CN1312040C - Purification production technique for producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade - Google Patents
Purification production technique for producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade Download PDFInfo
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- CN1312040C CN1312040C CNB2005100338127A CN200510033812A CN1312040C CN 1312040 C CN1312040 C CN 1312040C CN B2005100338127 A CNB2005100338127 A CN B2005100338127A CN 200510033812 A CN200510033812 A CN 200510033812A CN 1312040 C CN1312040 C CN 1312040C
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Abstract
The present invention discloses a purification production technique for producing high pure and high clear lithium hydroxide from lithium hydroxide in an industrial grade, which belongs to the technical field of lithium hydroxide purification. The present invention comprises the following steps that: (1) the raw material of lithium hydroxide in an industrial grade is sufficiently dissolved under the condition of low temperature of 20 to 30 DEG C and is quickly filtered for obtaining silica removing liquor; (2) when the silica removing liquor is heated to 40 to 50 DEG C in a reactor, carbonating purification agents are added; the liquor is continuously heated to boiling for partially carbonating and coprecipitating reactions; then, the filtration is carried out for obtaining purifying liquor; (3) after the purifying liquor is heated and concentrated to 1/3 or crystallization, the liquid solid separation is carried out in time for obtaining lithium hydroxide crystal; (4) the obtained lithium hydroxide crystal is purified, braked and dewatered for obtaining high pure and high clear lithium hydroxide. The production technology of the present invention has the advantages of simple manufacture process, short process, less investment, convenient operation, high product yield, technology quality in advanced world standard, and no environmental pollution. The present invention is used for producing the high pure and high clear lithium hydroxide from the lithium hydroxide in an industrial grade.
Description
Technical field
The present invention relates to the purification techniques of lithium hydroxide, be meant the method for purification of a kind of producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade that is used to produce high-tech lithium product especially.
Background technology
The high pure and high clear lithium hydroxide is to produce one of most important basic raw material of high-tech lithium product, and its high-purity notion is: main content (LiOHH
2O) reach more than 99.9% and (contain molecular crystal water), or each element and compound foreign matter content be all below 30ppm, critical impurities element (as Si) reaches below the 15ppm; High definition notion (being transmissivity or clarity) reaches more than 95%, can reach 99.5% at most.Be mainly used in the produce single crystal chip at present (as the high pure and high clear lithium tetraborate single crystal, high pure and high clear three lithium tetraborate monocrystalline etc.), ultra-pure product is (as ultra-pure Quilonum Retard, purity is 59, promptly more than 99.999%), green novel energy source is (as the heavy body lithium cell, lithium power vehicle etc.) and each side such as nanometer novel material, at microelectronics, digital technology, photoelectron science and technology, novel computer, national defense construction, video transmission, aerospace, military science and technology, various fields such as satellite communication have extensively and important use, along with the modern high technology industry constantly develops to " ultrapure; ultra-fine; super smart; the super appearance; ultra micro " direction, to high-purity, the demand of high definition novel material is strong day by day, and its application prospect is very huge.
Developed country produces the high purity lithium salt material, the main Technologies such as " electrolytic reduction, zone melting, vacuum distilling, vacuum-sublimations " that adopts, though have certain effect, technical sophistication, technical process is long, equipment is various, cost an arm and a leg, the tight lotus of working body condition (as high temperature, high pressure, high-strength, be able to bear strong corrosion, high vacuum, high sealing etc.).So production cost high enterprise, contaminate environment, press for change.
China has abundant lithium resource storage, and is along with rapid development of national economy, very surprising to the demand of novel energy and novel material.But because history and system can not realize still that to the high pure and high clear lithium hydroxide industrialization produces before this, and main dependence on import.
Summary of the invention
The object of the present invention is to provide that a kind of technology is simple, flow process weak point, less investment, easy to operate, product yield is high, technical quality is reached advanced world standards, and the method for purification of a kind of producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade of environmentally safe is to adapt to pressing for of domestic and international Hi-tech Industry Development.
