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Synthesis method of tri(1,1,1,3,3,3-hexafluoro-2-propyl) phosphorous acid

A synthesis method and phosphorous acid technology are applied in the fields of compounds, chemical instruments and methods, organic chemistry, etc. Low activity and toxicity, simple operation effect

Pending Publication Date: 2022-02-22
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the phosphorus trichloride used in this route is more active in nature, more dangerous, and the yield of this method is lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In this example, tris(1,1,1,3,3,3-hexafluoro-2-propyl)phosphorous acid was synthesized by using hexafluoroisopropanol, sodium hydroxide and triphenyl phosphite as raw materials. The organic solvent used during extraction is dichloromethane.

[0015] The specific steps are as follows: 1. Add 50.4g of hexafluoroisopropanol, 31g of triphenyl phosphite, and 12g of sodium hydroxide into a 250ml three-neck flask under the protection of an inert gas throughout.

[0016] 2. Stir at 30°C for 17 hours; add 100ml of water and 100ml of dichloromethane to extract after the reaction is completed, separate the dichloromethane layer and directly rectify, take the fraction with a top temperature of 125°C to 132°C under normal pressure, and obtain 45g of a colorless liquid. The purity is 99.2%, and the yield is 84.6%.

Embodiment 2

[0018] In this example, tris(1,1,1,3,3,3-hexafluoro-2-propyl)phosphorous acid was synthesized by using hexafluoroisopropanol, potassium hydroxide and triphenyl phosphite as raw materials. The organic solvent used in the extraction is dichloroethane.

[0019] The specific steps are as follows: 1. Add 101 g of hexafluoroisopropanol, 62 g of triphenyl phosphite, and 33.6 g of potassium hydroxide into a 250 ml three-necked flask under the protection of an inert gas throughout.

[0020] 2. Stir at 32°C for 20 hours; add 200ml of water and 200ml of dichloroethane to extract after the reaction is completed, separate the dichloroethane layer and then directly rectify, take the fraction with a top temperature of 125°C~132°C under normal pressure to obtain a colorless liquid 89.2g, purity 99.4%, yield 83.8%.

Embodiment 3

[0022] In this example, tris(1,1,1,3,3,3-hexafluoro-2-propyl)phosphorous acid was synthesized by using hexafluoroisopropanol, lithium hydroxide, and triphenyl phosphite as raw materials. The organic solvent used during extraction is ethyl acetate.

[0023] The specific steps are as follows: 1. Add 26g of hexafluoroisopropanol, 15.5g of triphenyl phosphite, and 3.6g of lithium hydroxide into a 100ml three-necked flask under the protection of an inert gas throughout.

[0024] 2. Stir at 30°C for 16 hours; add 50ml of water and 50ml of ethyl acetate for extraction after the reaction is completed, separate the ethyl acetate layer and then directly rectify, take the fraction with a top temperature of 125°C to 132°C under normal pressure to obtain 21g of a colorless liquid, The purity is 99.5%, and the yield is 78.94%.

[0025] It can be obtained from the above examples: 1. Simple operation, few reaction steps, high yield, and high purity of the obtained tris(1,1,1,3,3,3-hexafluoro...

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Abstract

The invention discloses a synthesis method of tris(1,1,1,3,3,3-hexafluoro-2-propyl) phosphorous acid. The synthesis method comprises the following steps: step 1, adding hexafluoroisopropanol, triphenyl phosphite and inorganic strong base into a reaction container under the protection of inert gas in the whole process; and step 2, stirring for 16-20 hours at the temperature of 30-35 DEG C, adding water and an organic solvent for extraction, and taking an organic layer for direct rectification to obtain a target product. The method has the advantages of simple process route, high safety and high product yield.

Description

technical field [0001] The invention relates to the technical field of synthesis of phosphite, in particular to a synthesis method of tris(1,1,1,3,3,3-hexafluoro-2-propyl)phosphorous acid. Background technique [0002] As an important phosphate additive in lithium battery electrolyte, phosphite can not only reduce the flammability of electrolyte, but also improve the cycle performance of lithium ion battery, so it is a relatively potential flame retardant. Tris(1,1,1,3,3,3-hexafluoro-2-propyl) phosphorous acid is a typical fluorine-containing phosphite electrolyte additive, the currently reported tris(1 , 1,1,3,3,3-hexafluoro-2-propyl) phosphorous acid has fewer synthetic routes, mainly by the reaction of hexafluoroisopropanol or sodium hexafluoroisopropoxide and phosphorus trichloride, and then The target product was obtained through distillation and purification. However, the phosphorus trichloride used in this route is more active in nature, more dangerous, and the yiel...

Claims

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Application Information

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IPC IPC(8): C07F9/141
CPCC07F9/1411
Inventor 陈晓龙刘磊时二波常楠刘栋成张明亮周铭柯
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD