CN111575504A

CN111575504A - Method for efficiently leaching lithium from lithium-containing claystone

Info

Publication number: CN111575504A
Application number: CN202010472603.7A
Authority: CN
Inventors: 黄苑龄; 杨光龙; 邓强; 张海; 胡万明; 张周位; 杨国彬; 张文兴
Original assignee: Guizhou Precious Metals Mineral Product Resource Integration Utilization Engineering Technology Research Center Co ltd; Guizhou Lithium New Energy Technology Co ltd
Current assignee: Guizhou Precious Metals Mineral Product Resource Integration Utilization Engineering Technology Research Center Co ltd; Guizhou Lithium New Energy Technology Co ltd
Priority date: 2020-05-29
Filing date: 2020-05-29
Publication date: 2020-08-25

Abstract

The invention discloses a method for efficiently leaching lithium from lithium-containing claystone. The method comprises the steps of crushing raw ores, grinding the crushed raw ores by a rod mill, filtering, drying and scattering the crushed raw ores, wherein the raw ores are mixed according to the weight ratio of a sample: mixing concentrated sulfuric acid proportionally, putting into a muffle furnace for heat preservation, taking out the sample for natural cooling and scattering, and then according to the sample: the water is stirred and leached according to the proportion, and the leaching solution is obtained by filtering after stirring. The leaching method has the advantages of less energy consumption, simple process, low production cost and convenience for subsequent industrial production.

Description

Method for efficiently leaching lithium from lithium-containing claystone

Technical Field

The invention relates to a method for efficiently leaching lithium from lithium-containing claystone, belonging to the field of mineral separation.

Background

Lithium and its compounds are important raw materials for the defense industry. In the nuclear industry, lithium is the feedstock for hydrogen bomb and controlled thermal nuclear reactors, as well as a high energy fuel for the aircraft, rocket, submarine and aerospace industries. In the high-altitude airplane, manned spacecraft and submarine sealed cabin, lithium can be used as a carbon dioxide adsorbent. The aluminum lithium and magnesium lithium alloy can be used as structural materials of aerospace planes. In addition, lithium series products are also widely applied to industries such as metallurgy, ceramics, high-energy batteries and the like.

At present, more than 150 lithium-containing minerals are known in the world, and spodumene, lepidolite, petalite, lepidolite, glauconite and the like are common.

The production of lithium salt in China currently forms three production bases of Xinjiang, Sichuan and Jiangxi, the production capacity of the lithium salt is converted into lithium carbonate which reaches more than 2 million tons, the lithium carbonate mainly comes from spodumene, lepidolite and the like, and salt lake type lithium resources are developed and utilized in Tibet and Qinghai at present.

At present, the mineral processing technology of spodumene and lepidolite is researched more in China, common leaching methods comprise a sulfuric acid method, a sulfate method, a chlorination roasting method, a soda press-boiling method and the like, and the technology is mature. The lithium-containing mica in the high-level state adopts a combined roasting-water leaching process, and chloride is added, wherein the roasting temperature is 950 ℃, and the leaching rate is more than 90%. Plum adopts high-temperature roasting for spodumene, roasting again after acid mixing, and a method of neutralization leaching to obtain higher leaching rate. However, the research on the development and utilization of lithium extraction of the lithium-containing claystone is less, and the direct low-temperature roasting acidification method for treating the ore is not reported.

Disclosure of Invention

The invention aims to provide a method for efficiently leaching lithium from lithium-containing claystone, which directly reduces leaching cost by roasting and acidifying at low temperature and lays a good economic foundation for subsequent lithium extraction.

Method for efficiently leaching lithium from lithium-containing claystone, and method for efficiently leaching lithium from lithium-containing claystoneThe main minerals of the raw ore comprise quartz, kaolinite, hectorite, pyrite and the like, wherein Li₂The O grade is 0.3% -0.5%, and the technical problem to be solved by the invention is realized by the following technical scheme, which mainly comprises the following steps:

(1) crushing raw ore to-2 mm;

(2) adding the crushed raw ore into a rod mill for grinding;

(3) filtering and drying the ore sample of the rod mill;

(4) drying and scattering the sample for later use;

(5) according to the sample: mixing concentrated sulfuric acid uniformly in proportion;

(6) putting the uniformly mixed sample into a muffle furnace for heat preservation;

(7) taking out the sample after heat preservation, naturally cooling and scattering;

(8) according to the sample: proportionally stirring and leaching water;

(9) stirring and filtering to obtain the leaching solution.

The ore dressing method provided by the invention has the further preferable technical scheme that: in the step (2), the grinding fineness is 75-85% of-0.038 mm.

The ore dressing method provided by the invention has the further preferable technical scheme that: in the step (5), the adding amount of the concentrated sulfuric acid is 60-80%.

The ore dressing method provided by the invention has the further preferable technical scheme that: in the step (6), the temperature of the muffle furnace is 150-.