The object of the present invention is achieved like this: a kind of method of purification of producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade, comprise the steps: (1) with the industrial raw material lithium hydroxide under 20～30 ℃ low temperature fully dissolving and filter fast silica removal liquid; When (2) silica removal liquid being heated to 40～50 ℃ in reactor, add carbonating purification reagent, continue to be heated to boil and carry out the part carbonating, coprecipitation reaction, filter then scavenging solution; (3) scavenging solution heating is concentrated into 1/3 or after visible crystals separates out, in time carry out liquid-solid separate the lithium hydroxide crystallization; (4) crystallization of gained lithium hydroxide is purified, smokes dehydration and promptly get the high pure and high clear lithium hydroxide.
Dissolving is under agitation to carry out in the method for purification step (1) of above-mentioned producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade, and the time is 10～20 minutes, leaves standstill then after 5～10 minutes to filter fast behind the removing surface impurity.
Carbonating purification reagent described in the method for purification step (2) of above-mentioned producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade is made up of the bicarbonate of ammonia of 80%～86% weight part, the oxalic acid of 10.2%～16.9% weight part and the lithium bicarbonate of 1.5%～3% weight part, and add-on is 2%～7% of a liquid weight.Carbonating purification reagent is that each component is formed particulate or Powdered after simple processing, under the half-light condition, mixes and stir forming.
The ebuillition of heated time in the method for purification step (2) of above-mentioned producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade is 40 minutes～1 hour, filtered while hot in 10～20 minutes after stopping to heat.
The method of purification step (3) of above-mentioned producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade is at the screening agent that is heated to the back adding liquid weight 0.05%～0.25% that boils, and screening agent can adopt EDTA.
Liquid-solid filtering separation temperature in the method for purification step (3) of above-mentioned producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade is 40～60 ℃.
Purification described in the method for purification step (4) of above-mentioned producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade is to adopt 70～80 ℃ twice of warm pure water drip washing; Smoking dehydration conditions is: 100～108 ℃ of temperature, 3.5～4 hours time.
Essence of the present invention is under the guidance of scientific and technological theory innovation achievement, carries out the achievement of a series of technological innovations.Its theory innovation at first shows " high pure and high clear " notion itself.In the past both at home and abroad industry that the requirement of new high-tech product raw material is concentrated on " high-purity " is conceptive, assert as long as raw material reaches higher purity, promptly can produce the new high-tech product that needs.But a large amount of practical experiences show, emphasize high-purity notion merely, and general differing satisfies needs of production surely.The same with high-purity notion, high definition (transmissivity clarity) specification of quality that is absolutely necessary equally, in a sense, or even even more important requirement.Practice shows to have only to reach indexs high-purity, high definition two aspects simultaneously, could guarantee that photoelectric properties, physicochemical property and the machining property etc. of end product really satisfy the new and high technology needs.The inventor herein finds through studying for a long period of time and confirms, contained various elements and compound impurity in lithium hydroxide, every Effect on Performance degree to product, exist great difference, wherein having the greatest impact of elemental silicon (Si) and compound impurity thereof accounts for 70%～80% of whole influence.Further deep discovering, the content of elemental silicon and compound impurity, and between the sharpness and even overall performance of product, not only present a kind of correlationship, and present a kind of quite strict linear relationship.Use the coordinate graphical presentation, as represent the element silicon foreign matter content with X-axis, (is unit with ppm), represent articulation index with Y-axis, with per 1% degree is unit, and each ppm gets equidistance unit with per 1% sharpness, then on the coordinate chart, the relation of the two is rendered as its slope (Y/X) and is about 0.33 straight line.
Another innovation of the present invention, promptly under the above-mentioned theory viewpoint instructs, removal of impurities at removal of impurities purification, particularly element silicon and compound is purified, researching and developing out a cover be the novel process method of main contents and characteristic with " dissolution in low temperature; filter fast; the co-precipitation of part carbonating, recrystallization ", and special for this reason and the carbonating purification reagent of development.
In traditional chemical high pure theory, it is a brand-new even strange notion that acidifying is purified.It is generally acknowledged that so-called acidifying is during basic metal, alkaline-earth metal component are purified, to neutralize by acidifying, produce precipitation of salts, thereby help removal of impurities, but because efficient is not high, only as a kind of supplementary means of chemical purification.
We are by long-term deep exploration and research, obtain the important discovery of a series of new product chemical combination in acidifying purification field, open up and deepened the understanding of acidifying purification theory greatly, enriched the theoretical content and the degree of depth of acidifying purification, made new contribution developing high pure theory.Invent and taken the lead in proposing the theory and the implementing process method thereof of " partial acidification (comprising part carbonating part phosphorylation, part oxalic acidization etc.) purification ", develop the acidifying purification reagent product of seriation, and obtained important breakthrough and gratifying result in practice.
