阅读说明：本技术 一种氟锂酸铍的制备方法 (Preparation method of fluorine lithium beryllium ) 是由 严永生 于 2020-12-03 设计创作，主要内容包括：本发明公开了一种氟锂酸铍的制备方法,其中将金属锂或者锂化合物溶解于氢氟酸或者含氟溶液中,在加入过量金属铍或者铍的化合物,形成氟锂酸铍溶液。氟锂酸铍溶液离子树脂脱附金属离子杂质,再通过电渗析浓缩,经过真空低温干燥,再经过高温烘箱烘干,粉碎成成品。(The invention discloses a preparation method of beryllium fluorolithiate, wherein metal lithium or a lithium compound is dissolved in hydrofluoric acid or a fluorine-containing solution, and an excessive amount of the metal beryllium or the beryllium compound is added to form the beryllium fluorolithiate solution. Desorbing metal ion impurities by using beryllium fluorolithiate solution ion resin, concentrating by electrodialysis, drying at low temperature in vacuum, drying by a high-temperature oven, and crushing into a finished product.)

1. The preparation method of beryllium fluorolithiate is characterized by comprising the following steps of:

dissolving, namely dissolving metal lithium or a lithium compound in hydrofluoric acid or a fluorine-containing solution, and adding a metal beryllium or a beryllium compound to form a lithium fluoberyllate solution;

impurity removal: passing the lithium fluoroberyllate through a resin tower for ion exchange adsorption;

③, concentrating: introducing the purified lithium fluoberyllinate solution into electrodialysis for concentration;

and fourthly, freeze drying: primarily drying the concentrated beryllium-containing solution by freeze drying;

drying at high temperature: after freeze drying, crushing and granulating after high-temperature drying;

wherein, the content of single ion of alkali metal ion is lower than 500ppm, and the content of single ion of other metal ion is not more than 150 ppm.

2. The method for preparing beryllium fluorolithiate as claimed in claim 1, which is characterized in that: the beryllium-containing material can be metallic beryllium, or beryllium fluoride, beryllium hydroxide, beryllium oxide, beryllium carbonate, or beryllium-containing ore feedstock.

3. The method for preparing beryllium fluorolithiate as claimed in claim 1, which is characterized in that: the hydrofluoric acid is electronic grade hydrofluoric acid or electronic grade hydrogen fluoride gas.

Technical Field

The invention relates to a preparation method of beryllium fluorolithiate, belonging to the field of fine chemicals.

Background

A Molten Salt Reactor (MSR) is a Reactor which uses Molten Salt dissolved with fissile materials and in a Molten state as nuclear fuel, is a Reactor of a nuclear power generation technology commonly used at present, and directly dissolves the nuclear fuel into the Molten Salt in the Molten state, the prepared liquid nuclear fuel, molten salt nuclear reactor, has many advantages of high neutron economy, high power density, controllable inherent load, large negative temperature coefficient, high conversion ratio, high reliability, low fuel combination consumption, breedability and the like, one of the fourth generation nuclear reactor designs identified as the priority development at the fourth generation nuclear reactor international seminar held in tokyo, japan in 2002, moreover, the molten salt has higher requirements on the content of anions and metal ions, wherein the content of the metal ions is less than 100ppm, and the content of the anions is less than 100 ppm. Wherein the content of metal ions such as Fe ions, Co ions, Ni ions, Mn ions, Cr ions, Ti ions, Mo ions, Al ions and W ions in the molten salt is controlled, and the content cannot be too high.

Disclosure of Invention

The invention aims to solve the technical problem that the ion content is high by adopting a plurality of purification means aiming at the current method for preparing high-purity beryllium fluoride.

In order to solve the technical problems, the invention adopts the following technical scheme:

a preparation method of beryllium fluorolithiate comprises the following steps:

dissolving, namely dissolving metal lithium or a lithium compound in hydrofluoric acid or a fluorine-containing solution, and adding a metal beryllium or a beryllium compound to form a lithium fluoroberyllium acid solution;

secondly, removing impurities: passing the lithium fluoroberyllate through a resin tower for ion exchange adsorption;

thirdly, concentrating: introducing the purified lithium fluoberyllinate solution into electrodialysis for concentration;

fourthly, freeze drying: primarily drying the concentrated beryllium-containing solution by freeze drying;

fifthly, high-temperature drying: after freeze drying, crushing and granulating after high-temperature drying;

sixthly, wherein the content of alkali metal ion single ions is lower than 500ppm, and the content of other metal ion single ions is not more than 150 ppm.

The beryllium-containing substance can be metallic beryllium, or beryllium fluoride, beryllium hydroxide, beryllium oxide, beryllium carbonate or a beryllium-containing ore raw material.

The hydrofluoric acid is electronic grade hydrofluoric acid or electronic grade hydrogen fluoride gas.

Detailed Description

Example 1:

firstly, dissolving: dissolving metal lithium by 49% of electronic grade hydrofluoric acid, and adding pure water 3 to obtain a lithium-containing solution 4, wherein the mass content of the lithium-containing solution is more than 100 g/L; then adding metal beryllium, and removing impurities: introducing the beryllium-containing solution 4 into a 5-resin tower for ion exchange adsorption; the ion exchange resin adopts cation exchange resin, anion exchange resin and mixed resin which are connected in series to treat the beryllium-containing solution. Thirdly, concentrating: introducing the purified beryllium-containing solution 5 into an electrodialysis 6 for concentration;

fourthly, freeze drying: the concentrated beryllium-containing solution is subjected to primary drying by freeze drying 7; fifthly, high-temperature drying: drying the freeze-dried mixture at high temperature for 8 hours, and then drying the freeze-dried mixture in a sectional manner, wherein the drying is carried out by heating the freeze-dried mixture at 120 ℃ for two hours, heating the freeze-dried mixture at 180 ℃ for eight hours, heating the freeze-dried mixture at 360 ℃ for 12 hours and heating the freeze-dried mixture at 400 ℃ for 12 hours. Sixthly, wherein the content of alkali metal ion single ions is lower than 500ppm, and the content of other metal ion single ions is not more than 150 ppm.