CN-118477602-B - Device and method for preparing lithium carbonate micro powder

CN118477602BCN 118477602 BCN118477602 BCN 118477602BCN-118477602-B

Abstract

The invention provides a device and a method for preparing lithium carbonate micro powder, belonging to the field of lithium carbonate preparation, the preparation device comprises a carbonization reaction box, carbon dioxide bubble generating equipment and a feeder which are communicated with the carbonization reaction box, and stirring equipment and foam scraping equipment which are arranged in the carbonization reaction box. The preparation method comprises the steps of mixing and pumping lithium hydroxide solution and a foaming agent into a carbonization reaction box, pumping micro-nano-level CO 2 bubbles into the carbonization reaction box by carbon dioxide bubble generating equipment, starting stirring equipment, starting foam scraping equipment after carbonization is finished, scraping and collecting lithium carbonate micro-powder suspension, and collecting lithium carbonate large-particle suspension at the bottom of the carbonization reaction box. According to the invention, a large amount of bubbles are generated in the carbonization process of the lithium hydroxide solution by adding the foaming agent, the agglomeration and crystallization growth phenomena of lithium carbonate are inhibited, the small-particle-size lithium carbonate micro powder is carried out by virtue of the bubbles, and a small part of large-particle-size lithium carbonate is precipitated at the bottom of the device, so that the preparation of the lithium carbonate micro powder and the large-particle-size lithium carbonate product is realized.

Inventors

HU QIYANG
JIA GUIBIN
HU ZEXIANG
HE DONGMEI
HUANG HAO

Assignees

江西云威新材料股份有限公司
九江云威锂业有限公司

Dates

Publication Date: 20260508
Application Date: 20240507

Claims (3)

1. A method for preparing lithium carbonate micropowder, characterized in that the method comprises the following steps: preparing raw materials, preparing lithium hydroxide and water into a lithium hydroxide solution in a feeder according to a proportion, and mixing the lithium hydroxide solution with a foaming agent; Mixing and pumping a lithium hydroxide solution and a foaming agent into a carbonization reaction tank, pumping micro-nano CO 2 bubbles into the carbonization reaction tank by carbon dioxide bubble generating equipment, starting stirring equipment while performing carbonization reaction, and performing carbonization reaction on the lithium hydroxide solution and CO 2 to generate lithium carbonate solid, wherein the lithium carbonate solid mainly exists in the form of lithium carbonate micro powder under the action of foam, and a small amount of lithium carbonate solid is aggregated and deposited at the bottom of the carbonization reaction tank to form lithium carbonate large particles; and (3) collecting lithium carbonate, suspending lithium carbonate micro powder on the surface of the liquid surface of the carbonization reaction tank under the action of foam to form lithium carbonate micro powder suspension, starting foam scraping equipment after carbonization is finished, scraping the lithium carbonate micro powder suspension outside the carbonization reaction tank and collecting, collecting lithium carbonate large particle suspension at the bottom of the carbonization reaction tank, and simultaneously preparing lithium carbonate micro powder with the particle size of 1-3 mu m and lithium carbonate large particle products with the particle size of 5-7 mu m.
2. The method of preparing lithium carbonate micropowder according to claim 1, further comprising: The lithium carbonate micro powder suspension is filtered by a micro-pore filter device, and the wet lithium carbonate micro powder is collected and dried and crushed to prepare lithium carbonate micro powder; and filtering the lithium carbonate large-particle suspension by a centrifugal device, collecting the lithium carbonate large-particle wet material, and drying and crushing to obtain lithium carbonate powder.
3. The method for preparing the lithium carbonate micro powder according to claim 1 is characterized in that the foaming agent is water-soluble and has a foaming effect under alkaline conditions, the foaming agent is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and sodium fatty alcohol polyoxyethylene ether sulfate, and the amount of the foaming agent is 1-10 g/kg of lithium hydroxide dry material.

