CN106115746A - The technique that a kind of lepidolite prepares lithium fluoride - Google Patents
The technique that a kind of lepidolite prepares lithium fluoride Download PDFInfo
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- CN106115746A CN106115746A CN201610080309.5A CN201610080309A CN106115746A CN 106115746 A CN106115746 A CN 106115746A CN 201610080309 A CN201610080309 A CN 201610080309A CN 106115746 A CN106115746 A CN 106115746A
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Abstract
The present invention provides the technique that a kind of lepidolite prepares lithium fluoride, described lepidolite is prepared the technique of lithium fluoride and is included lepidolite acidifying, grog water logging, heavy aluminum and concentrate the processing steps such as sinker, wherein lepidolite acidification technique step includes: the gas water that described lepidolite acidification reaction produces absorbs and ammonification, obtains ammonium fluoride solution；It can thus be appreciated that, the present invention makes full use of the elemental lithium in lepidolite and fluorine element generates lithium fluoride, without additionally introducing fluorine-containing raw material in the preparation technology of whole lithium fluoride, the technique relatively being produced lithium fluoride by Fluohydric acid. and lithium carbonate, low cost, flow process is short and simple to operate, meanwhile, the raw material ratio of each step of preparation technology and response time etc. are accurately controlled by the present invention, and reaction efficiency is higher, therefore, the present invention can solve the problem that prior art production cost is higher.
Description
Technical field
The present invention relates to a kind of field of ore extraction, be specifically related to the technique that a kind of lepidolite prepares lithium fluoride.
Background technology
Lithium fluoride is a kind of alkali halide, and molecular formula is LiF, white powder or cubic crystal, is insoluble in water, insoluble in alcohol, is dissolved in acid, is widely used in the fields such as nuclear industry, porcelain enamel industry, optical glass manufacture, desiccant and flux.Concrete, lithium fluoride can make electrolyte components in Aluminium Industry, can improve electrical conductivity and current efficiency；Neutron shielding material can be used as in atomic energy industry, solvent can be used as in fusedsalt reactor；The transparency window of ultraviolet can be used as in optical material.High purity lithium fluoride can be additionally used in lithium fluoride glass processed, makes spectrometer and the prism of X ray monochromator.Meanwhile, battery-grade lithium fluoride still produces one of necessary raw material of lithium ion battery common electrolyte lithium hexafluoro phosphate.Along with the high speed development of the high-technology fields such as aluminium lithium alloy, lithium battery, nuclear fusion, the demand of lithium fluoride is also being strengthened by modern industry day by day.
The method of industrial production lithium fluoride mainly has neutralisation and two kinds of methods of double decomposition, and double decomposition production lithium fluoride, mainly by ammonium fluoride and lithium carbonate or Lithium hydrate metathesis reaction, through filtering, be dried and obtaining lithium fluoride.This kind of process is easily controllable, but it is too much to there is Mother liquid, and environmental protection pressure is relatively big and in product, impurity content crosses high shortcomings.Therefore, current commercial production many employings neutralisation production lithium fluoride, neutralisation is solid lithium carbonate or Lithium hydrate to be added in hydrogen fluoride solution, is allowed to reaction and separates out lithium fluoride, through filtering, after drying, is evaporated to dryness and prepares in platinum ware or lead ware.
Neutralisation is used to prepare lithium fluoride, although it is simple to operate, but there is following shortcomings: the shortcomings such as the complex process of preparation, equipment manufacturing cost are high, energy expenditure is high, reaction efficiency is low, product impurity content is high, the cost ultimately resulting in lithium fluoride production remains high, it is impossible to meet the use demand that modern industry is growing to lithium fluoride.
Summary of the invention
The invention provides a kind of process route being prepared lithium fluoride by lepidolite, solve the technical problem that in prior art, the production technology of lithium fluoride is relatively costly.The present invention directly utilizes lithium sulfate solution and prepares lithium fluoride with ammonium fluoride solution reaction, and the lithium in Ore and fluorine can be comprehensively utilized, the most first prepare lithium carbonate compared to current production technology to react with Fluohydric acid. the most again, the present invention utilizes route simple, cost is relatively low, and social meaning and economic benefit are the most great.
