WO2012083677A1 - Monohydrate d'hydroxyde de lithium exempt de poussière, et son procédé de préparation - Google Patents

Monohydrate d'hydroxyde de lithium exempt de poussière, et son procédé de préparation Download PDF

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Publication number
WO2012083677A1
WO2012083677A1 PCT/CN2011/076973 CN2011076973W WO2012083677A1 WO 2012083677 A1 WO2012083677 A1 WO 2012083677A1 CN 2011076973 W CN2011076973 W CN 2011076973W WO 2012083677 A1 WO2012083677 A1 WO 2012083677A1
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WIPO (PCT)
Prior art keywords
sodium
lithium hydroxide
hydroxide monohydrate
lioh
caking agent
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PCT/CN2011/076973
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English (en)
Chinese (zh)
Inventor
姚开林
金鹏
霍立明
何东利
何开茂
彭宗惠
涂明江
杨柳
江虎成
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雅安华汇锂业科技材料有限公司
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Priority to CA2822196A priority Critical patent/CA2822196C/fr
Publication of WO2012083677A1 publication Critical patent/WO2012083677A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/02—Oxides; Hydroxides

Definitions

  • the present invention relates to a dust-free grade lithium hydroxide monohydrate and a preparation method thereof, and belongs to the technical field of lithium hydroxide preparation. Background technique
  • Lithium hydroxide monohydrate ( ⁇ 2 0) is widely used in the manufacture of high-grade lithium-based greases. It is currently the largest consumer of ⁇ 2 0. Li-based greases produced by LiOH 0 are suitable for a wide temperature range (- 50 ° C ⁇ +300 ° C;), good fire performance, difficult to oxidize, multiple heating _ cooling _ heating cycle stability, long service life, strong water resistance.
  • ⁇ 20 is also widely used in the fields of chemical industry, national defense, and battery. Alkaline battery additives in the battery industry can extend their life and increase their storage capacity. It can absorb radioisotopes as an ion exchange resin in national defense and can be used as a heat carrier for nuclear reactors and as a protective agent for metal surfaces.
  • ⁇ 20 can be used for air purification in submarines, breathing masks for pilots.
  • ⁇ 2 0 can also be used as a water purifying agent, an emulsifier for the production of porous concrete, a special optical glass raw material, and a raw material for synthesizing vitamin A and many other lithium salt products.
  • the preparation methods of LiOH H 2 0 mainly include:
  • the lithium-containing ore and limestone are mixed and ground in a certain mass ratio.
  • the ground slurry is then sent to a rotary kiln for calcination, and the CaO produced by the decomposition of calcium carbonate reacts with the lithium ore to form LiOH.
  • the shortcomings of high energy consumption, high material flow, high cost and difficult product quality it is rarely used.
  • the ⁇ -spodumene concentrate is calcined in a rotary kiln at 1050 ° C to 1100 ° C to be converted into ⁇ -spodumene, and a certain amount of Na 2 C0 3 is added and uniformly mixed, and the temperature is leached at 200 ° C.
  • the soluble LiHC0 3 is formed by passing through C0 2 , and the residue is removed by filtration, and then the refined lime milk is added in a stoichiometric ratio, and the reaction liquid is concentrated and crystallized to obtain ⁇ 20 .
  • the brine is concentrated to a Li content of 5% to 7% (35% to 44% in terms of LiCl), and after filtration, the pH is adjusted to 10.5 to 1.5, and the calcium and magnesium ions in the brine are removed by precipitation to obtain a purified brine (the main component is LiCl), then the refined brine is electrolyzed in a special electrolytic cell as an electrolyte, the anolyte is refined brine, the catholyte is water or LiOH solution; there is a cation selective permeation between the anolyte and the catholyte Membrane (e.g., perfluorosulfonic acid membrane Rf-S0 3 H, perfluorocarboxylic acid membrane Rf-COOH, etc.), the cation can pass, and the anion is blocked from passing.
  • a cation selective permeation between the anolyte and the catholyte Membrane (e.g., perfluorosulfonic acid membrane R
  • Li + can migrate through the membrane to the cathode and convert to LiOH.
  • the H 2 and Cl 2 produced by the reaction can be used as a by-product to manufacture HC1.
  • a LiOH solution having a concentration of about 14% can be obtained at the cathode, and the crystal is dried to obtain a LiOH product.
  • this method has high energy consumption, high cost, and great environmental impact.
  • a fluorine-containing cation exchange resin for example, C 2 H 4 and CF 2
  • LiOH is prepared by ion-exchange membrane electrolysis, which not only has high Li recovery rate (nearly 100%), no secondary pollution, but also has high purity (>99%), which can be directly used to produce lithium lubricant.
  • the method requires very high content of impurity ions in the refined brine: the total concentration of Na + and K + is below 5%, and the total amount of Ca 2+ and Mg 2+ is not more than 0.004%.
  • the ion film is expensive and difficult to maintain, and the production cost of preparing LiOH is relatively increased.
  • the method produces lithium hydroxide by using 10% sodium aluminate as a raw material, and carbonizing and decomposing 40% of C0 2 to obtain Al(OH) 3 , and adding aluminum to lithium by weight ratio of 13 ⁇ 15 to boron.
  • brine containing 0.13% Li
  • pH 6.8 ⁇ 7.0 is controlled, temperature is 90 °C
  • Al(OH) 3 can form stable aluminum lithium compound with Li + in brine (LiCl'2Al(OH nH 2 0) Precipitation, lithium precipitation rate of 95%.
  • the obtained aluminum lithium precipitate is calcined in the presence of a neutral salt (such as NaN0 3 , NaCl, etc.) at 120 ° C ⁇ 130 ° C for 20 min ⁇ 30 min, which is decomposed into ⁇ 1 ( ⁇ ) 3 and soluble lithium salt, hot water Leaching to separate the aluminum lithium in the precipitate.
