CN108439437B - Method for preparing lithium carbonate by using lepidolite ore - Google Patents
Method for preparing lithium carbonate by using lepidolite ore Download PDFInfo
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- CN108439437B CN108439437B CN201810519044.3A CN201810519044A CN108439437B CN 108439437 B CN108439437 B CN 108439437B CN 201810519044 A CN201810519044 A CN 201810519044A CN 108439437 B CN108439437 B CN 108439437B
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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- C01D15/08—Carbonates; Bicarbonates
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Abstract
The invention discloses a method for preparing lithium carbonate by using lepidolite ore, which comprises the following specific steps: crushing lepidolite ore, putting the crushed lepidolite ore into a sintering furnace, introducing water vapor into the sintering furnace, adding excessive sulfuric acid into the sintering furnace, and filtering the mixture to obtain a first mixture; step two, mixing the first mixture with a cucumber extracting solution, and then processing in an electric field to obtain a second mixture; step three, roasting the second mixture to obtain a third mixture; step four, adding water into the third mixture, heating to boiling, stirring, adding ammonia water while stirring, and filtering to obtain a first filtrate; and step five, adjusting the pH value of the first filtrate, filtering to obtain a second filtrate, adding soluble carbonate into the second filtrate while stirring, continuing stirring after the second filtrate is completely added, then aging for 1.5-2.6 hours, and obtaining a lithium carbonate product after centrifugal separation, countercurrent washing and drying. The method is simple to operate, and the purity of the lithium carbonate in the prepared finished product is high.
Description
Technical Field
The invention relates to the field of lithium carbonate preparation, in particular to a method for preparing lithium carbonate by using lepidolite ore.
Background
Lithium carbonate is a raw material for preparing various lithium compounds, is the product with the largest yield and the widest application in lithium salt products, and is used as a lithium salt
It is widely used in chemical industry, metallurgy, ceramics, medicine, refrigeration and other industries, and can also be used for preparing catalysts for chemical reactions, and is called industrial monosodium glutamate. With the rapid development of low-carbon economy and green new energy industry, particularly with the breakthrough and popularization and application of high-capacity power battery technology, the novel lithium-ion power automobile industry rises rapidly, the lithium-ion power industry which is vigorously developed becomes a common consensus of people, the traditional limitation of industrial monosodium glutamate is brought to the promotion of lithium demand, and the new era of energy metal is met.
The main raw materials for extracting lithium are spodumene, lepidolite, lithia feldspar and salt lake brine. According to different raw materials, the extraction of lithium is divided into two methods of extraction from lithium ore and salt lake brine. The methods for extracting and preparing lithium carbonate from lithium ore are a high-temperature roasting method and a leaching method, and the purity of lithium carbonate in products prepared by the methods is not high, which brings trouble to the preparation of lithium carbonate.
Disclosure of Invention
The invention aims to provide a method for preparing lithium carbonate by using lepidolite ore so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing lithium carbonate by using lepidolite ore comprises the following specific steps:
step one, pretreatment: crushing lepidolite ore to 40-60 meshes, then placing the crushed lepidolite ore into a sintering furnace at 860 ℃ and 930 ℃ for 50-70 minutes, introducing water vapor into the sintering furnace for 10-16 minutes, then adding excessive sulfuric acid into the sintering furnace for defluorination reaction, and filtering the obtained product after the reaction is finished to obtain a first mixture;
step two, mixing the first mixture and the cucumber extracting solution, uniformly ball-milling the mixture, wherein the mass ratio of the cucumber extracting solution to the first mixture is 0.18-0.25:1, and then treating the mixture in an electric field of 1.6-3.3KV for 10-16 minutes to obtain a second mixture;
step three, roasting the second mixture at the temperature of 160-185 ℃ for 30-45 minutes to obtain a third mixture;
step four, adding water with the weight 4-5 times of that of the third mixture into the third mixture, heating to boiling, stirring while heating, adding ammonia water while stirring, adjusting the pH value to 10.5-11.6, continuously stirring for 25-30 minutes after the third mixture is completely added, and filtering to obtain a first filtrate;
and step five, adjusting the pH value of the first filtrate to 5.2-6.5, uniformly stirring, filtering to obtain a second filtrate, adding soluble carbonate into the second filtrate while stirring, wherein the mass ratio of the second filtrate to the soluble carbonate is 2.7-3.4:0.5-0.8, continuously stirring for 50-80 minutes after the second filtrate is completely added, then aging for 1.5-2.6 hours, and obtaining a lithium carbonate product after centrifugal separation, countercurrent washing and drying.
As a further scheme of the invention: the flow rate of the water vapor in the step one is 0.026m3/h-0.038m3/h。
As a further scheme of the invention: the cucumber extract is obtained by soaking fresh cucumber slices in 45-52% ethanol aqueous solution 4-6 times of the cucumber slices by mass and using ultrasonic wave for assistance.
As a further scheme of the invention: the power of the ultrasonic wave assistance is 160-240W, and the frequency is 12-15 KHz.
As a further scheme of the invention: the stirring speed in the step five is 240-300 rpm.
As a further scheme of the invention: in the fifth step, the soluble carbonate comprises at least one of sodium carbonate, potassium carbonate and ammonium carbonate.
As a further scheme of the invention: the mass fraction of the sulfuric acid in the first step is 15-30%, and the mass fraction of the ammonia water in the fourth step is 26-37%.
Compared with the prior art, the invention has the beneficial effects that: the method provided by the invention is simple to operate, is suitable for large-scale industrial development, and the prepared finished product of lithium carbonate has high purity, so that the resource utilization rate is improved, and the use requirements of people can be met.
Detailed Description
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
Example 1
A method for preparing lithium carbonate by using lepidolite ore comprises the following specific steps:
step one, pretreatment: crushing lepidolite ore to 50 meshes, putting the crushed lepidolite ore into a sintering furnace at 880 ℃ for 56 minutes, introducing water vapor into the sintering furnace for 12 minutes, wherein the flow rate of the water vapor is 0.029m3Adding excessive sulfuric acid into the mixture for defluorination reaction, and filtering the mixture after the reaction is finished to obtain a first mixture;
step two, mixing the first mixture and cucumber extract and performing ball milling uniformly, wherein the cucumber extract is obtained by soaking fresh cucumber slices in a 48% ethanol aqueous solution with the weight 4 times that of the cucumber slices and using ultrasonic wave for assistance, the mass ratio of the cucumber extract to the first mixture is 0.22:1, and then treating the cucumber extract and the first mixture in an electric field of 2.4KV for 14 minutes to obtain a second mixture;
step three, roasting the second mixture at 172 ℃ for 34 minutes to obtain a third mixture;
step four, adding water with the weight being 4 times that of the third mixture into the third mixture, heating to boiling, stirring while heating, adding ammonia water while stirring, adjusting the pH value to 10.8, continuously stirring for 28 minutes after the third mixture is completely added, and filtering to obtain a first filtrate;
and step five, adjusting the pH value of the first filtrate to 5.8, uniformly stirring, filtering to obtain a second filtrate, adding soluble carbonate into the second filtrate while stirring, wherein the mass ratio of the second filtrate to the soluble carbonate is 2.8:0.53, continuously stirring for 65 minutes after the second filtrate is completely added, then aging for 1.7 hours, and obtaining a lithium carbonate product after centrifugal separation, countercurrent washing and drying.
Example 2
A method for preparing lithium carbonate by using lepidolite ore comprises the following specific steps:
step one, pretreatment: crushing lepidolite ore to 60 meshes, then placing the crushed lepidolite ore into a sintering furnace at 915 ℃ for 58 minutes, introducing water vapor into the sintering furnace for 14 minutes, then adding excessive sulfuric acid into the sintering furnace for defluorination reaction, and filtering the mixture after the reaction is finished to obtain a first mixture;
step two, mixing the first mixture and cucumber extract and performing ball milling uniformly, wherein the cucumber extract is obtained by soaking fresh cucumber slices in 6 times of ethanol aqueous solution with the mass fraction of 48% and performing ultrasonic assistance, the power of the ultrasonic assistance is 190W, the frequency is 13.4KHz, the mass ratio of the cucumber extract to the first mixture is 0.22:1, and then treating for 14 minutes in an electric field of 2.8KV to obtain a second mixture;
step three, roasting the second mixture at 178 ℃ for 34 minutes to obtain a third mixture;
step four, adding water with the weight being 4 times that of the third mixture into the third mixture, heating to boiling, stirring while heating, adding ammonia water while stirring, adjusting the pH value to 11.3, continuously stirring for 28 minutes after the third mixture is completely added, and filtering to obtain a first filtrate;
and step five, adjusting the pH value of the first filtrate to 5.8, uniformly stirring at a rotating speed of 270rpm, filtering to obtain a second filtrate, adding soluble carbonate into the second filtrate while stirring at a rotating speed of 255rpm, wherein the soluble carbonate comprises a mixture of potassium carbonate and ammonium carbonate, the mass ratio of the second filtrate to the soluble carbonate is 2.96:0.61, continuously stirring at a rotating speed of 285rpm for 66 minutes after the second filtrate is completely added, then aging for 2.4 hours, and obtaining a lithium carbonate product after centrifugal separation, countercurrent washing and drying.
Example 3
A method for preparing lithium carbonate by using lepidolite ore comprises the following specific steps:
step one, pretreatment: crushing lepidolite ore to 40 meshes, putting the crushed lepidolite ore into a sintering furnace at 885 ℃ for 55 minutes, introducing water vapor into the sintering furnace for 14 minutes, wherein the flow rate of the water vapor is 0.035m3Adding excessive sulfuric acid into the mixture for defluorination reaction, wherein the mass fraction of the sulfuric acid is 22%, and filtering the mixture after the reaction is finished to obtain a first mixture;
step two, mixing the first mixture and cucumber extracting solution, performing ball milling uniformly, wherein the mass ratio of the cucumber extracting solution to the first mixture is 0.23:1, and then treating for 14 minutes in an electric field of 2.7KV to obtain a second mixture;
step three, roasting the second mixture at 166 ℃ for 45 minutes to obtain a third mixture;
step four, adding water with the weight being 4 times of that of the third mixture into the third mixture, heating to boiling, stirring while heating, adding ammonia water while stirring, adjusting the pH value to 10.7, wherein the mass fraction of the ammonia water is 36%, continuously stirring for 28 minutes after the ammonia water is completely added, and filtering to obtain a first filtrate;
and step five, adjusting the pH value of the first filtrate to 6.2, uniformly stirring, filtering to obtain a second filtrate, adding potassium carbonate into the second filtrate while stirring, wherein the mass ratio of the second filtrate to the potassium carbonate is 3.24:0.67, continuously stirring for 70 minutes after the second filtrate is completely added, then aging for 2.4 hours, and obtaining a lithium carbonate product after centrifugal separation, countercurrent washing and drying.
Example 4
A method for preparing lithium carbonate by using lepidolite ore comprises the following specific steps:
step one, pretreatment: crushing lepidolite ore to 60 meshes, then placing the crushed lepidolite ore into a sintering furnace at 920 ℃ for 66 minutes, and introducing water vapor into the sintering furnace for 13 minutes, wherein the flow rate of the water vapor is 0.031m3Adding excessive sulfuric acid into the mixture for defluorination reaction, wherein the mass fraction of the sulfuric acid is 23%, and filtering the mixture after the reaction is finished to obtain a first mixture;
step two, mixing the first mixture and cucumber extract, uniformly ball-milling, soaking fresh cucumber slices in 5 times of ethanol aqueous solution with the mass fraction of 50% by weight of the cucumber extract, and performing ultrasonic assistance to obtain the cucumber extract, wherein the ultrasonic assistance power is 225W, the frequency is 14.2KHz, the mass ratio of the cucumber extract to the first mixture is 0.23:1, and then treating in an electric field of 2.7KV for 15 minutes to obtain a second mixture;
step three, roasting the second mixture at 180 ℃ for 42 minutes to obtain a third mixture;
step four, adding water which is 5 times of the third mixture in weight, heating to boiling, stirring while heating, adding ammonia water while stirring, adjusting the pH value to 11.3, keeping the mass fraction of the ammonia water at 34%, continuing stirring for 26 minutes after the ammonia water is completely added, and filtering to obtain a first filtrate;
and step five, adjusting the pH value of the first filtrate to 5.8, uniformly stirring at the rotation speed of 285rpm, filtering to obtain a second filtrate, adding soluble carbonate into the second filtrate while stirring at the rotation speed of 300rpm, wherein the soluble carbonate comprises a mixture of sodium carbonate, potassium carbonate and ammonium carbonate, the mass ratio of the second filtrate to the soluble carbonate is 3.16:0.75, continuously stirring at the rotation speed of 240rpm for 75 minutes after the second filtrate is completely added, then aging for 2.4 hours, and obtaining a lithium carbonate product after centrifugal separation, countercurrent washing and drying.
