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Method used for preparing tetrabutylammonium fluoride trihydrate

A technology of tetrabutylammonium fluoride and trihydrate, which is applied in the field of preparation of organic fluorine compounds, can solve the problems of complicated operation and high cost, and achieve the effects of convenient operation, short steps and high product quality

Active Publication Date: 2015-07-29
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

J.Am.Chem.Soc., 2007,129(4),746-747 reported that tetrabutylammonium fluoride clathrate hydrate can be used as a low-pressure hydrogen storage material, but the method for preparing clathrate hydrate in the prior art operates cumbersome and costly

Method used

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  • Method used for preparing tetrabutylammonium fluoride trihydrate
  • Method used for preparing tetrabutylammonium fluoride trihydrate

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 80.57g (0.25mol) of tetrabutylammonium bromide, 21.79g (0.375mol) of potassium fluoride and 600mL of water into a 1L four-necked flask, and mechanically stir to dissolve. The solution was placed in a low-temperature bath at 1-10°C for crystallization, and a large amount of solids precipitated after half an hour. The crystallization was continued for one hour, and a large amount of white solid was obtained by suction filtration. Wash with a small amount of deionized water. Vacuum drying at 40°C for 24 hours gave a white solid.

[0021] That 1 H-NMR spectrum see figure 1 , 19 F-NMR spectrum see figure 2 ,Data are as follows: 1 H NMR: (400MHz, D 2 O) 0.96(t, 12H), 1.38(m, 8H), 1.67(m, 8H), 3.21(m, 8H), 19 F NMR: (376MHz, D 2 (0) -122.44. After identification, its structural formula is N(CH 2 CH 2 CH 2 CH 3 ) 4 F·3H 2 O, namely tetrabutylammonium fluoride trihydrate. Yield 81.2%, moisture 17.25%.

Embodiment 2

[0023] Add 80.57g (0.25mol) of tetrabutylammonium bromide, 17.4g (0.30mol) of potassium fluoride and 600mL of water into a 1L four-necked flask, and mechanically stir to dissolve. The solution was placed in a low-temperature bath at 1-10°C for crystallization, and a large amount of solids precipitated after half an hour. The crystallization was continued for one hour, and a large amount of white solid was obtained by suction filtration. Wash with a small amount of deionized water. Vacuum drying at 40°C for 24 hours gave a white solid. Its nuclear magnetic data is identical with embodiment 1. Yield 75.5%, moisture 17.80%.

Embodiment 3

[0025] Add 80.57g (0.25mol) of tetrabutylammonium bromide, 145g (2.50mol) of potassium fluoride and 600mL of water into a 1L four-neck flask, and mechanically stir to dissolve. The solution was placed in a low-temperature bath at 1-10°C for crystallization, and a large amount of solids precipitated after half an hour. The crystallization was continued for one hour, and a large amount of white solid was obtained by suction filtration. Wash with a small amount of deionized water. Vacuum drying at 40°C for 24 hours gave a white solid. Its nuclear magnetic data is identical with embodiment 1. Yield 82.5%, moisture 18.35%.

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Abstract

The invention relates to a method used for preparing tetrabutylammonium fluoride trihydrate. According to the method, a tetrabutylammonium salt and potassium fluoride are dissolved in water; low temperature crystallization is carried out; pumping filtration is carried out so as to obtain tetrabutylammonium fluoride clathrate hydrate; and tetrabutylammonium fluoride trihydrate is obtained via vacuum drying. Reaction conditions of the method are mild; reaction processes are carried out in water; no organic solvent is used; the method is green and friendly to the environment; tetrabutylammonium fluoride trihydrate is obtained via crystallization separation of the tetrabutylammonium fluoride clathrate hydrate; steps are short; operation is simple and convenient; hydrofluoric acid is not used; no ion exchange column is used; no special requirement on equipment is proposed; cost is low; yield is high; and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to the field of preparation methods of organic fluorine compounds, in particular to a preparation method of tetrabutylammonium fluoride trihydrate. Background technique [0002] Tetrabutylammonium fluoride is widely used in the field of organic synthesis, and can be used as a fluorinating reagent, a silylation catalyst for alcohols, a phase transfer catalyst, etc. Because tetrabutylammonium fluoride is very easy to absorb moisture, the product is usually sold in the form of tetrabutylammonium fluoride trihydrate or tetrabutylammonium fluoride tetrahydrofuran solution. Ammonium oxide, then neutralized with hydrofluoric acid to obtain tetrabutylammonium fluoride monohydrate. [0003] Clathrate hydrate is a cage-like structure crystal formed by water molecules. The crystal contains a large number of cavities, and each cavity is composed of polyhedrons surrounded by some water molecules. It is used in seawater desalination, gas separ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07C209/12
Inventor 李义涛伍阳刘新烁李凯曾水明张兵兵卢沁月屈季春
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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