CN1313373C - Process for producing lithium carbonate magnesium oxide and hydrogen chloride by high magnesium lithium-containing halogen water - Google Patents
Process for producing lithium carbonate magnesium oxide and hydrogen chloride by high magnesium lithium-containing halogen water Download PDFInfo
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- CN1313373C CN1313373C CNB2005100858329A CN200510085832A CN1313373C CN 1313373 C CN1313373 C CN 1313373C CN B2005100858329 A CNB2005100858329 A CN B2005100858329A CN 200510085832 A CN200510085832 A CN 200510085832A CN 1313373 C CN1313373 C CN 1313373C
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- hydrochloric acid
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Abstract
本发明属于盐化工技术领域，尤其涉及一种用高镁含锂卤水生产碳酸锂、氧化镁和盐酸的方法。该方法的工艺流程为喷雾干燥、煅烧、加水洗涤、蒸发浓缩、沉淀工序后得到碳酸锂产品，煅烧工序后产生的混合气体经盐酸吸收工序后得工业盐酸产品，加水洗涤工序产生的滤饼经干燥后得高纯氧化镁产品，工艺条件喷雾干燥工序的进料温度为室温～130℃，喷雾干燥塔进风温度为200～450℃，出风温度为150～240℃，煅烧温度为554～1200℃，煅烧时间为0.5秒～2.5小时，蒸发浓缩工序的控制终点为卤水中Li+含量为14～21g/l。此方法不但有效解决了高镁含锂卤水镁锂分离生产碳酸锂的关键技术难题，而且又获得了价高质优的碳酸锂和高纯氧化镁产品，又副产了工业盐酸，从而降低了生产成本，资源得到了有效的综合利用，有较好的实用价值。
The invention belongs to the technical field of salt chemical industry, and in particular relates to a method for producing lithium carbonate, magnesium oxide and hydrochloric acid by using high-magnesium lithium-containing brine. The technical process of the method is to obtain lithium carbonate product after spray drying, calcining, washing with water, evaporation and concentration, and precipitation; the mixed gas produced after the calcining process is subjected to the hydrochloric acid absorption process to obtain industrial hydrochloric acid product; After drying, high-purity magnesium oxide products are obtained. The process conditions of the spray drying process are: the feed temperature of the spray drying process is from room temperature to 130°C, the inlet air temperature of the spray drying tower is 200-450°C, the outlet air temperature is 150-240°C, and the calcination temperature is 554-240°C. 1200°C, the calcination time is 0.5 seconds to 2.5 hours, and the control end point of the evaporation and concentration process is that the Li + content in the brine is 14 to 21 g/l. This method not only effectively solves the key technical problem of separating magnesium and lithium from high-magnesium lithium-containing brine to produce lithium carbonate, but also obtains high-quality lithium carbonate and high-purity magnesium oxide products, and produces industrial hydrochloric acid as a by-product, thereby reducing the production cost of lithium carbonate. The production cost and resources are effectively comprehensively utilized, and the utility model has good practical value.
Description
One, technical field:
The invention belongs to the salt chemical engineering technical field, relate in particular to a kind of method of producing Quilonum Retard, magnesium oxide and hydrochloric acid with high-Mg Li-contained bittern.
Two, technical background:
Utilize high-Mg Li-contained bittern to produce Quilonum Retard, the sepn process one of magnesium lithium is directly subordinate to global problem, and traditional method has the precipitator method, extraction process etc., and the defective of the precipitator method is that the rate of recovery is lower than 30%, and also there are the high deficiency of production cost in production cost height, extraction process.
