CN102030344A - Preparation method of lithium fluoride - Google Patents
Preparation method of lithium fluoride Download PDFInfo
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- CN102030344A CN102030344A CN2009101964376A CN200910196437A CN102030344A CN 102030344 A CN102030344 A CN 102030344A CN 2009101964376 A CN2009101964376 A CN 2009101964376A CN 200910196437 A CN200910196437 A CN 200910196437A CN 102030344 A CN102030344 A CN 102030344A
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- quilonum retard
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Abstract
The invention provides a preparation method of lithium fluoride, which comprises the following steps: (1) introducing carbon dioxide into water, then adding the raw material lithium carbonate to obtain a lithium bicarbonate solution, then adding a precipitant, introducing carbon dioxide until the pH of the solution is 8-9, filtering, and collecting the lithium bicarbonate solution; and (2) adding hydrofluoric acid to the filtrate obtained in the step (1), carrying out fluoridation, then adding a lithium hydroxide solution, regulating the pH of the system to be 7-7.5, then filtering, collecting the filter cake, and drying to obtain the product lithium fluoride. In the invention, the industrial grade lithium carbonate is used, the total yield of the technical process achieves more than 97%, the purity is as high as 99.9% or above, and the impurity content in the product is as low as 80PPm or below.
Description
Technical field
The present invention relates to the preparation technology of lithium fluoride.
Background technology
Lithium fluoride can be used for enamel, glass, china and pottery industry is made fusing assistant, also braze-welding flux and fused salt chemistry in make fusing assistant, in addition, also in spaceship, store solar radiation heat energy as the heat sink raw material.In recent years along with the continuous development of lithium battery technology, lithium ion battery with its specific energy height, power density height, have extended cycle life, self-discharge is little, ratio of performance to price advantages of higher has become current portable type electronic product can fill the formula power supply again at main alternative.Meanwhile, for alleviating environmental stress, the hybrid-electric car (HEV) of battery and mechanical power and usefulness is competitively developed in countries in the world, and according to the market forecast of day USA and Europe, Vehicular battery will be based on lithium ion battery after 2010.Can lithium ion battery realize that commercialization will depend primarily on performance and price.
Lithium ion battery be meant that use can suck or the carbon materials of desorb lithium ion as negative electrode active material; Use can suck or desorb lithium ion and the metal oxide that contains lithium ion as positive active material, based on the rechargeable cell of the above use organic solution of carrying out the principle of chemical reaction and making as electrolytic solution.During battery charging and discharging, positive and negative electrode suck repeatedly or desorb be lithium ion (Li+), so be referred to as lithium ion battery.It mainly is made up of positive pole, negative pole, barrier film, electrolytic solution etc.Wherein mainly contain cobalt acid lithium, cobalt acid nickel, lithium manganate, ferrous acid lithium, LiFePO 4 etc. as the positive electrode material positive active material.As the negative material negative electrode active material mainly is graphite, also has hard charcoal, soft charcoal etc.And electrolytic solution actual be liquid electrolyte, add monomer therein, can make after the polymerization solid electrolyte so-called polymer dielectric, thereby can produce the polymer Li-ion battery of so-called total solids, it is smaller and more exquisite, safe, easily process arbitrary shape, is referred to as s-generation lithium ion battery.Electrolytic solution is to be made in mixed organic solvents by dissolving electrolyte salt, electrolytic salt has inorganic salt and organic salt, inorganic salt have lithium perchlorate (only using), LiBF4, hexafluoroarsenate lithium and lithium hexafluoro phosphate in disposable lithium ion battery, organic salt has trifluoromethyl sulfonic acid lithium, two, trifluoromethane sulfonic acid Lithamide etc.Wherein LiBF4 and lithium hexafluoro phosphate are the most commonly used.And lithium fluoride is as the main raw material of producing LiBF4, along with its demand of continuous increase of lithium ion battery output also in continuous increase.
Lithium-ion secondary cell does not directly adopt metallic lithium or lithium alloy to make negative pole, but adopts the carbon material that can make the lithium ion embedding and take off embedding to make negative pole.For the ease of difference,, be also referred to as lithium-ion secondary cell so this battery is called lithium-ions battery.It has kept advantages such as high-energy-density that lithium cell has, long circulation life.So lithium-ion secondary cell is the focus that people study always.The application market of lithium-ion secondary cell constantly enlarges, and its application percentage in civilian small electric apparatus constantly increases, and can predict that the sales volume of this Battery Market will might be occupied an leading position above other batteries.