New achievement in research shows: acidifying purification theory never only is " neutralization, precipitation, removal of impurities " so simple process.On the contrary, under new theoretical direction, the work of adopting novel acidified purification reagent to carry out is a very complicated physical chemistry moving process and a microscopic system engineering with rich connotation.
Studies show that, in the acidifying purification process, physics, the chemokinesis process of following a few class complexity takes place to the major general: at first, the bicarbonate of ammonia in the reagent etc. are met thermolysis, not only are easy to and contain lithium ion etc. and form insoluble carbonate (as Li
2CO
3, CaCO
3, BaCO
3, PbCO
3) etc., simultaneously, because HCO
3 -Ion forms the poly-or poly effect of ring by hydrogen bond, not only is easy to chemical combination and generates many kinds of bicarbonate salts (MHCO
3Class), and its solubility is significantly descended, also can form some insoluble subcarbonates (as 2PbCO
3.Pb (OH)
2, CuCO
3Cu (OH)
2, (BiO)
2CO
3Deng), in above-mentioned chemical process,, produce so-called coprecipitation phenomena and postprecipitation phenomenon because the effect in the free field of force of ionic charge and absorption and the bag that combination reaction is brought rapidly stay effect.In addition, it should be noted that under the effect of acid ion a series of unique and complex chemical physics reaction process also can take place solvable silicon ion etc. in the solution, wherein silicon ion and lithium easily form lithium silicate, and can form the multiple polymers body, promptly form siliceous colloid; Silicon ion is easy to chlorine, the fluorine plasma forms multiple mixture, and form a series of baroque polyacid materials with other multiple acid ions, because molecular weight, proportion, solubleness, molecular structure, the noticeable change of aspects such as volume, purify for taking the removal of impurities of novel process method in the capital, the precondition of science is provided.
The present invention has carried out deep exploration and research to the physical chemistry moving process of above-mentioned a series of complexity, accurate definition to all kinds of reactions, genesis mechanism, the evolution rule, to the meaning of Purification and contribution degree with and each other a series of important theory problems such as relation carried out deep, the research of qualitative, quantitative, some precious new discoveries have been obtained, a large amount of firsthand data and data have been obtained, derive a collection of mathematical formula and theoretical model, and then some important theory achievement and scientific conclusions have been drawn, take the lead in proposing and enrichment and development the partial acidification theory of purifying, and obtained gratifying effect in practice, the more important thing is that (the comprising the partial acidification purification) theory that takes the lead in acidifying is purified raises the height of high-purity mainstream theory of chemistry and beam method.
For implementing the carbonating purification reagent of the special development of processing method of the present invention, mainly form by bicarbonate of ammonia, lithium bicarbonate, three kinds of materials of oxalic acid.Its prescription is subdivided into (weight %): bicarbonate of ammonia: 80～86%, and lithium bicarbonate: 1.5～3%, oxalic acid: 10.2～16.9%.The user can be in above-mentioned formulation data scope, according to the difference of the impurity segmentation situation of every batch of raw material, is suitably selected to increase and decrease.Above-mentioned each component raw material is after simple processing (is particulate or Powdered as fine ground screening), and under the half-light condition, mixing is also stirred fully, and each raw material thorough mixing is evenly formed.Should avoid high temperature, daylight, wet environment to finish drilling preserves.The carbonating purification reagent outward appearance that processes is white or pale powder or crystallite shape thing, has stronger ammonia flavor and slight sharp flavor.Proportion is about 1.86～2.04.Practice shows, what of this carbonating purification reagent usage quantity have more significantly influence to the removal of impurities refining effect.Too small as usage quantity, (as below 1.5%), then the acidifying coprecipitation reaction is abundant inadequately, and refining effect is undesirable, and the solution filtration difficulty; Influencing subsequent handling carries out.Otherwise, be usage quantity excessive (as more than 8%), then the lithium loss is bigger, reduces product yield.Therefore, carbonating purification reagent usage quantity (calculating with reagent and liquor capacity ratio) is with 2%～7%.Scope is advisable.The use temperature of carbonating purification reagent begins to be incorporated as during with 40～50 ℃ suitable.Cross low temperature and use, will delay chemical combination removal of impurities purification efficiency, use in the excessive temperature, take place easily not only then that boiling is prosperous to go out.Cause waste, and easily personnel are brought injury.Equipment and workshop should be furnished with air-bleed system during use, in time discharge ammonia and other peculiar smell.Answer close observation during operation, prevent that roof fall from overflowing, pollute and waste.
