride, control the rate of addition, so that the temperature of the reaction solution does not change significantly.

[0023] After dropping, it took 7.5 hours, at -34°C, stop cooling, continue to stir, and raise the temperature naturally.

[0024] The temperature was raised to -2°C, and the reaction was stopped after 2 hours.

[0...

Embodiment 2

[0027] Add 20.3g (0.35mol) allyl alcohol, 25.28g (0.32mol) pyridine, and 50mL toluene to a 250mL four-neck bottle under nitrogen protection, stir for 5 minutes, remove the nitrogen protection from the reaction bottle, tightly seal the bottle mouth, and place it in a low temperature constant temperature Reaction bath (Gongyi DFY-5), set to cool down.

[0028] The temperature was lowered to -34° C., and 15.3 g (0.1 mol) of phosphorus oxychloride was added dropwise, and the rate of addition was controlled so that the temperature of the reaction solution did not change significantly.

[0029] After dropping, it took 3.5 hours, at -36°C, stop cooling, and let the temperature rise naturally.

[0030] The temperature was raised to 0°C, and the reaction was stopped after 2.5 hours.

[0031] The reaction solution was filtered to remove white solid pyridine hydrochloride, and the filter cake was washed with a small amount of toluene. The filter cake pyridine hydrochloride is very easy...

Embodiment 3

[0033] Add 20.3g (0.35mol) allyl alcohol, 30.3g (0.3mol) triethylamine, and 40mL toluene to a 250mL four-neck bottle under nitrogen protection, stir for 5 minutes, remove the nitrogen protection from the reaction bottle, seal the bottle mouth tightly, and place Low temperature and constant temperature reaction bath (Gongyi DFY-5), set to cool down.

[0034] The temperature was lowered to -42°C, and 15.3 g (0.1 mol) of phosphorus oxychloride was added dropwise, and the rate of addition was controlled so that the temperature of the reaction solution did not change significantly.

[0035] After dropping, it took 5.4 hours, at -42°C, stop cooling, and let the temperature rise naturally.

[0036] The temperature was raised to -2°C, and it took 2.3 hours to stop the reaction.

[0037] The reaction solution was filtered to remove 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 ...

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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 synthesis method of triallyl phosphate. The synthesis 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] The synthesis of triallyl phosphate mainly contains the following methods at present: [0004] 1. Under the protection of an inert gas, u...

Claims

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Application Information

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Patent Type & Authority Patents(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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