Along with the progress of microelectronics and the development of a large amount of mobile electronic equipments that come out, as mobile phone, pick up camera and the electromobile that occurs in recent years etc., all require high-energy, volume power supply little, dependable performance to do power, particularly (energy density is more and more urgent at the needs of 250~300Wh/L) battery, and this demand provides practical power for the development of serondary lithium battery at 100~150Wh/kg to energy.If last century, the late nineteen seventies serondary lithium battery only was breadboard product, after so short 20 years, be that the battery of negative pole has obtained developing rapidly with the metal.From being used for the Li/MnO of Computer Storage protection
2The commercialization of battery and to have the military and civilian potentiality to insert compound with carbon be negative pole is with LiCoO
2, LiNiO
2, LiMn
2O
4For the anodal lithium-ion secondary cell with to the development of specific conductivity near the solid electrolyte of liquid electrolyte, each sport technique segment of serondary lithium battery has all had considerable progress.To the beginning of this century, lithium ion battery and Ni/Cd, Ni/MeH battery form the situation of standing like the legs of a tripod.In recent ten years, countries in the world government all drops into great amount of manpower and material resources, joins in this field technology competition.In addition, lithium fluoride is a main raw material of producing LiBF4.
Usually, lithium fluoride prepares with the following method: hydrofluoric acid is joined direct reaction obtains lithium fluoride in the suspension liquid of Quilonum Retard and water.The major defect of this method is: the Quilonum Retard raw material is unprocessed, and its foreign matter content has directly determined the quality of product.Reaction not exclusively, owing to be solid-liquid reaction, and the product lithium fluoride of reaction output also is a solid, even guarantee higher acidity, in the Quilonum Retard surface coverage behind the lithium fluoride, therefore fluoridation just can not be carried out fully, and all wrapping to mix in the lithium fluoride product that obtains with this method has a certain amount of Quilonum Retard.Product granularity is thinner, and solid-liquid separation is incomplete, and the solubility magazine is brought into more, and the product clustering phenomena is comparatively serious when dry, thereby influences sieving technology.Need to regulate PH, increased product cost, introduce related impurities simultaneously with alkaline matters such as more ammoniacal liquor.
Summary of the invention
The object of the present invention is to provide a kind of lithium fluoride preparation method, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
(1) carbonic acid gas is fed in the water, add the raw material Quilonum Retard then, obtain lithia water, add precipitation agent again, make calcium (Ca), magnesium (Mg), sulfate radical (SO in the described solution
4 2-) wait impurity to form precipitation, the feeding carbonic acid gas is 8~9 to the pH of solution, lithia water is collected in filtration;
The weight content of raw material Quilonum Retard in water is 4.0~4.2%.
Described raw material Quilonum Retard is the technical grade Quilonum Retard, wherein, the weight content of Quilonum Retard is 99.0%, sodium (Na) for 500PPm or above, magnesium (Mg) for 100PPm or above, iron (Fe) content be 50PPm or more than, potassium (K), aluminium (Al), copper (Cu) be 20PPm or more than, calcium (Ca) be 200PPm or more than, sulfate radical (SO
4 2-) be 1000PPm or more than.
Technical grade lithium carbonate product national standard (GB/T 11075-2003)
The weight of precipitation agent is 0.1~0.5% of raw material Quilonum Retard weight;
Described precipitation agent is selected from more than one in oxalic acid, ammonium oxalate, hydrated barta, barium carbonate, oxalate or the barium salt;
(2) hydrofluoric acid is added the filtrate that step (1) obtains, 20~50 ℃ were reacted 20~40 minutes down, add weight concentration then and be 12~15% lithium hydroxide solution, the pH to 7 of regulation system~7.5, filter then, collect filter cake, dry, final drying temperature is 130~135 ℃, obtains the product lithium fluoride;
The consumption of hydrofluoric acid is: 0.05~0.057Kg/L lithia water;
Method of the present invention, used the comparatively raw material one technical grade Quilonum Retard on basis, the technological process total recovery reaches more than 97%, purity up to 99.9% or more than, impurity natrium in the product (Na), magnesium (Mg), iron (Fe) content are low to moderate 50PPm or following, potassium (K), aluminium (Al), copper (Cu) content are low to moderate 10PPm or following, and calcium (Ca) content is low to moderate 30PPm or following, sulfate radical (SO
4 2-) content is low to moderate 80PPm or following.Therefore advantage of the present invention is to produce high yield, high purity, the battery-grade lithium fluoride of lower cost.