Description

Device and method for preparing lithium carbonate micro powder Technical Field The invention belongs to the technical field of lithium carbonate preparation, and particularly relates to a device and a method for preparing lithium carbonate micro powder. Background Lithium is currently the lightest known metal and has unique and excellent physicochemical properties, and lithium and compounds thereof are widely applied to ceramics, glass, aerospace materials, nuclear industry and new energy materials, and in recent years, the price of lithium is rising due to the rapid development of new energy automobile industry. Lithium carbonate is one of the basic compounds of lithium, can be converted into various industrial raw materials of lithium, and is also a lithium product which is mainly required in the lithium ion battery industry. Industrial production sources of lithium carbonate include lithium ore (spodumene and lepidolite) extraction and salt lake brine extraction, and in order to produce lithium carbonate, the rear end of the process flow of the two is to carry out carbonization operation on extracted refined lithium salt solution (lithium sulfate, lithium chloride, lithium hydroxide solution and the like) to prepare lithium carbonate, the carbonization operation is usually carried out by adopting a mode of adding carbonate, and in order to avoid introducing new impurities, a mode of introducing carbon dioxide gas into the lithium hydroxide solution is generally adopted to prepare lithium carbonate. The application of lithium carbonate in the aspect of lithium ion battery materials is mainly used as a lithium source of a positive electrode material and an additive of electrolyte, and the lithium carbonate product is required to have smaller particle size, so that lithium carbonate micro powder is a main form requirement, and the preparation method of the lithium carbonate micro powder at present usually carries out repeated grinding and crushing on the prepared large-particle-size lithium carbonate product until the particle size reaches the requirement, and the preparation method has long working procedure and high cost. At present, the carbonization method is used for preparing lithium carbonate, the phenomena of crystal growth and powder agglomeration are very easy to occur in the carbonization process, the particle size of the prepared lithium carbonate micro powder is larger, the particle size of the product is reduced by an additional crushing procedure in the follow-up process, and the complexity and the cost of the process are greatly increased. Disclosure of Invention In view of the above, the present invention aims to provide a device and a method for preparing lithium carbonate micropowder, which aims to solve at least one technical problem in the background art. The invention is realized in the following way: An apparatus for preparing lithium carbonate micropowder, comprising: The carbonization reaction box is characterized in that a carbonization reaction is carried out on the lithium hydroxide solution and carbon dioxide in the carbonization reaction box to form foam, and the foam reacts to form lithium carbonate micro powder suspension and lithium carbonate large particle suspension; The carbon dioxide bubble generation equipment is used for preparing carbon dioxide gas into micro-nano-level bubbles and conveying the micro-nano-level bubbles into the carbonization reaction box, and the carbon dioxide bubble generation equipment is communicated with the side wall of the carbonization reaction box; A feeder for mixing the lithium hydroxide solution with the foaming agent and pumping the mixture into the carbonization reaction tank, wherein the feeder is communicated with a feed inlet of the carbonization reaction tank; The stirring equipment is vertically arranged in the carbonization reaction box and used for accelerating the carbonization reaction rate; The foam scraping equipment is arranged inside the carbonization reaction tank and above the stirring equipment, and is used for scraping lithium carbonate micro powder suspension out of the carbonization reaction tank, wherein the lithium carbonate micro powder suspension is foam for adsorbing lithium carbonate micro particles. Further, a pH sensor is installed inside the carbonization reaction tank. Further, the carbon dioxide bubble generating device comprises a CO 2 storage container, an inflator pump and a bubble generator which are sequentially connected through pipelines, and an outlet of the bubble generator is communicated with the side wall of the carbonization reaction box. The carbon dioxide bubble generating device has the working process that an inflator pump introduces carbon dioxide gas into a bubble generator from a CO 2 storage container to be mixed with water to form micro-nano-level CO 2 bubbles, and then the micro-nano-level CO 2 bubbles are conveyed to a microporous foaming mesh enclosure through a pipeline and uniform