CN103101934A

CN103101934A - Method for preparing high-purity lithium carbonate

Info

Publication number: CN103101934A
Application number: CN 201110374234
Authority: CN
Inventors: 肖福常
Original assignee: Individual
Current assignee: Individual
Priority date: 2011-11-09
Filing date: 2011-11-09
Publication date: 2013-05-15

Abstract

The invention discloses a method for preparing high-purity lithium carbonate. The method is characterized by using CO2 generated during hydrolyzation of urea as a CO2 gas source during recrystallization, so that a local reaction of overquick crystallization and separation by directly using CO2 gas is avoided. The lithium carbonate product prepared by using the method comprises large particles and has less possibility of generating secondary aggregation, and foreign ions of a solution system are not contained in the particles, so that the foreign ions are effectively removed, the product quality is improved and the production cost of the product is reduced.

Description

The preparation method of pure Lithium Carbonate

Technical field

The present invention relates to a kind of preparation method of industrial chemicals, especially a kind of preparation method of pure Lithium Carbonate.

Background technology

The lithium formate recrystallization method that Japanese Patent JP57095827 mentions is with thick Li ₂CO ₃Generate HCOOLi with the reaction of highly purified formic acid, during high temperature after dissolving HCOOLi, control suitable temperature and make that HCOOLi is cooling, crystallization, and foreign ion is stayed in solution.Then, HCOOLi is passed into high-purity CO in ammonia alkali solution ₂Gas obtains high-purity Li ₂CO ₃

Summary of the invention

Background technology is used high-purity CO ₂Gas, cost is higher.And, CO ₂Discharge rapidly, reaction not exclusively causes the gas waste.In order to solve the defective of background technology, the present invention adopts following technical scheme to make pure Lithium Carbonate:

1, a kind of preparation method of pure Lithium Carbonate is characterized in that: first technical grade Quilonum Retard raw material is made organic acid lithium solution, then add therein carbon amide solution, thereby be settled out pure Lithium Carbonate.

2, according to the preparation method of technical scheme 1 described pure Lithium Carbonate, it is characterized in that: the temperature that its organic acid lithium solution and its carbon amide solution fully react is 80～90 ℃, and its reaction times is more than 2 hours.

Chemical formula main in above technical scheme is as follows:

Quilonum Retard+formic acid → lithium formate+water+carbon dioxide

Li ₂CO ₃+2HCOOH→2CHLiO ₂+H ₂O+CO ₂↑

Lithium formate+carboxamide+water → Quilonum Retard+volatile salt

2CHLiO ₂+CO(NH ₂) ₂+2H ₂O→Li ₂CO ₃+(NH4) ₂CO ₃

Beneficial effect

A kind of preparation method of pure Lithium Carbonate is characterized in that the CO that uses the carboxamide hydrolysis to produce ₂As CO in recrystallization ₂Direct use CO has been avoided in the source of gas ₂The local reaction that the gas crystallization is too fast.The lithium carbonate product particle that the present invention makes is large, is difficult for Second Aggregation occurs, and the particle internal cause does not contain the foreign ion of solution system.So, effectively remove foreign ion, thereby improved quality product, also reduced the production cost of product.

Embodiment (row)

1, get the Quilonum Retard 100g of technical grade, put into the beaker of a 5000ml, add pure water 3000ml, then to add concentration be 35% formic acid 200ml, insert agitator, be stirred at normal temperatures abundant dissolving, make lithium formate solution.

2, regulate the pH value of above lithium formate solution with lithium hydroxide solution, make them between 9～10.Then, filtering solution, standing 2 hours, stand-by.

3, separately get carboxamide 100g, put into the beaker of another 2000ml, then add entry 800ml, stir, it is fully dissolved, make carbon amide solution.

4, filter carbon amide solution, standing 2 hours, stand-by.

5, the lithium formate solution to 80 that more than the heating, (2) prepare～100 ℃, and under the condition that slowly stirs, the carbon amide solution that adds gradually above (4) to prepare in its lithium formate solution fully reacts more than 2 hours it, until be settled out the Quilonum Retard particle fully.

6, filtering solution takes out Quilonum Retard, with pure water washing Quilonum Retard, after filtering unnecessary moisture.Oven dry Quilonum Retard under 100～105 ℃ of conditions.Then, vacuumize wrapped product with plastics bag.So far, just completed the preparation of pure Lithium Carbonate of the present invention.

Claims

1. the preparation method of a pure Lithium Carbonate, is characterized in that: first technical grade Quilonum Retard raw material is made organic acid lithium solution, then add therein carbon amide solution, thereby be settled out pure Lithium Carbonate.

2. the preparation method of pure Lithium Carbonate according to claim 1, it is characterized in that: the temperature that its organic acid lithium solution and its carbon amide solution fully react is 80～90 ℃, its reaction times is more than 2 hours.