The ore dressing method provided by the invention has the further preferable technical scheme that: in the step (8), the sample: water =1:3, stirring speed 400 r/min, stirring temperature 80 ℃, and stirring time 1 h.

The method for efficiently leaching lithium from lithium-containing claystone can obtain Li₂The leaching rate of O is more than 91 percent, the leaching cost is reduced by direct low-temperature roasting and acidification, and a good economic foundation is laid for subsequent lithium extraction.

Drawings

Fig. 1 is a process flow of the method for efficiently leaching lithium from lithium-containing claystone.

Detailed description of the preferred embodiment 1

The present invention will be further described with reference to the following embodiments.

The raw ore is a Guizhou sedimentary lithium ore resource, and the main valuable elements in the raw ore sample are lithium and Li₂The O content is 0.46%, the main minerals comprise lithium chlorite, kaolinite, pyrite, quartz and the like, and the chemical analysis of the main elements of the raw ore is shown in Table 1.

TABLE 1 Multi-element analysis of raw ores

Element(s)	Li₂O	SiO₂	K₂O	Na₂O	MnO₂	TiO₂
							Content/%	0.46	68.34	0.35	0.036	0.005	0.69
Element(s)	Al₂O₃	Fe₂O₃	CaO	MgO	TS	P₂O₅
							Content/%	16.27	3.81	0.29	0.17	1.82	0.078

The process flow diagram is shown in figure 1, and the steps are as follows:

(1) crushing raw ore to-2 mm;

(2) grinding the crushed raw ore in a rod mill to obtain an ore grinding fineness of-0.038 mm 82.96%;

(3) filtering and drying the ore sample of the rod mill;

(4) drying and scattering the sample for later use;

(5) according to the sample: uniformly mixing concentrated sulfuric acid =5:3 in proportion;

(6) putting the uniformly mixed sample into a muffle furnace, and keeping the temperature at 150 ℃ for 4 h;

(8) according to the sample: stirring and leaching with water =1:3, wherein the stirring speed is 400 r/min, the stirring temperature is 80 ℃, and the stirring time is 1 h;

(9) stirring and filtering to obtain the leaching solution.

Finally obtaining a sample Li₂The O leaching rate is a good index of 91.74%.

Detailed description of the preferred embodiment 2

The raw ore is a certain lithium-containing chlorite type alteration residual carbonate rock of Guizhou, wherein the main components are CaO and SiO₂And Al₂O₃Available valuable component is Li₂O, content 0.46%, the ore is the alteration residual structure, block structure. The main components are calcite, quartz and clay minerals, and lithium is mainly present in lithium chlorite. The chemical analysis of the main elements of the raw ore is shown in table 2.

TABLE 2 test results of multielement analysis of the integrated sample

Element/%)	Li₂O	SiO₂	K₂O	Na₂O	MnO₂	TiO₂
							Content (wt.)	0.46	40.96	1.29	0.11	0.02	0.62
Element(s)	Al₂O₃	Fe₂O₃	CaO	MgO	TS	P₂O₅
							Content/%	17.98	5.11	13.08	1.13	3.30	0.07

The process flow diagram is shown in figure 1, and the steps are as follows:

(1) crushing raw ore to-2 mm;

(2) grinding the crushed raw ore in a rod mill to obtain an ore grinding fineness of-0.038 mm 76.94%;

(3) filtering and drying the ore sample of the rod mill;

(4) drying and scattering the sample for later use;

(5) according to the sample: uniformly mixing concentrated sulfuric acid =5:4 in proportion;

(6) putting the uniformly mixed sample into a muffle furnace, and keeping the temperature at 210 ℃ for 1 h;

(9) stirring and filtering to obtain the leaching solution.

Finally obtaining a sample Li₂The O leaching rate is a good index of 92.43%.

Claims

1. A method for efficiently leaching lithium from lithium-containing claystone is characterized by mainly comprising the following steps:

(1) crushing raw ore to-2 mm;

(2) adding the crushed raw ore into a rod mill for grinding;

(3) filtering and drying the ore sample of the rod mill;

(4) drying and scattering the sample for later use;

(8) according to the sample: proportionally stirring and leaching water;

(9) stirring and filtering to obtain the leaching solution.

2. A beneficiation process according to claim 1, characterized by: in the step (2), the grinding fineness is 75-85% of-0.038 mm.

3. A beneficiation process according to claim 1, characterized by: in the step (5), the adding amount of the concentrated sulfuric acid is 60-80% of the total amount of the raw ore.

4. A beneficiation process according to claim 1, characterized by: in the step (6), the temperature of the muffle furnace is 150-.

5. A beneficiation process according to claim 1, characterized by: in the step (8), the sample: water =1:3, stirring speed 400 r/min, stirring temperature 80 ℃, and stirring time 1 h.