Preparation method of anhydrous hydrogen fluoride
A technology of anhydrous hydrogen fluoride and hydrogen fluoride salt, applied in the direction of hydrogen fluoride, fluorine/hydrogen fluoride, chemical instruments and methods, etc., can solve the problems of ammonium bifluoride melting, low fluorine conversion rate, difficult to control, etc.
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[0019] The preparation method of the anhydrous hydrogen fluoride of the present invention comprises the following steps: reacting hydrogen fluoride salt with concentrated sulfuric acid; the hydrogen fluoride salt is alkali metal or alkaline earth metal hydrogen fluoride salt.
[0020] Preferably, the reaction temperature is 200-300°C.
[0021] Preferably, the reaction time is 0.5-3 hours. More preferably, the reaction time is 1-2 hours.
[0022] Preferably, the hydrogen fluoride salt is at least one of sodium hydrogen fluoride, potassium hydrogen fluoride, lithium hydrogen fluoride, and magnesium hydrogen fluoride. Further preferably, the hydrogen fluoride salt is sodium hydrogen fluoride.
[0023] The hydrogen fluoride salt is prepared by the mixed reaction of ammonium hydrogen fluoride, sulfate and water. The hydrogen fluoride salt can also use commercially available products.
[0024] The mixing of the ammonium bifluoride, sulfate and water is as follows: the sulfate is...
Embodiment 1
[0039] The preparation method of the anhydrous hydrogen fluoride of the present embodiment comprises the following steps:
[0040] (1) Ammonium fluoride solution and silicon dioxide are prepared by ammonium fluoride solution and silicon dioxide by ammonium lysis of 500 g of fluorosilicic acid solution (produced by phosphate fertilizer, fluorine chemical industry and other industry by-products) with a mass percentage content of 10%, and the obtained filter cake is separated by filtration It is silicon dioxide ointment, and after washing and drying, a white carbon black product is obtained; the obtained filtrate is ammonium fluoride solution;
[0041] (2) After the ammonium fluoride solution is evaporated and concentrated, the ammonium fluoride solid is obtained, and then the ammonium fluoride is heated and decomposed in a solid state to obtain 58.8g (1.03mol) of ammonium bifluoride and ammonia gas, and the ammonia gas is used in the step (1) after being absorbed by water ) in t...
Embodiment 2
[0046] The preparation method of the anhydrous hydrogen fluoride of the present embodiment comprises the following steps:
[0047] (1) ammonium fluoride solution and silicon dioxide are prepared by ammonium fluoride solution and silicon dioxide by ammonium lysis of 500 g of fluorosilicic acid solution (produced by phosphate fertilizer, fluorine chemical industry and other industry by-products) with a mass percentage content of 30%, and the obtained filter cake is separated by filtration It is silicon dioxide ointment, and after washing and drying, a white carbon black product is obtained; the obtained filtrate is ammonium fluoride solution;
[0048] (2) The ammonium fluoride solution is evaporated and concentrated to obtain ammonium fluoride solid, and then the ammonium fluoride is heated and decomposed in a solid state to obtain 172.5g (3.03mol) of ammonium bifluoride and ammonia gas, which is used in step (1) for silicon fluoride Ammonolysis of acid solution;
[0049] (3) I...
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