For solving above-mentioned technical problem, the technical scheme is that
A kind of lepidolite prepares the technique of lithium fluoride, and described technique comprises the steps: lepidolite acidifying, grog water logging, heavy aluminum, purifies and concentrate sinker.
Lepidolite of the present invention prepares the technique of lithium fluoride, comprises the steps:
1): lepidolite is acidified: lepidolite is obtained grog with sulfuric acid reaction；
2): grog water logging: described grog is mixed with water leaching, after solid-liquor separation, obtains leaching liquid；
3): heavy aluminum: in described leaching liquid, add one or more in sodium, potassium or ammonium sulfate and arbitrarily ratio mixing, be cooled to less than-5 DEG C, by solid-liquor separation, obtain low aluminium sulfate solution；
4): purify: regulate the PH=8-12 of above-mentioned low aluminium sulfate solution, the impurity such as calcium, magnesium, ferrum are removed, it is thus achieved that pure lithium sulfate scavenging solution；
5): concentrate sinker: the lithium oxide content in step 4) sulfate liquor is concentrated into 35-60g/L, add ammonium fluoride solution and carry out sinker, then by solid-liquor separation, obtain mother solution and lithium fluoride crude product, described lithium fluoride crude product is washed, dries, obtain lithium fluoride product.The ammonium fluoride solution mass concentration added in the present invention is more than 15%, and in the ammonium fluoride added, fluorine is 1.1:1 with the mol ratio of lithium.The double salt that Chen Lv workshop section is formed can become potassium-ammonium sulfate mixing fertilizer and the hydrogen aluminum etc. of high added value with deep processing, effectively alleviates China's agricultural demand to potassium ammonium fertilizer.
In described step 1), the reaction temperature of acidifying is 200-300 DEG C, and the response time is 0.5-8 hour.
In described step 1), the mass concentration of sulphuric acid is more than or equal to 50%, and lepidolite and sulphuric acid are according to mass ratio 1:0.6-1.5.
Described step 2) described in the liquid-solid ratio of grog and water be 1～4:1, leaching time is 0.5 3 hours.
In described step 3), sulfate is one or more arbitrarily ratio mixing of sodium sulfate, potassium sulfate, ammonium sulfate, and the sulfate of addition is 1:1 with the mol ratio of aluminum sulfate in leaching liquid.
The reaction temperature adding ammonium fluoride solution sinker in described step 5) is 30-80 DEG C, and the response time is 0.1-3 hour
The gas water that described step 1) acidification reaction produces absorbs and obtains hexafluosilicic acid, then ammonification, obtains ammonium fluoride solution, and obtained ammonium fluoride solution is in the concentration sinker of step 5).The present invention makes full use of the elemental lithium in lepidolite and fluorine element generates lithium fluoride, and without additionally introducing fluorine-containing raw material in the preparation technology of whole lithium fluoride, the technique relatively being produced lithium fluoride by Fluohydric acid. and lithium carbonate, low cost, flow process is short and simple to operate.
Mother solution in step 5) of the present invention adds in step 3).Double salt can be formed with aluminum sulfate and effectively remove impurity salt, can effectively save the alkaline matter used by remove impurity workshop section.