  • a neutral salt such as NaN0 3 , NaCl, etc.
  • the leachate is passed through an exchange column containing a strongly acidic cation exchange resin, and the cations such as Li + and Mg 2+ in the solution are replaced in an exchange column, and then eluted with 1% to 20% caustic solution.
  • the impurity ions such as Mg 2+ and Ca 2+ are precipitated in the exchange column, and Li + forms LiOH to flow out with the solution; or the leachate is passed through an exchange column containing a strong basic anion exchange resin in the solution.
  • the LiCl is converted to LiOH and flows out with the solution, and impurity ions such as Mg 2+ and Ca 2+ are precipitated and left in the exchange column to be separated.
  • the concentration of LiOH solution obtained by the method is about 6%, and the recovery rate of lithium is above 90%.
  • the obtained LiOH solution was concentrated by evaporation and dried by crystallization to obtain a LiOH product.
  • the soda ash and aluminum hydroxide recovered from the carbonized liquid are calcined at 900 ° C, and the sodium aluminate obtained after leaching can be recycled.
  • the disadvantage of this method for industrial scale production is that the obtained aluminum lithium precipitate is a colloid, the solid weight is only about 10%, the average particle is only ⁇ , it is difficult to filter and the process is complicated, and the energy consumption is high.
  • the brine is made of boron, evaporated to 50% of water, calcined at 700 ° C for 2 h, the magnesium chloride in the brine is pyrolyzed to magnesium oxide, the decomposition rate is 93%, and then leached with water, the leachate (containing 0.14% of lithium) milk of lime and soda ash removing calcium and magnesium ions, Na 3 P0 4 were added precipitated Li 3 P0 4. Filtration, the Li 3 P0 4 precipitate is mixed with CaO and A1 2 3 3 in a ratio of 1:6: 2, and calcined in an electric resistance furnace at 2300 ° C for 2 h, and then the calcined mixture is used at 85 ° C to 95 ° C.
  • the hot water is leached, filtered, and the filtrate is concentrated by evaporation, crystallized, and dried to obtain a LiOH product.
  • the method has the advantages that the resources such as lithium magnesium can be comprehensively utilized, and the chemical raw materials are required to be small; the calcination can remove impurities such as boron and magnesium, and improve the purity of lithium hydroxide.
  • the disadvantages are: The use of magnesium makes the process complex, the equipment is seriously corroded, the amount of evaporated water is large, and the energy consumption is high.
  • Patent No. ZL 200710051016.5 provides a method for preparing battery-grade lithium hydroxide monohydrate.
  • the method comprises the following steps: evaporating and concentrating the lithium sulphate leaching solution, adding NaOH, filtering and removing impurities such as Fe, Ca, Mn, and then freezing to - After 5 ⁇ 3 °C, Na 2 S (V 10H 2 O was separated by filtration, and then the filtrate was concentrated by evaporation to crystallize the crude ⁇ 2 0, and the crude ⁇ 2 0 was redissolved and transferred to the crude ⁇ 2 Adding the refined preparation to the 0 heavy solution, in addition to Na, cooling and crystallizing and separating, the solid is wet ⁇ 2 0, and then dried to obtain ⁇ 2 0 product.
  • the lithium silicate conversion method is to co-melt the obtained lithium carbonate with silicic acid to form lithium silicate, and the lithium silicate is hydrolyzed to produce lithium hydroxide; the lithium sulfate conversion method first converts lithium in the salt lake brine into lithium sulfate. Reuse lithium sulphate and barium hydroxide The reaction produces lithium hydroxide.
  • the lithium silicate method and the lithium sulphate method for preparing lithium hydroxide are still immature and are under study.
  • the ⁇ 20 prepared by the above method has a problem of flying nose dust flying in use, and as the environmental awareness of people increases, higher requirements are placed on the working environment, and the problem of dust flying is imminent.
  • the undried wet ⁇ ⁇ 20 can solve the problem of dust flying
  • the wet ⁇ 20 has a knot.
  • the knot will appear, and it needs to be tapped into small pieces and then used for feeding. If it is not used for 3-4 days, it will become a plate with a high hardness and it is difficult to use. If it is more than 4 days, it is difficult to knock with a hammer and it cannot be used. Therefore, the procurement and production requirements are high, which seriously affects the use. Therefore, solving the problem of the knot of the wet ⁇ ⁇ 20 and the problem of the dust flying of the ⁇ ⁇ 20 has raised new issues in the field.
  • the technical problem to be solved by the present invention is that there is a problem of compaction of the existing wet ⁇ ⁇ 20, and there is a problem of dust flying in the dry ⁇ ⁇ 20 , and a new ⁇ 2 0 is provided, that is, a dust-free, non-boarding list.
  • Lithium hydroxide in water Lithium hydroxide in water.
  • the technical solution of the present invention is:
  • the lithium hydroxide monohydrate of the present invention is a loose granular wet product. Can be stored for 3-5 months without squashing, still retain loose particles.
  • the lithium hydroxide monohydrate is a loose granular wet product, wherein the moisture content is 3.5%, and the surface of the lithium hydroxide monohydrate is coated with a trace amount of an anti-caking agent, and the anti-caking agent is sodium dodecyl sulfate.
  • the anti-caking agent is sodium dodecyl sulfate.
  • the dust-free lithium hydroxide monohydrate of the present invention is prepared by the following method:
  • step (2) Evaporate the LiOH solution obtained in step (1) until the liquid-solid ratio is 1:0.8 ⁇ 1.5, add a small amount of anti-caking agent, stir evenly, separate and wash to obtain dust-free industrial grade ⁇ 2 0 product, vacuum
  • the sealed package is not tied for several months.
  • the temperature at which the anti-caking agent is added is preferably 90-100 ° C, and when the temperature is lowered to 90 ° C or lower, the S0 4 2 - content of the obtained wet product is extremely high.
  • step (1) controls S0 4 2 agricultural degree 8 g/l, and controls Na 2 0 concentration 2 g/l, CaO concentration 0.01 g/l; (2) When the anti-caking agent is added, the LiOH solution is evaporated to a liquid-to-solid ratio of 1:0.8 to 1.1.
  • the effect of controlling the liquid-solid ratio of evaporation is mainly used as a control means for the end point of evaporation.
  • the liquid-solid ratio is too high, and the evaporation end point is too advanced, which affects the yield and crystallization effect, and the crystal form is poor. If the liquid-solid ratio is too low, the evaporation end point will be too high, and the concentration of the liquid will be too high, which will make the impurities in the product higher.
  • Industrial products have higher levels of impurities than battery-grade products, so the concentration of liquid at the end of the evaporation can be higher than the concentration of the liquid at the end of the production of the battery-grade product, that is, the liquid-solid concentration of the liquid at the end of the production of industrial grade products.
  • the ratio may be less than the liquid to solid ratio of the battery level production evaporation end point liquid.
  • the anti-caking agent of the present invention may be: a sodium salt or a potassium salt such as sodium lauryl sulfate, sodium ferrocyanide, potassium ferrocyanide, sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, Or methylpentanol, triethylhexylphosphoric acid, cellulose derivatives, and the like.
  • a sodium salt or a potassium salt such as sodium lauryl sulfate, sodium ferrocyanide, potassium ferrocyanide, sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, Or methylpentanol, triethylhexylphosphoric acid, cellulose derivatives, and the like.
  • an insoluble anti-caking agent such as sodium aluminosilicate, tricalcium phosphate, amorphous silica or the like.
  • the insoluble anti-caking agent has a very small solubility, and the mixing effect in the slurry is poor, and its use amount is relatively large, which leads to an excessively high impurity of the product, so that the insoluble anti-caking agent is preferably not used.
  • the production environment of lithium hydroxide monohydrate is an inorganic salt system. According to the principle of similar compatibility of chemical substances, it is preferable not to use organic substances in the selection of anti-caking agents.
  • the LiOH solution in the step (1) can be prepared by using the prior art, or the crude ⁇ 2 0 is dissolved in water to purify and remove impurities to obtain a LiOH solution.
  • Lithium ore and limestone calcined to form LiOH which is obtained by impurity removal; ⁇ -spodumene is mixed with Na 2 C0 3 Evenly, the temperature is leached at 200 ° C, the soluble LiHC0 3 is formed by adding C0 2 , the refined lime milk is added according to the stoichiometric ratio, and the residue is obtained after the reaction; the lime milk and the lithium carbonate are causticized to obtain a LiOH solution; The brine is obtained by LiOH solution; the Li 2 SO 4 solution is electrolyzed to obtain LiOH solution; the sodium aluminate is decomposed by C0 2 carbonization to obtain Al(OH) 3 , which reacts with the brine to form a stable aluminum lithium compound (LiCl'2Al(OH) 3 'nH 2 0) Precipitation, calcination in the presence of a neutral salt (such as NaN0 3 , NaCl, etc.), which is decomposed into ⁇ 1(
  • the key point of the present invention is that a small amount of an additive and an anti-caking agent which do not affect the quality of the ⁇ 20 product are added during the precipitation of LiOH, and the precipitation process is regulated, so that the precipitated wet product ⁇ 20 is not plated during storage. Avoid the problem of dust flying after drying.
  • deionized water is used as much as possible during the formulation and rinsing process.
  • the invention has the advantages of simple production process, easy operation, less equipment investment, low product cost, high lithium recovery rate, stable product quality, and no flaws in the product, and the dust-free grade ⁇ 2 0 product completely produced. It can meet the quality needs and environmental requirements of the downstream industry.
  • the filtrate was a purified LiOH solution; the Li 2 0 concentration of 72 g/l LiOH solution, S0 4 2 agricultural degree 8g / l, and control Na 2 0 concentration 2g / l, CaO concentration of 0.01g / l.
  • the preparation process was the same as in Example 1, except that the amount of the anti-caking agent used and the type of the anti-caking agent were different. The specific results are shown in Table 1.
  • the crude product adding deionized water, stirring to completely dissolve it, and making the concentration of Li 2 0 in the solution 70g/L, separating and filtering, the filtrate is LiOH pure liquid; wherein the concentration of Li 2 0 is 70 g / l LiOH solution, S0 4 2 agricultural degree 12g / l, and control Na 2 0 concentration 5g / l, CaO concentration 0.06g / l.
  • the LiOH solution obtained in the step (1) is evaporated to a liquid-solid ratio of 1:1.2, the anti-caking agent is added, the mixture is evenly stirred, and the temperature of the material is maintained at 90°, and the solid obtained by separation and washing is industrial-grade dust-free ⁇ 2 0 .
  • Table 2 The condition of the tube after vacuum packaging is shown in Table 2.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