Embodiment
The following example is only illustrating the present invention, and does not limit the scope of the invention.
Embodiment 1
The raw material Quilonum Retard is the technical grade Quilonum Retard, and wherein, the weight content of Quilonum Retard is 99.07%, sodium (Na) is that 775PPm, magnesium (Mg) are 52PPm for 112PPm, iron (Fe), potassium (K), aluminium (Al), copper (Cu) are 20PPm, and calcium (Ca) is 221PPm, sulfate radical (SO
4 2-) be 1466PPm.
(1) 1.8M
3In the stainless steel reaction tower, add pure water 1400L, open carbonic acid gas (pressure-controlling is at 0.15Mpa), add technical grade Quilonum Retard 60Kg, add 0.12Kg oxalic acid, add the 0.29Kg hydrated barta; Feed carbonic acid gas, to pH=8, Quilonum Retard dissolves fully, filters with polypropylene sheet frame pressure filter again, obtains lithia water.
(2) 5M
3In the polypropylene reactive tank, the lithia water 4000L that adds step (1), add hydrofluoric acid 242Kg then, pH value of solution=5,35 a ℃ maintenance was stirred 30 minutes, the adding weight concentration is 15% lithium hydroxide solution, regulator solution pH to 7 filters then, and isolated lithium fluoride is placed Vacuumdrier, final drying temperature is 135 ℃, and dryer inner pressure is-0.09Mpa.The lithium fluoride that oven dry is good is cooled under 35 ℃ with recirculated cooling water.Obtain the 115.8Kg product.Total recovery is 97.31%.
Adopt the method for national Specification to detect, lithium fluoride purity up to 99.9% or more than, impurity natrium in the product (Na), magnesium (Mg), iron (Fe) content are low to moderate 50PPm or following, potassium (K), aluminium (Al), copper (Cu) content are low to moderate 10PPm or following, calcium (Ca) content is low to moderate 30PPm or following, sulfate radical (SO
4 2-) content is low to moderate 80PPm or following.
Embodiment 2
The raw material Quilonum Retard is the technical grade Quilonum Retard, and wherein, the weight content of Quilonum Retard is 99.12%, sodium (Na) content is that 855PPm, magnesium (Mg) content are that 107PPm, iron (Fe) are 48PPm, potassium (K), aluminium (Al), copper (Cu) are 20PPm, and calcium (Ca) content is 285PPm, sulfate radical content (SO
4 2-) be 1521PPm.
(1) 1.8M
3In the stainless steel reaction tower, add pure water 1400L, open carbonic acid gas (pressure-controlling is at 0.2Mpa), add technical grade Quilonum Retard 60Kg, add 0.16Kg oxalic acid, add the 0.301Kg hydrated barta, feed carbonic acid gas, to pH=8, Quilonum Retard dissolves fully, filters with polypropylene sheet frame pressure filter again, obtains lithia water.
(2) 5M
3In the polypropylene reactive tank, add the lithia water 4000L of step (1), add hydrofluoric acid 242.3Kg then, pH value of solution=5,34.3 a ℃ maintenance was stirred 34 minutes, the adding weight concentration is 15% lithium hydroxide solution, and regulator solution pH to pH=7 filters then, with isolated lithium fluoride, place Vacuumdrier, final drying temperature is 134.6 ℃, and dryer inner pressure is-0.09Mpa.The lithium fluoride that oven dry is good is cooled under 35 ℃ with recirculated cooling water.Obtain the 116.05Kg product.Total recovery is 97.27%.
Adopt the method for national Specification to detect, lithium fluoride purity up to 99.9% or more than, impurity natrium in the product (Na), magnesium (Mg), iron (Fe) content are low to moderate 50PPm or following, potassium (K), aluminium (Al), copper (Cu) content are low to moderate 10PPm or following, calcium (Ca) content is low to moderate 30PPm or following, sulfate radical (SO
4 2-) content is low to moderate 80PPm or following.
