Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing lithium carbonate through fluorinating and calcining spodumene and extracting lithium

A technology of spodumene and lithium carbonate, applied in the field of spodumene, can solve the problems of high energy consumption and low utilization rate of ore, and achieve the effect of high product purity, suitable for large-scale production and low environmental pollution

Inactive Publication Date: 2017-10-20
WUHAN UNIV OF TECH
View PDF4 Cites 14 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The problem to be solved by the present invention is: aiming at the disadvantages of high energy consumption of sulfuric acid roasting and limestone roasting and low utilization rate of ore, to provide a kind of unstable fluorine-containing additive to convert a large amount of silicon dioxide in the ore into added value high silica and NH 4 F, Fluorine can be used for recycling; method of re-extracting exposed lithium oxide and producing lithium carbonate, which has no requirements on ore grade

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing lithium carbonate through fluorinating and calcining spodumene and extracting lithium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: mixed material roasting process

[0032]Take 20.029g of spodumene particles and 29.4g of ammonium fluoride (1.0 times the theoretical amount), mix the materials evenly, grind to 100 mesh and compact. Put the mixed material into a muffle furnace, heat up to 300°C for 30 minutes, and roast for 3 hours to obtain 20.746 g of solid slag, which is a secondary ore that removes a large amount of silica and exposes lithium oxide; SiO 2 Content 20.847% (SiO in raw ore 2 Content 59.607%).

[0033] Take 30.060g of spodumene particles, 61.745g of a mixture of ammonium fluoride and lithium fluoride (1.4 times the theoretical amount), mix the materials evenly, grind to 100 mesh and compact. Put the mixed material into the muffle furnace, raise the temperature to 300°C for 30 minutes, and roast for 3 hours to obtain 35.273 g of solid slag; SiO 2 Content 21.393% (SiO in raw ore 2 Content 59.607%), F content is 42.583%.

[0034] Take 20.029g of spodumene particles and ...

Embodiment 4

[0037] Embodiment 4: the preparation technology of lithium sulfate solution

[0038] Take 10g of secondary ore roasted at 400°C for 3 hours with 1.2 times the theoretical amount of ammonium fluoride, but it cannot be wetted well and forms mud, so the next experiment cannot be carried out.

[0039] Take 10g of secondary ore roasted at 400°C for 3h with 1.2 times the theoretical amount of ammonium fluoride, add 30mL of distilled water, and stir at room temperature for 1h; successively wash the slag and filter to obtain a lithium sulfate solution with a lithium oxide leaching rate of 4.43%.

[0040] Take 10 g of secondary ore roasted at 400°C for 3 h with 1.2 times the theoretical amount of ammonium fluoride, add 50 mL of distilled water, and stir for 1 h at room temperature; successively wash the slag and filter to obtain a lithium sulfate solution with a lithium oxide leaching rate of 4.17%.

[0041] Take 10g of secondary ore roasted at 400°C for 3h with 1.2 times the theoretic...

Embodiment 7

[0048] Embodiment 7: the preparation technology of lithium carbonate product

[0049] Take 200mL of lithium sulfate mother liquor with a lithium content of 421.9μg / ml, heat and concentrate, and continue heating to 85°C, add sodium hydroxide solution, stir while adding, and measure the pH of the solution with pH test paper; when pH=7, continue Add saturated sodium carbonate solution to pH = 10; filter while hot to remove the formed Fe and Mg precipitates, keep the temperature at 85°C, and add sodium carbonate particles until pH = 14, centrifuge for 10 minutes to obtain the crude lithium carbonate product, after drying Sent for component detection, the purity of lithium carbonate was 96.4%.

[0050] In the above embodiments, the raw materials can be ground by a ball mill. The ball mill adopts LGB04 omnidirectional planetary ball mill.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The method for extracting lithium from spodumene by fluorination roasting provided by the present invention includes the following steps: 1) taking 50-200 mesh spodumene, adding a fluorine-containing compound in a molar ratio of 1:1-1:3, and mixing Grind to 100~200 meshes uniformly, roast at 200~600℃, and the reaction time is 2~5h to obtain slag; 2) Add 1~6mol / L at a liquid-solid ratio of 1:1~1:5 at 30~90℃ 3) Evaporating and concentrating the lithium sulfate mother liquor, adding hydrogen peroxide, basic compounds (one or more of NaOH, Na CO , ammonia water, etc.) in turn, precipitating the Al3+, Mg2+, Fe3+, etc., add soluble carbonate (one or more of Na2CO3, K2CO3, etc.) to the filtrate, heat to 50-100 ° C to precipitate lithium, filter and wash to obtain lithium carbonate with a purity of more than 96.4%. In addition, SiF4 can be absorbed and aged to obtain high-purity silica and NH4F during the roasting process. The invention has simple equipment requirements, low energy consumption, and is suitable for industrial production.

Description

technical field [0001] The invention relates to spodumene, a method for preparing lithium carbonate by roasting spodumene with an unstable compound containing fluorine and extracting lithium. Background technique [0002] Lithium (Li) is a silver-white metal element, soft and the least dense metal. Because lithium has a high charge density and a stable helium-type double electron layer, it is easy for lithium to polarize other molecules or ions, but itself is not easily polarized. It is mostly used in atomic reactors, light alloys and batteries. At present, the utilization rate of soluble lithium resources in my country is not high, and the utilization is mainly based on insoluble lithium resources. There are many ways to extract lithium from spodumene, such as limestone roasting, chlorination roasting, sulfuric acid roasting, etc. In comparison, the fluorination roasting method can use cheap and unstable fluorine-containing compounds, and the temperature is lower than oth...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08C01B33/18C05D9/00C03C1/00C01D5/16
CPCC01D15/08C01B33/184C01D5/16C01P2006/80C03C1/002C05D9/00
Inventor 张光旭龚鹏韩洋
Owner WUHAN UNIV OF TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com