Beneficial effects of the present invention: the present invention provides the technique that a kind of lepidolite prepares lithium fluoride, described lepidolite is prepared the technique of lithium fluoride and is included lepidolite acidifying, grog water logging, heavy aluminum, purifies and concentrate sinker processing step, the lithium fluoride that this technique is prepared meets the growing raw materials requirement of lithium battery electrolytes lithium hexafluoro phosphate, the most great for China's development lithium electricity new forms of energy meaning；Wherein lepidolite acidification technique step includes: the gas water that described lepidolite acidification reaction produces absorbs and ammonification, obtains ammonium fluoride solution；Corresponding, concentrate sinker processing step to include: carry out sinker by sulfate liquor adds the described ammonium fluoride solution obtained in step 1), the present invention makes full use of the elemental lithium in lepidolite and fluorine element generates lithium fluoride, without additionally introducing fluorine-containing raw material in the preparation technology of whole lithium fluoride, the technique relatively being produced lithium fluoride by Fluohydric acid. with lithium carbonate, low cost, flow process is short and simple to operate, simultaneously, the raw material ratio of each step of preparation technology and response time etc. are accurately controlled by the present invention, reaction efficiency is higher, therefore, the present invention can solve the problem that prior art production cost is higher.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Illustrating exemplary embodiment in detail here in conjunction with accompanying drawing, its example represents in the accompanying drawings.
Embodiment
1
A kind of lepidolite prepares the technique of lithium fluoride, is realized by following steps:
1) lepidolite acidifying, puts in reactor by lepidolite and 50% sulphuric acid according to mass ratio 1:1.5, reaction temperature 300 DEG C, 0.5 hour response time；The gas that reaction produces absorbs with water in time；
2) grog water logging, after being stirred 3 hours according to liquid-solid ratio 1:1 water extraction by grog good for lepidolite acidification reaction, solid-liquor separation obtains leaching liquid；
3) heavy aluminum, the arbitrarily ratio of one or more added in above-mentioned leaching liquid in sodium, potassium, ammonium sulfate is 1:1 except aluminum, addition sulfate with the mol ratio of aluminum sulfate, is cooled to less than-5 DEG C, and solid-liquor separation obtains low aluminium sulfate solution；
4) purify, regulate above-mentioned low aluminium sulfate solution PH=8-12, remove the impurity such as calcium, magnesium, ferrum, it is thus achieved that pure lithium sulfate scavenging solution；
5) sinker is concentrated, above-mentioned lithium sulfate scavenging solution is concentrated into lithium oxide content 35g/L, add ammonium fluoride solution sinker, temperature controls at 30 80 DEG C, react 3 hours, obtain lithium fluoride crude product after solid-liquor separation, after washing, drying, obtain lithium fluoride product, the mother solution containing sulfate such as sodium, potassium, ammoniums is returned step 3).
Embodiment
2
A kind of lepidolite prepares the technique of lithium fluoride, is realized by following steps:
1) lepidolite acidifying, puts in reactor by lepidolite and 70% sulphuric acid according to mass ratio 1:1.1, reaction temperature 250 DEG C, 4 hours response time；The gas that reaction produces absorbs with water in time；
2) grog water logging, after being stirred 2 hours according to liquid-solid ratio 2:1 water extraction by grog good for lepidolite acidification reaction, solid-liquor separation obtains leaching liquid；
3) heavy aluminum, the arbitrarily ratio of one or more added in above-mentioned leaching liquid in sodium, potassium, ammonium sulfate is 1:1 except aluminum, addition sulfate with the mol ratio of aluminum sulfate, is cooled to less than-5 DEG C, and solid-liquor separation obtains low aluminium sulfate solution；
4) purify, regulate above-mentioned low aluminium sulfate solution PH=8-12, remove the impurity such as calcium, magnesium, ferrum, it is thus achieved that pure lithium sulfate scavenging solution；
5) sinker is concentrated, above-mentioned lithium sulfate scavenging solution is concentrated into lithium oxide content 50g/L, add ammonium fluoride solution sinker, temperature controls at 30 80 DEG C, react 1.5 hours, obtain lithium fluoride crude product after solid-liquor separation, after washing, drying, obtain lithium fluoride product, the mother solution containing sulfate such as sodium, potassium, ammoniums is returned step 3).