Comparative example 1
Lithium carbonate is prepared by the existing method.
The products obtained in examples 1 to 4 and comparative example 1 were subjected to composition testing to obtain the mass fraction of lithium carbonate, and the test data are shown in table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | |
| Lithium carbonate/%) | 98.76 | 99.21 | 99.42 | 98.93 | 93.45 |
As can be seen from Table 1, the purity of lithium carbonate in the finished products prepared by the methods of examples 1-4 was over 98.6%, which is much higher than 93.45% of comparative example 1, and the product purity was high.
According to the invention, high-temperature roasting is carried out, then water vapor and excessive sulfuric acid are sequentially introduced for defluorination, then the cucumber extract is uniformly ball-milled and treated in an electric field, then low-temperature roasting is carried out, iron ions and aluminum ions are removed by ammonia water, and finally lithium carbonate is generated with soluble carbonate.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (2)
1. A method for preparing lithium carbonate by using lepidolite ore is characterized by comprising the following specific steps:
step one, pretreatment: crushing lepidolite ore to 40-60 meshes, putting the crushed lepidolite ore into a sintering furnace at 860 ℃ and 930 ℃ for 50-70 minutes, and introducing water vapor into the sintering furnace for 10-16 minutes, wherein the flow rate of the water vapor is 0.026m3/h-0.038m3Adding excessive sulfuric acid into the mixture for defluorination reaction, wherein the mass fraction of the sulfuric acid is 15-30%, and filtering the mixture after the reaction is finished to obtain a first mixture;
step two, mixing the first mixture and cucumber extract and performing ball milling uniformly, wherein the mass ratio of the cucumber extract to the first mixture is 0.18-0.25:1, then treating the mixture in an electric field of 1.6-3.3KV for 10-16 minutes to obtain a second mixture, wherein the cucumber extract is obtained by soaking fresh cucumber slices in 45-52% ethanol aqueous solution which is 4-6 times of the weight of the cucumber slices and adopting ultrasonic assistance, the power of the ultrasonic assistance is 160-240W, and the frequency is 12-15 KHz;
step three, roasting the second mixture at the temperature of 160-185 ℃ for 30-45 minutes to obtain a third mixture;
step four, adding water with the weight being 4-5 times of that of the third mixture into the third mixture, heating to boiling, stirring while heating, adding ammonia water while stirring, adjusting the pH value to 10.5-11.6, wherein the mass fraction of the ammonia water is 26-37%, continuously stirring for 25-30 minutes after the ammonia water is completely added, and filtering to obtain a first filtrate;
and step five, adjusting the pH value of the first filtrate to be 5.2-6.5, uniformly stirring, filtering to obtain a second filtrate, adding soluble carbonate into the second filtrate while stirring at the stirring speed of 240-3.4 rpm, wherein the mass ratio of the second filtrate to the soluble carbonate is 2.7-3.4:0.5-0.8, continuously stirring for 50-80 minutes after the second filtrate is completely added, then aging for 1.5-2.6 hours, and obtaining a lithium carbonate product after centrifugal separation, countercurrent washing and drying.
2. The method for preparing lithium carbonate by using lepidolite ore according to claim 1, wherein the soluble carbonate in the fifth step includes at least one of sodium carbonate, potassium carbonate and ammonium carbonate.
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| CN103145158B (en) * | 2013-02-28 | 2014-11-05 | 江西赣锋锂业股份有限公司 | Method for preparing lithium carbonate from lepidolite through sulfuric acid roasting method |
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