The high pure and high clear lithium hydroxide that adopts processing method of the present invention to produce, its technology quality index is reached advanced world standards comprehensively, and the part key index significantly is better than the currently available products of developed country.Because this technology all processes all carries out in normal pressure, middle low temperature, employing common stainless steel chemical industry equipment, make technology greatly simplify shortening, easy to operate simple and direct, product yield is higher, environmentally safe, its required equipment cost only is external about 1/10th, and production cost only is an external like product about 1/3rd.
Description of drawings
Below in conjunction with drawings and Examples the present invention is described in further detail, but does not constitute any limitation of the invention.
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Embodiment 1
Consult as shown in fig. 1, the method for purification of producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade of the present invention, raw material adopts Xinjiang Lithium Salt Factory to produce, 1 grade of quality standard of industry.Its main quality index is: LiOHH
2O master's content: 〉=56.5 (molecular crystal water end counts), each impurity content is as follows: CO
2: 0.5%, K
+: 0.15%, Na
+: 0.05%, CaO:0.035%, Fe
2+: 0.003%, Cl
-: 0.004%, SO
4 2-: 0.03%, hydrochloric acid insoluble substance: 0.01%, water-insoluble: 0.02%.Silicon in this raw material (Si) foreign matter content mainly represents that with hydrochloric acid insoluble substance and water-insoluble form the two adds up to 0.03%, i.e. 300ppm.About 170kg of lithium hydroxide in industrial grade feeds intake, add the about 650kg of conductivity water, introduce among the dissolving tank A, stir down for 20 ℃ in room temperature and made abundant dissolving in 20 minutes, leave standstill after 5 minutes and remove surface impurity, filter fast then, elimination accounts for gross weight 0.2% insoluble sediment, gets silica removal liquid 1, heating will be begun among the silica removal liquid 1 injecting reactor B, when temperature reaches 40 ℃, add 5% carbonating purification reagent, carry out part carbonating coprecipitation reaction.Emit ammonia and hydrogen in the reaction process, in time discharge and reclaim, continue to be heated to boil (about 100～105 ℃), keep boiling 40 minutes, all kinds of reactions are carried out fully with ventilation installation.Stop to heat filtered while hot in back 10 minutes, carry out liquid-solid separate scavenging solution 2, to evaporate among the scavenging solution 2 introducing reactor C, the EDTA that is heated to the back adding 0.05% of boiling is as screening agent, continue to boil to solution concentration to original volume about 1/3, or the visible crystallization of visual inspection is when beginning to separate out, stop heating, leave standstill cooling, carry out the liquid-solid body of filtering separation when liquid temperature drop to 40 ℃, filtrate is returned in the dissolving tank A and is recycled, the gained solid phase prod is with 70 ℃ warm pure water drip washing 2 times, centrifuge dehydration is sent in the vacuum drying oven then, and oven dry is 4 hours under 100 ℃ of temperature, obtains the High Purity Hydrogen Lithium Oxide 98min.
Embodiment 2
Adopt same materials with embodiment 1, about 170kg of the lithium hydroxide in industrial grade that feeds intake adds the about 650kg of conductivity water, introduce among the dissolving tank A, made abundant dissolving in 10 minutes 30 ℃ of following stirrings of room temperature, leave standstill and remove surface impurity after 10 minutes, filter fast then, elimination accounts for gross weight 0.1～0.2% insoluble sediment, get silica removal liquid 1, with beginning heating among the silica removal liquid 1 injecting reactor B, when temperature reaches 50 ℃, the carbonating purification reagent of adding 7% carries out part carbonating coprecipitation reaction.Emit ammonia and hydrogen in the reaction process, in time discharge and reclaim, continue to be heated to boil (about 100～105 ℃), keep boiling 1 hour, all kinds of reactions are carried out fully with ventilation installation.Stop to heat filtered while hot in back 20 minutes, carry out liquid-solid separate scavenging solution 2, to evaporate among the scavenging solution 2 introducing reactor C, the EDTA that is heated to the back adding 0.25% of boiling is as screening agent, continue to boil to solution concentration to original volume about 1/3, or the visible crystallization of visual inspection is when beginning to separate out, stop heating, leave standstill cooling, carry out the liquid-solid body of filtering separation when liquid temperature drop to 60 ℃, filtrate is returned in the poor A of dissolving and is recycled, the gained solid phase prod is with 80 ℃ warm pure water drip washing 2 times, centrifuge dehydration is sent in the vacuum drying oven then, and oven dry is 3.5 hours under 108 ℃ of temperature, obtains the High Purity Hydrogen Lithium Oxide 98min.
Embodiment 3
Adopt same materials with embodiment 1, about 170kg of the lithium hydroxide in industrial grade that feeds intake adds the about 650kg of conductivity water, introduce among the dissolving tank A, made abundant dissolving in 15 minutes 25 ℃ of following stirrings of room temperature, leave standstill and remove surface impurity after 8 minutes, filter fast then, elimination accounts for gross weight 0.1～0.2% insoluble sediment, get silica removal liquid 1, with beginning heating among the silica removal liquid 1 injecting reactor B, when temperature reaches 45 ℃, the carbonating purification reagent of adding 41% carries out part carbonating coprecipitation reaction.Emit ammonia and hydrogen in the reaction process, in time discharge and reclaim, continue to be heated to boil (about 100～105 ℃), keep boiling 50 minutes, all kinds of reactions are carried out fully with ventilation installation.Stop to heat filtered while hot in back 15 minutes, carry out liquid-solid separate earning liquid 2, to evaporate among the earning liquid 2 introducing reactor C, the EDTA that is heated to the back adding 0.15% of boiling is as screening agent, continue to boil to solution concentration to original volume about 1/3, or the visible crystallization of visual inspection is when beginning to separate out, stop heating, leave standstill cooling, carry out the liquid-solid body of filtering separation when liquid temperature drop to 50 ℃, filtrate is returned in the dissolving tank A and is recycled, the gained solid phase prod is with 75 ℃ warm pure water drip washing 2 times, centrifuge dehydration is sent in the vacuum drying oven then, and oven dry is 3.5 hours under 1055 ℃ of temperature, obtains the High Purity Hydrogen Lithium Oxide 98min.
The High Purity Hydrogen Lithium Oxide 98min produced of the foregoing description after testing, its quality and technical index is: main content: 99.9%, CO
2: 0.001%, K
+: 0.0003%, Na
+: 0.001%, Ca
2+: 0.0004%, Fe
2+: 0.0003%, C1
-: 0.0004%, SO
4 2-: 0.0003%, hydrochloric acid insoluble substance, water-insoluble (Si): 0.001%, optical clarity (transmissivity): 97%.Produce the about 166.8kg of high pure and high clear lithium hydroxide by every batch of method of the present invention, direct yield reaches 98.2%.
Claims (8)
1. the method for purification of a producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade, its feature comprise the steps: (1) with the industrial raw material lithium hydroxide under 20～30 ℃ low temperature fully dissolving and filter fast silica removal liquid; When (2) silica removal liquid being heated to 40～50 ℃ in reactor, add carbonating purification reagent, continue to be heated to boil and carry out the part carbonating, coprecipitation reaction, filter then scavenging solution; (3) scavenging solution heating is concentrated into 1/3 or after visible crystals separates out, in time carry out liquid-solid separate the lithium hydroxide crystallization; (4) crystallization of gained lithium hydroxide is purified, smokes dehydration and promptly get the high pure and high clear lithium hydroxide; Carbonating purification reagent described in the step (2) is made up of the bicarbonate of ammonia of 80%～86% weight part, the oxalic acid of 10.2%～16.9% weight part and the lithium bicarbonate of 1.5%～3% weight part, and add-on is calculated as 2%～7% with reagent and liquor capacity ratio.
2. method of purification according to claim 1 is characterized in that: dissolving is under agitation to carry out in the step (1), and the time is 10～20 minutes, leaves standstill then after 5～10 minutes to filter fast behind the removing surface impurity.