Embodiment
3
A kind of lepidolite prepares the technique of lithium fluoride, is realized by following steps:
1) lepidolite acidifying, puts in reactor by lepidolite and 98% sulphuric acid according to mass ratio 1:0.77, reaction temperature 200 DEG C, 6 hours response time；The gas that reaction produces absorbs with water in time；
2) grog water logging, after being stirred 0.5 hour according to liquid-solid ratio 4:1 water extraction by grog good for lepidolite acidification reaction, solid-liquor separation obtains leaching liquid；
3) heavy aluminum, the arbitrarily ratio of one or more added in above-mentioned leaching liquid in sodium, potassium, ammonium sulfate is 1:1 except aluminum, addition sulfate with the mol ratio of aluminum sulfate, is cooled to less than-5 DEG C, and solid-liquor separation obtains low aluminium sulfate solution；
4) purify, regulate above-mentioned low aluminium sulfate solution PH=8-12 and remove the impurity such as calcium, magnesium, ferrum, it is thus achieved that pure lithium sulfate scavenging solution；
5) sinker is concentrated, above-mentioned lithium sulfate scavenging solution is concentrated into lithium oxide content 35g/L, add ammonium fluoride solution sinker, temperature controls at 30 80 DEG C, react 0.5 hour, obtain lithium fluoride crude product after solid-liquor separation, after washing, drying, obtain lithium fluoride product, the mother solution containing sulfate such as sodium, potassium, ammoniums is returned step 3).
Embodiment
4
The present embodiment provides a kind of lepidolite to prepare the technique of lithium fluoride, and described lepidolite is prepared the technique of lithium fluoride and comprised the following steps:
1) lepidolite acidifying: lepidolite and 98% sulphuric acid are added in reactor according to the mass ratio of 1:0.6, obtain grog, the gas water that described lepidolite acidification reaction produces absorbs and ammonification, obtain ammonium fluoride solution, wherein, the reaction temperature of described acidifying is 200 DEG C, and the response time of acidifying is 6 hours；
2) grog water logging: after being stirred 0.5 hour according to liquid-solid ratio 4:1 water extraction by grog good for lepidolite acidification reaction, solid-liquor separation obtains leaching liquid；
3) heavy aluminum: the arbitrarily ratio of one or more added in above-mentioned leaching liquid in sodium, potassium, ammonium sulfate is 1:1 except aluminum, addition sulfate with the mol ratio of aluminum sulfate, is cooled to less than-5 DEG C, and solid-liquor separation obtains low aluminium sulfate solution；
4) purify: regulate above-mentioned low aluminium sulfate solution PH=8-12 and remove the impurity such as calcium, magnesium, ferrum, it is thus achieved that pure lithium sulfate scavenging solution；
5) sinker is concentrated: the lithium oxide content in sulfate liquor is concentrated into 40g/L, add the described ammonium fluoride solution obtained in step S51 and carry out sinker, the reaction temperature of described sinker reaction is 45 DEG C, the response time of described sinker be 2.5 hours again by solid-liquor separation, obtain mother solution and lithium fluoride crude product, described lithium fluoride crude product is washed, dries, obtain lithium fluoride product.
Embodiment
5
The present embodiment provides a kind of lepidolite to prepare the technique of lithium fluoride, and described lepidolite is prepared the technique of lithium fluoride and comprised the following steps:
1) lepidolite acidifying: lepidolite and 98% sulphuric acid are added in reactor according to the mass ratio of 1:0.8, obtain grog, the gas water that described lepidolite acidification reaction produces absorbs and ammonification, obtain ammonium fluoride solution, wherein, the reaction temperature of described acidifying is 250 DEG C, and the response time of acidifying is 3 hours；
2) grog water logging: after being stirred 0.5 hour according to liquid-solid ratio 4:1 water extraction by grog good for lepidolite acidification reaction, solid-liquor separation obtains leaching liquid；
3) heavy aluminum: the arbitrarily ratio of one or more added in above-mentioned leaching liquid in sodium, potassium, ammonium sulfate is 1:1 except aluminum, addition sulfate with the mol ratio of aluminum sulfate, is cooled to less than-5 DEG C, and solid-liquor separation obtains low aluminium sulfate solution；
4) purify: regulate above-mentioned low aluminium sulfate solution PH=8-12 and remove the impurity such as calcium, magnesium, ferrum, it is thus achieved that pure lithium sulfate scavenging solution；
5) sinker is concentrated: the lithium oxide content in sulfate liquor is concentrated into 50g/L, add the described ammonium fluoride solution obtained in step S61 and carry out sinker, the reaction temperature of described sinker reaction is 45 DEG C, the response time of described sinker be 1.5 hours again by solid-liquor separation, obtain mother solution and lithium fluoride crude product, described lithium fluoride crude product is washed, dries, obtain lithium fluoride product.