Claims (7)
1. the lithium fluoride preparation method is characterized in that, comprises the steps:
(1) carbonic acid gas is fed in the water, add the raw material Quilonum Retard then, obtain lithia water, add precipitation agent again, the feeding carbonic acid gas is 8~9 to the pH of solution, and lithia water is collected in filtration;
Described raw material Quilonum Retard is the technical grade Quilonum Retard;
(2) hydrofluoric acid is added the filtrate that step (1) obtains, carry out fluoridation, add lithium hydroxide solution then, filter then the pH to 7 of regulation system~7.5, collects filter cake, and drying obtains the product lithium fluoride.
2. method according to claim 1 is characterized in that, in the step (1), the weight content of raw material Quilonum Retard in water is 4.0~4.2%.
3. method according to claim 1, it is characterized in that, in the described technical grade Quilonum Retard, described raw material Quilonum Retard is the technical grade Quilonum Retard, and wherein, the weight content of Quilonum Retard is for being 99.0%, sodium (Na) for 500PPm or above, magnesium (Mg) for 100PPm or above, iron (Fe) content be 50PPm or more than, potassium (K), aluminium (Al), copper (Cu) be 20PPm or more than, calcium (Ca) be 200PPm or more than, sulfate radical (SO
4 2-) be 1000PPm or more than.
4. method according to claim 1 is characterized in that described precipitation agent is selected from more than one in oxalic acid, ammonium oxalate, hydrated barta, barium carbonate, oxalate or the barium salt.
5. method according to claim 4 is characterized in that, the weight of precipitation agent is 0.1~0.5% of raw material Quilonum Retard weight.
6. method according to claim 1, it is characterized in that, in the step (2), hydrofluoric acid is added the filtrate that step (1) obtains, and 20~50 ℃ of reactions 20~40 minutes down add weight concentration and are 12~15% lithium hydroxide solution then, the pH to 7 of regulation system~7.5, filter then, collect filter cake, dry, final drying temperature is 130~135 ℃.
7. method according to claim 1 is characterized in that, the consumption of hydrofluoric acid is: 0.05~0.057Kg/L lithia water.
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Cited By (16)
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CN102807237A (en) * | 2011-06-01 | 2012-12-05 | 上海中锂实业有限公司 | Method for preparing anhydrous lithium nitrate |
CN102807236A (en) * | 2011-06-01 | 2012-12-05 | 上海中锂实业有限公司 | Method for preparing lithium nitrate |
CN102849759A (en) * | 2012-10-11 | 2013-01-02 | 江西本源新材料科技有限公司 | Method for extracting lithium fluoride |
CN103232482A (en) * | 2013-04-11 | 2013-08-07 | 多氟多化工股份有限公司 | Preparation method for lithium bis (oxalate) borate |
CN103236562A (en) * | 2013-04-11 | 2013-08-07 | 多氟多化工股份有限公司 | Preparation method for lithium tetrafluoroborate |
WO2013174938A1 (en) | 2012-05-25 | 2013-11-28 | Lanxess Deutschland Gmbh | Production of high-purity lithium fluoride |
CN104326482A (en) * | 2013-07-23 | 2015-02-04 | 上海中锂实业有限公司 | Lithium tetrafluoroborate preparation method |
CN106025253A (en) * | 2016-05-12 | 2016-10-12 | 天津普兰能源科技有限公司 | Method for preparing lithium titanate |
CN106315629A (en) * | 2016-08-30 | 2017-01-11 | 山东瑞福锂业有限公司 | Technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor |
CN107043115A (en) * | 2017-05-05 | 2017-08-15 | 江西东鹏新材料有限责任公司 | A kind of production technology of lithium fluoride |
CN107055576A (en) * | 2017-05-02 | 2017-08-18 | 乐山沃耐稀电子材料有限公司 | A kind of preparation method of high-purity lithium fluoride |
CN111559750A (en) * | 2020-03-27 | 2020-08-21 | 白银中天化工有限责任公司 | Efficient continuous electronic-grade lithium fluoride production process |