3. method of purification according to claim 3 is characterized in that: described carbonating purification reagent is that each component is formed particulate or Powdered after simple processing, under the half-light condition, mixes and stir forming.
4. method of purification according to claim 1 is characterized in that: the ebuillition of heated time in the step (2) is 40 minutes～1 hour, filtered while hot in 10～20 minutes after stopping to heat.
5. method of purification according to claim 1 is characterized in that: step (3) is at the screening agent that is heated to the back adding liquid weight 0.05%～0.25% that boils, and described screening agent is EDTA.
6. method of purification according to claim 1 is characterized in that: the liquid-solid filtering separation temperature in the step (3) is 40～60 ℃.
7. method of purification according to claim 1 is characterized in that: the purification described in the step (4) is to adopt 70～80 ℃ twice of warm pure water drip washing.
8. method of purification according to claim 1 is characterized in that: the dehydration conditions of smoking described in the step (4) is: 100～108 ℃ of temperature, 3.5～4 hours time.
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| CNB2005100338127A CN1312040C (en) | 2005-06-22 | 2005-06-22 | Purification production technique for producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade |
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| CNB2005100338127A CN1312040C (en) | 2005-06-22 | 2005-06-22 | Purification production technique for producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade |
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| CN1312040C true CN1312040C (en) | 2007-04-25 |
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| FI121785B (en) * | 2009-03-11 | 2011-04-15 | Outotec Oyj | Process for the purification of lithium bicarbonate |
| CN102491377B (en) * | 2011-12-14 | 2015-08-05 | 江南大学 | A kind of method of lithium hydroxide purifying |
| JP2015000826A (en) * | 2013-06-14 | 2015-01-05 | 出光興産株式会社 | Method of producing dehydrated inorganic metal salt |
| CN103449480B (en) * | 2013-08-30 | 2016-03-16 | 新疆有色金属研究所 | Battery-grade high-purity lithium fluoride and preparation method thereof |
| CN105859542B (en) * | 2016-06-15 | 2019-02-05 | 湖北百杰瑞新材料股份有限公司 | A kind of preparation method of high-purity oxalic acid lithium |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2090503C1 (en) * | 1994-09-06 | 1997-09-20 | Научно-производственное акционерное общество "Экостар" | Method of preparing lithium hydroxide or salts thereof of high purity from mother liquors |
| RU2196735C1 (en) * | 2001-07-20 | 2003-01-20 | Закрытое акционерное общество "Экостар-Наутех" | Process of extracting monohydrate of high-purity lithium hydroxide from materials containing lithium carbonate |
| US6608008B1 (en) * | 2000-09-20 | 2003-08-19 | Toxco Inc. | Lithium hydroxide compositions |
| CN1486931A (en) * | 2002-09-30 | 2004-04-07 | 南通泛亚锂业有限公司 | Production process of lithium hydroxide monohydrate |
-
2005
- 2005-06-22 CN CNB2005100338127A patent/CN1312040C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2090503C1 (en) * | 1994-09-06 | 1997-09-20 | Научно-производственное акционерное общество "Экостар" | Method of preparing lithium hydroxide or salts thereof of high purity from mother liquors |
| US6608008B1 (en) * | 2000-09-20 | 2003-08-19 | Toxco Inc. | Lithium hydroxide compositions |
| RU2196735C1 (en) * | 2001-07-20 | 2003-01-20 | Закрытое акционерное общество "Экостар-Наутех" | Process of extracting monohydrate of high-purity lithium hydroxide from materials containing lithium carbonate |
| CN1486931A (en) * | 2002-09-30 | 2004-04-07 | 南通泛亚锂业有限公司 | Production process of lithium hydroxide monohydrate |
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Address after: Two kilometers south of Shaoguan City, Guangdong Province, China logistics one or two Patentee after: Ruixin Lithium Energy New material Science and Technology Co., Ltd., Guangzhou Address before: Room two, building 11, 202 precious stone road, Guangzhou economic and Technological Development Zone, Guangdong, China Patentee before: Ruixin Lithium Energy New material Science and Technology Co., Ltd., Guangzhou |
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| DD01 | Delivery of document by public notice |
Addressee: Ruixin Lithium Energy New material Science and Technology Co., Ltd., Guangzhou Document name: Notification of Termination of Patent Right |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070425 Termination date: 20120622 |