Method for producing lithium compound
The present invention relates to a lithium compound manufacturing method comprising the steps of heat treatment of lithium-containing ore; roasting the heat-treated ore with sulfuric acid to prepare an acid product; mixing the acid product with leaching water to prepare a leachate; purifying the leachate; and adding a phosphorus supply material and a basic material to the purified leachate to obtain a solid lithium phosphate.
1 . A method of manufacturing lithium compound comprising:
heating a lithium-containing ore;
preparing an acid product by roasting the heated ore with sulfuric acid;
preparing a leachate by mixing the acid product with leaching water;
purifying the leachate;
obtaining a solid lithium phosphate by adding a phosphorus supply material and a basic material to the purified leachate; and
obtaining a solid lithium sulfate by reacting the solid lithium phosphate with sulfuric acid,
wherein, in the step of preparing an acid product,
an equivalent ratio (lithium:sulfuric acid) of lithium in the heat-treated ore and the sulfuric acid is 1:1.1 to 1:1.4,
wherein,
the step of purifying the leachate comprises:
separating primary impurities including Al, Si or a combination thereof by adjusting the pH of the leachate to 5 to 8; and
removing secondary impurities including Mg, Ca, Mn or a combination thereof by adjusting the pH of the leachate from which the primary impurities are separated to 10 or more,
wherein, the step of obtaining the solid lithium sulfate comprises:
mixing the lithium phosphate with a phosphoric acid solution having a concentration of 30 to 50 wt %;
preparing a mixture by adding sulfuric acid to lithium phosphate mixed with the phosphoric acid solution; and
filtering the mixture and separating the solid lithium sulfate and filtrate.
2 . The method of claim 1 ,
wherein, in the step of heating a lithium-containing ore,
temperature is 1000 to 1250° C.
3 . The method of claim 1 ,
wherein, in the step of preparing an acid product,
the roasting temperature is 150 to 250° C.
4 . The method of claim 1 ,
wherein, in the step of preparing the leachate,
a weight ratio (acidproduct:leachate) of the acid product and the leachate is 1:1 to 1:3.
5 . The method of claim 1 , wherein:
in the step of separating the primary impurities,
20 to 40 g/L of lithium-dissolved lithium hydroxide aqueous solution is added to adjust the pH.
6 . The method of claim 1 , wherein:
in the step of separating the secondary impurities,
sodium carbonate is added to the leachate from which the primary impurities are separated and the leachate is stirred, and then sodium hydroxide is added and the leachate stirred.
7 . The method of claim 6 , wherein:
in the step of separating the secondary impurities,
an equivalent ratio of the secondary impurity and the sodium carbonate (secondary impurity:sodium carbonate) is 1:3 to 1:5.
8 . The method of claim 1 , wherein:
after the step of separating the secondary impurities,
the method further comprises, passing the leachate from which the secondary impurities are separated through an ion exchange resin to remove residual Ca.
9 . The method of claim 1 , wherein:
in the step of obtaining the lithium phosphate,
the basic material controls the pH of the purified leachate to 9 to 12.
10 . The method of claim 1 , wherein:
in the step of obtaining the lithium phosphate,
the phosphorus supply material contains at least one of phosphoric acid, sodium phosphate and lithium phosphate, and
the basic material contains at least one of sodium hydroxide, calcium hydroxide, potassium hydroxide, barium hydroxide, magnesium hydroxide and calcium oxide.
11 . The method of claim 1 , wherein:
in the step of obtaining the solid lithium phosphate,
a remaining filtrate which is caused the solid lithium phosphate extraction is used as the leaching water.
12 . The method of claim 1 , wherein:
in the step of mixing the lithium phosphate with a phosphoric acid solution,
the filtrate is used as the phosphoric acid solution.
13 . The method of claim 1 wherein: in the step of separating into the solid lithium sulfate and filtrate, a total concentration of phosphorus (P) and sulfur (S) in the filtrate is 5 mol/L or more.
14 . The method of claim 1 , wherein:
after the step of obtaining the solid lithium sulfate, the method further comprises:
obtaining an aqueous solution of lithium sulfate by dissolving the solid lithium sulfate in a solvent; and
obtaining an aqueous solution of lithium hydroxide by adding the aqueous solution of lithium sulfate to a bipolar electrodialyzer.
15 . The method of claim 14 , wherein:
in the step of obtaining the aqueous solution of lithium hydroxide,
a desalting solution in which 1.5 to 2.0 g/L of lithium is dissolved is obtained, together with the lithium hydroxide aqueous solution.
16 . The method of claim 15 , wherein:
in the step of obtaining the aqueous solution of lithium sulfate,
the desalting solution is used as the solvent.
17 . The method of claim 14 , wherein:
after the step of obtaining the aqueous lithium hydroxide solution, the method further comprises:
drying the aqueous solution of lithium hydroxide to crystallize; and
obtaining a crystallization filtrate in which the crystallized lithium hydroxide and 33 to 37 g/L of lithium are dissolved.
18 . The method of claim 17 , wherein:
in the step of purifying the leachate,
the crystallization filtrate is used to purify the leachate.
19 . The method of claim 17 , wherein:
in the step of obtaining the aqueous solution of lithium sulfate,
by adding the crystallization filtrate together, the pH of the lithium sulfate aqueous solution is adjusted to 10 or higher.