Embodiment
6
The present embodiment provides a kind of lepidolite to prepare the technique of lithium fluoride, and described lepidolite is prepared the technique of lithium fluoride and comprised the following steps:
1) lepidolite acidifying: lepidolite and 98% sulphuric acid are added in reactor according to the mass ratio of 1:1.1, obtain grog, the gas water that described lepidolite acidification reaction produces absorbs and ammonification, obtain ammonium fluoride solution, wherein, the reaction temperature of described acidifying is 250 DEG C, and the response time of acidifying is 1.5 hours；
2) grog water logging: after being stirred 0.5 hour according to liquid-solid ratio 3:1 water extraction by grog good for lepidolite acidification reaction, solid-liquor separation obtains leaching liquid；
3) heavy aluminum: the arbitrarily ratio of one or more added in above-mentioned leaching liquid in sodium, potassium, ammonium sulfate is 1:1 except aluminum, addition sulfate with the mol ratio of aluminum sulfate, is cooled to less than-5 DEG C, and solid-liquor separation obtains low aluminium sulfate solution；
4) purify: regulate above-mentioned low aluminium sulfate solution PH=8-12 and remove the impurity such as calcium, magnesium, ferrum, it is thus achieved that pure lithium sulfate scavenging solution；
5) sinker is concentrated: the lithium oxide content in sulfate liquor is concentrated into 50g/L, add the described ammonium fluoride solution obtained in step S71 and carry out sinker, the reaction temperature of described sinker reaction is 60 DEG C, the response time of described sinker be 1 hour again by solid-liquor separation, obtain mother solution and lithium fluoride crude product, described mother solution is added in the sulfate liquor described in step S73 and carry out heavy reactive aluminum, described lithium fluoride crude product is washed, dries, obtain lithium fluoride product.
Embodiment
7
The present embodiment provides a kind of lepidolite to prepare the technique of lithium fluoride, and described lepidolite is prepared the technique of lithium fluoride and comprised the following steps:
1) lepidolite acidifying: lepidolite and 70% sulphuric acid are added in reactor according to the mass ratio of 1:1.5, obtain grog, the gas water that described lepidolite acidification reaction produces absorbs and ammonification, obtain ammonium fluoride solution, wherein, the reaction temperature of described acidifying is 300 DEG C, and the response time of acidifying is 1.5 hours；
2) grog water logging: after being stirred 1 hour according to liquid-solid ratio 3:1 water extraction by grog good for lepidolite acidification reaction, solid-liquor separation obtains leaching liquid；
3) heavy aluminum: the arbitrarily ratio of one or more added in above-mentioned leaching liquid in sodium, potassium, ammonium sulfate is 1:1 except aluminum, addition sulfate with the mol ratio of aluminum sulfate, is cooled to less than-5 DEG C, and solid-liquor separation obtains low aluminium sulfate solution；
4) purify: regulate above-mentioned low aluminium sulfate solution PH=8-12 and remove the impurity such as calcium, magnesium, ferrum, it is thus achieved that pure lithium sulfate scavenging solution；
5) sinker is concentrated: the lithium oxide content in sulfate liquor is concentrated into 60g/L, add the described ammonium fluoride solution obtained in step S81 and carry out sinker, the reaction temperature of described sinker reaction is 70 DEG C, the response time of described sinker be 2 hours again by solid-liquor separation, obtain mother solution and lithium fluoride crude product, described mother solution is added in the sulfate liquor described in step S83 and carry out heavy reactive aluminum, described lithium fluoride crude product is washed, dries, obtain lithium fluoride product.