L'invention concerne un monohydrate d'hydroxyde de lithium exempt de poussière et son procédé de préparation, qui relèvent du domaine technique de la préparation de l'hydroxyde de lithium. Le problème technique à résoudre consiste à obtenir un monohydrate d'hydroxyde de lithium (LiOH•H2O) exempt de poussière, non durcissable, qui apporte une solution au problème de durcissement du LiOH•H2O humide et de poussiérage du LiOH•H2O sec de l'art antérieur. Le monohydrate d'hydroxyde de lithium est un produit granulaire en vrac humide, dont la teneur en humidité est inférieure ou égale à 3,5%, et dont la surface est enrobée d'une petite quantité d'un agent de durcissement. La méthode de préparation du monohydrate d'hydroxyde de lithium exempt de poussière consiste à: 1) préparer une solution de LiOH à 70 ± 5 g/L selon une concentration du Li2O de 70±5 g/L, la concentration de SO4 2- étant régulée pour être inférieure ou égale à 15 g/L; 2) évaporer la solution de LiOH obtenue à l'étape (1) selon un rapport liquide-solide de 1:0,8 à 1,5 puis ajouter une petite quantité de l'agent anti-durcissement, agiter de manière homogène, séparer et laver pour obtenir le LiOH•H2O humide exempt de poussière, non durcissable en 3 à 5 mois dans un boîtier scellé sous vide.
PCT/CN2011/076973 2010-12-23 2011-07-08 Monohydrate d'hydroxyde de lithium exempt de poussière, et son procédé de préparation WO2012083677A1 (fr)