CN111606336A (en) * | 2020-05-19 | 2020-09-01 | 百杰瑞(荆门)新材料有限公司 | Preparation method of lithium fluoride |
WO2021003895A1 (en) * | 2019-07-06 | 2021-01-14 | 贵州理工学院 | Method and device for preparing high-purity lithium fluoride |
CN112357937A (en) * | 2020-11-12 | 2021-02-12 | 萍乡市拓源实业有限公司 | Method for preparing battery-grade lithium carbonate from lithium iron phosphate |
CN112408437A (en) * | 2020-11-19 | 2021-02-26 | 江西天新药业股份有限公司 | Method for recovering lithium salt |
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2009
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CN102807237A (en) * | 2011-06-01 | 2012-12-05 | 上海中锂实业有限公司 | Method for preparing anhydrous lithium nitrate |
CN104364198A (en) * | 2012-05-25 | 2015-02-18 | 朗盛德国有限责任公司 | Production of high-purity lithium fluoride |
US9923232B2 (en) | 2012-05-25 | 2018-03-20 | Lanxess Deutschland Gmbh | Production of high-purity lithium fluoride |
AU2013265257B2 (en) * | 2012-05-25 | 2017-02-02 | Lanxess Deutschland Gmbh | Production of high-purity lithium fluoride |
CN104364198B (en) * | 2012-05-25 | 2016-07-06 | 朗盛德国有限责任公司 | The preparation of high-purity lithium fluoride |
WO2013174938A1 (en) | 2012-05-25 | 2013-11-28 | Lanxess Deutschland Gmbh | Production of high-purity lithium fluoride |
CN102849759B (en) * | 2012-10-11 | 2014-07-23 | 江西本源新材料科技有限公司 | Method for extracting lithium fluoride |
CN102849759A (en) * | 2012-10-11 | 2013-01-02 | 江西本源新材料科技有限公司 | Method for extracting lithium fluoride |
CN103236562B (en) * | 2013-04-11 | 2015-03-25 | 多氟多化工股份有限公司 | Preparation method for lithium tetrafluoroborate |
CN103232482B (en) * | 2013-04-11 | 2016-01-13 | 多氟多化工股份有限公司 | A kind of preparation method of biethyl diacid lithium borate |
CN103236562A (en) * | 2013-04-11 | 2013-08-07 | 多氟多化工股份有限公司 | Preparation method for lithium tetrafluoroborate |
CN103232482A (en) * | 2013-04-11 | 2013-08-07 | 多氟多化工股份有限公司 | Preparation method for lithium bis (oxalate) borate |
CN104326482B (en) * | 2013-07-23 | 2016-05-18 | 上海中锂实业有限公司 | Prepare the method for LiBF4 |
CN104326482A (en) * | 2013-07-23 | 2015-02-04 | 上海中锂实业有限公司 | Lithium tetrafluoroborate preparation method |
CN106025253A (en) * | 2016-05-12 | 2016-10-12 | 天津普兰能源科技有限公司 | Method for preparing lithium titanate |
CN106315629B (en) * | 2016-08-30 | 2018-01-30 | 山东瑞福锂业有限公司 | A kind of technique for preparing pure Lithium Carbonate using battery-level lithium carbonate sinker disposing mother liquor |
CN106315629A (en) * | 2016-08-30 | 2017-01-11 | 山东瑞福锂业有限公司 | Technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor |
CN107055576B (en) * | 2017-05-02 | 2019-02-01 | 乐山沃耐稀电子材料有限公司 | A kind of preparation method of high-purity lithium fluoride |
CN107055576A (en) * | 2017-05-02 | 2017-08-18 | 乐山沃耐稀电子材料有限公司 | A kind of preparation method of high-purity lithium fluoride |
CN107043115A (en) * | 2017-05-05 | 2017-08-15 | 江西东鹏新材料有限责任公司 | A kind of production technology of lithium fluoride |
WO2021003895A1 (en) * | 2019-07-06 | 2021-01-14 | 贵州理工学院 | Method and device for preparing high-purity lithium fluoride |
CN111559750A (en) * | 2020-03-27 | 2020-08-21 | 白银中天化工有限责任公司 | Efficient continuous electronic-grade lithium fluoride production process |
CN111606336A (en) * | 2020-05-19 | 2020-09-01 | 百杰瑞(荆门)新材料有限公司 | Preparation method of lithium fluoride |
CN112357937A (en) * | 2020-11-12 | 2021-02-12 | 萍乡市拓源实业有限公司 | Method for preparing battery-grade lithium carbonate from lithium iron phosphate |
CN112408437A (en) * | 2020-11-19 | 2021-02-26 | 江西天新药业股份有限公司 | Method for recovering lithium salt |
CN112408437B (en) * | 2020-11-19 | 2023-03-28 | 江西天新药业股份有限公司 | Method for recovering lithium salt |
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Application publication date: 20110427 |