Invention described above embodiment, is not intended that limiting the scope of the present invention.Any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
The above is only the detailed description of the invention of the present invention, makes to skilled artisans appreciate that or realize the present invention.Multiple amendment to these embodiments will be apparent to one skilled in the art, and generic principles defined herein can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is to fit to the widest scope consistent with principles disclosed herein and features of novelty.
Claims (10)
1. the technique that a lepidolite prepares lithium fluoride, it is characterised in that: described technique comprises the steps: lepidolite acidifying, grog water logging, heavy aluminum, purifies and concentrate sinker.
The technique that lepidolite the most according to claim 1 prepares lithium fluoride, it is characterised in that: described technique comprises the steps:
1): lepidolite is acidified: lepidolite is obtained grog with sulfuric acid reaction；
2): grog water logging: described grog is mixed with water leaching, leaching liquid is obtained after solid-liquor separation；
3): heavy aluminum: in described leaching liquid, add sodium, potassium, the sulfate of ammonium, be cooled to less than-5 DEG C, by solid-liquor separation, obtain low aluminium sulfate solution；
4): purify: regulate the PH=8-12 of above-mentioned low aluminium sulfate solution, the impurity such as calcium, magnesium, ferrum are removed, it is thus achieved that pure lithium sulfate scavenging solution；
5): concentrate sinker: the lithium oxide content in step 4) sulfate liquor is concentrated into 35-60g/L, add ammonium fluoride solution and carry out sinker, then by solid-liquor separation, obtain mother solution and lithium fluoride crude product, described lithium fluoride crude product is washed, dries, obtain lithium fluoride product.
The technique that lepidolite the most according to claim 2 prepares lithium fluoride, it is characterised in that in described step 1), the reaction temperature of acidifying is 200-300 DEG C, and the response time is 0.5-8 hour.
The technique that lepidolite the most according to claim 2 prepares lithium fluoride, it is characterised in that in described step 1), lepidolite is more than or equal to 50% with sulphuric acid according to mass ratio 1:0.6-1.5, the mass concentration of sulphuric acid.
The technique that lepidolite the most according to claim 2 prepares lithium fluoride, it is characterised in that described step 2) described in the liquid-solid ratio of grog and water be 1～4:1, leaching time is 0.5 3 hours.
The technique that lepidolite the most according to claim 2 prepares lithium fluoride, it is characterized in that, in described step 3), sulfate is one or more arbitrarily ratio mixing of sodium sulfate, potassium sulfate, ammonium sulfate, and the sulfate of addition is 1:1 with the mol ratio of aluminum sulfate in leaching liquid.
The technique that lepidolite the most according to claim 2 prepares lithium fluoride, it is characterised in that the reaction temperature adding ammonium fluoride solution sinker in described step 5) is 30-80 DEG C, and the response time is 0.1-3 hour.
The technique that lepidolite the most according to claim 2 prepares lithium fluoride, it is characterised in that: the gas water that described step 1) acidification reaction produces absorbs and obtains hexafluosilicic acid, then ammonification, obtains ammonium fluoride solution.
The technique that lepidolite the most according to claim 8 prepares lithium fluoride, it is characterised in that: described ammonium fluoride solution is in the concentration sinker of step 5).
The technique that lepidolite the most according to claim 2 prepares lithium fluoride, it is characterised in that: the mother solution in described step 5) adds in step 3).
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| CN113929118A (en) * | 2021-11-19 | 2022-01-14 | 山东泰普锂业科技有限公司 | Process for preparing lithium fluoride from lepidolite |
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Application publication date: 20161116 |