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CN2010106028943A CN102020294B (zh) 2010-12-23 2010-12-23 无尘级单水氢氧化锂及其制备方法

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CN112272654A (zh) * 2018-05-18 2021-01-26 奥图泰(芬兰)公司 用于回收氢氧化锂的方法
CN114276214A (zh) * 2021-12-10 2022-04-05 湖北宜化化工股份有限公司宜都分公司 一种回收利用电石渣生产季戊四醇的生产方法
CN115215357A (zh) * 2022-07-22 2022-10-21 江苏容汇通用锂业股份有限公司 一种由粗品硫酸锂制备电池级单水氢氧化锂的方法
CN115432721A (zh) * 2022-07-08 2022-12-06 江苏容汇通用锂业股份有限公司 一种制备氢氧化锂的工艺

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CN102020294B (zh) * 2010-12-23 2012-04-25 雅安华汇锂业科技材料有限公司 无尘级单水氢氧化锂及其制备方法
RU2512310C2 (ru) * 2012-08-06 2014-04-10 Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом"-Госкорпорация "Росатом" Способ получения раствора ферроцианида лития
CN102786069B (zh) * 2012-09-07 2014-02-12 雅安华汇锂业科技材料有限公司 无尘级单水氢氧化锂的制备方法
CN102838140B (zh) * 2012-09-14 2014-03-12 四川国润新材料有限公司 用锂辉石直接生产环保型LiOH.H2O的方法
CN104163442B (zh) * 2014-08-06 2016-03-23 四川天齐锂业股份有限公司 无尘级单水氢氧化锂及制备方法
KR101839460B1 (ko) 2017-10-24 2018-03-16 성일하이텍㈜ 리튬 함유 용액으로부터 고순도의 탄산리튬 회수방법
CN111889300A (zh) * 2020-06-16 2020-11-06 四川兴晟锂业有限责任公司 一种防沉积块化的单水氢氧化锂晶体及其制备方法
CN112279279B (zh) * 2020-10-26 2023-05-12 荆门市格林美新材料有限公司 一种电池级单水氢氧化锂的制备方法
CN112216834B (zh) * 2020-10-29 2021-08-03 湖南永杉锂业有限公司 一种喷雾包覆制备改性无水氢氧化锂的方法
CN113896214B (zh) * 2021-11-29 2023-03-21 福州大学 一种硫酸锂溶液吸附碳化制备高纯碳酸锂的方法

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CN101214978A (zh) * 2007-12-28 2008-07-09 四川天齐锂业股份有限公司 电池级单水氢氧化锂的制备方法
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112272654A (zh) * 2018-05-18 2021-01-26 奥图泰(芬兰)公司 用于回收氢氧化锂的方法
CN112272654B (zh) * 2018-05-18 2024-03-15 美卓奥图泰芬兰有限公司 用于回收氢氧化锂的方法
CN114276214A (zh) * 2021-12-10 2022-04-05 湖北宜化化工股份有限公司宜都分公司 一种回收利用电石渣生产季戊四醇的生产方法
CN115432721A (zh) * 2022-07-08 2022-12-06 江苏容汇通用锂业股份有限公司 一种制备氢氧化锂的工艺
CN115215357A (zh) * 2022-07-22 2022-10-21 江苏容汇通用锂业股份有限公司 一种由粗品硫酸锂制备电池级单水氢氧化锂的方法
CN115215357B (zh) * 2022-07-22 2023-11-24 江苏容汇通用锂业股份有限公司 一种由粗品硫酸锂制备电池级单水氢氧化锂的方法

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CA2822196C (fr) 2016-10-18
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