Lithium Tetrafluoroborate CAS 14283-07-9

A preparation method of lithium tetrafluoroborate, making up the following steps:

1) According to the proportion of the mole proportion of H3BO3 to HF of 1:4 ～ 6, including boric acid to hydrofluoric acid to react to get a fluoroboric acid remedy;
2) According to the ratio of Li to B molar proportion of 1.05 to 1.5:1, take the lithium substance and add it to the fluoroboric acid service gotten symphonious 1) to respond to obtain a lithium tetrafluoroborate option;
3) Focus the lithium tetrafluoroborate solution obtained in step 2), take shape by air conditioning, as well as filter to acquire lithium tetrafluoroborate crystals;
4) drying the lithium tetrafluoroborate crystals acquired symphonious 3) to obtain an unrefined lithium tetrafluoroborate;
5) The crude lithium tetrafluoroborate acquired symphonious 4) is positioned in an activator, and fluorine gas or a fluorine-nitrogen blended gas is presented to react to obtain the lithium tetrafluoroborate.

A preparation approach of high-purity lithium tetrafluoroborate, comprising the adhering to steps:

(1) Under the condition of -10 ℃ ～ 10 ℃, gradually include boric acid to the hydrofluoric acid solution, control the molar proportion of boric acid as well as anhydrous hydrofluoric acid to be: H3BO3: HF= 1:( 4 ～ 6), after that continue Stir, react for 0.5-5h, and also prepare a fluoroboric acid remedy;
(2) Under the condition of -10 ℃ ～ 15 ℃, the lithium compound is added to the fluoroboric acid service obtained symphonious (1) according to the molar ratio Li: B= 1.05 ～ 1.5, and also the response is mixed for 0.5-5h to obtain tetrafluoroethylene Lithium borate option;
(3) The lithium tetrafluoroborate option is concentrated under the problems of -0.05 ～ -0.09 MPa and 50 ° C ～ 90 ° C, focused to 1/3 ～ 1/8 of the initial volume of the lithium tetrafluoroborate service, and after that reduced to space temperature level Condensation by cooling down, filtering system, the acquired solid is lithium tetrafluoroborate crystal;
(4) The lithium tetrafluoroborate crystal is at first dried at 30-60 ° C for 2-8h, and afterwards vacuum-dried at 50-100 ° C for 2-8h to get an unrefined lithium tetrafluoroborate;
(5) the lithium tetrafluoroborate unrefined product obtained in step (4) is liquified in anhydrous hydrofluoric acid to acquire a response solution, and the response temperature level is managed from 0 ° C to 15 ° C, and also fluorine gas or fluorine-nitrogen blended gas is passed into the reaction option Accomplish contamination elimination, in which the intake of fluorine gas is: the mole number of fluorine gas: the mole variety of crystal water=( 1.5 ～ 15) in the lithium tetrafluoroborate crude item: 1, it is shown by experiments that under this problem, lithium tetrafluoroborate The contamination elimination effect in the unrefined product is excellent, the obtained product has high pureness, and the lithium tetrafluoroborate hydrofluoric acid mommy liquor is obtained after eliminating impurities by fluorine;
(6) Gradient air conditioning as well as formation of the lithium tetrafluoroborate hydrofluoric acid mother alcohol, the formation temperature is -40 ~ 0 ℃, filter, as well as the crystallization item is dried at 30 ~ 80 ℃ under nitrogen security to obtain a high-purity lithium tetrafluoroborate item, Filtrate recovery and also recycling.