Three, summary of the invention:
What the objective of the invention is to design at the deficiencies in the prior art a kind ofly produces Quilonum Retard with high-Mg Li-contained bittern, the method of magnesium oxide and hydrochloric acid, this method is used and is carried potassium, the lithium bischofite saturated solution of carrying behind the boron that contains is the raw material production Quilonum Retard, by-product high-purity magnesium oxide and hydrochloric acid, this method has not only solved the key technical problem of Mg and Li from high-Mg Li-contained bittern separation of produced Quilonum Retard, and by-product hydrochloric acid can be used as the cheap raw material in boric acid workshop in the sepn process of magnesium lithium, the high-purity magnesium oxide product can also obtain fair margin of profit, thereby effectively reduce production cost, make resource obtain comprehensive utilization preferably.
Technical scheme is: the raw material high-Mg Li-contained bittern is to carry potassium, carry the bischofite saturated solution behind the boron.The technical process of this method is as shown in Figure 1: technical process is spraying drying, calcine, add after water washing, evaporation concentration, the precipitation operation lithium carbonate product, the mixed gas that produces behind the calcination process after hydrochloric acid absorbs operation the technical hydrochloric acid product, add after the filter cake drying operation that the water washing operation produces the high-purity magnesium oxide product; Processing condition are that the feeding temperature of spraying drying operation high-Mg Li-contained bittern is room temperature～130 ℃, the inlet temperature of spray-drying tower is 200～450 ℃, exhaust temperature is 150～240 ℃, the calcining temperature of calcination process is 554～1200 ℃, calcination time is 0.5 second～2.5 hours, and hydrochloric acid absorbs operation and mixed gas is cooled to is lower than 200 ℃ and enters the hydrochloric acid absorption unit again and produce hydrochloric acid.Spraying drying is that the raw material high-Mg Li-contained bittern is removed by filter insolubles impurity earlier, dewater with spray-dired method again and make the process that contains the lithium magnesium chloride, containing the lithium magnesium chloride is lithium chloride, magnesium chloride+crystal water, spray drying device can be selected drying machine with centrifugal spray for use, Pressuresprayingdrier or Airstreamsprayingdrier are for control solid product major part becomes MgCl
22H
2O or MgCl
2H
2O, the feeding temperature of this operation high-Mg Li-contained bittern are room temperature～130 ℃, and the inlet temperature of spray-drier is 200～450 ℃, and the air outlet temperature of tail gas is 150～240 ℃.Calcination process is to be under 554～1200 ℃ with containing the lithium magnesium chloride in calcining temperature, calcination time is 0.5 second～2.5 hours, make it to become the process of solid and mixed gas, this operation can adopt rotary calciner, fluidized-bed kiln or eddy flow dynamic calcining stove, inlet temperature is generally 554～800 ℃ when adopting rotary calciner and fluidized-bed kiln, air outlet temperature is 150～300 ℃, inlet temperature is 850～1200 ℃ when adopting eddy flow dynamic calcining stove, 620～820 ℃ of air outlet temperatures, the tail gas gas solid separation can be finished with cyclonic separator or sack cleaner.It is to absorb the process of making the technical hydrochloric acid product with the mixed gas that the hydrochloric acid absorption unit will contain hydrogenchloride that hydrochloric acid absorbs operation, the mixed gas of this operation is because temperature is higher than the temperature that domestic hydrochloric acid absorption equipment can bear, should at first it be cooled to and enter hydrochloric acid absorption unit absorption hydrochloric acid when being lower than 200 ℃ again, the method for cooling can take to mix the method for cold wind or spray cold water in the mixed gas pipeline.Add the water washing operation and be the process that the solid matter that obtains after will calcination process handling washs with fresh water, this operation can be the NaCl in the solid, KCl, LiCl and undecomposed MgCl
2Dissolving enters liquid phase, and wash temperature is a room temperature, in order to access washing effect and water saving preferably, preferably adopts countercurrent washing 3～6 times.The evaporation concentration operation is that magnesium, the calcium impurities of influence precipitation Quilonum Retard purity in the washings are removed, and revaporization dewaters and makes Li in the bittern
+Content is the process of 14～21g/l.The calcium magnesium addition can be removed with precipitation and filtering method.The precipitation operation is to add excessive soda ash in concentrated solution, makes Li
+Be precipitated as Quilonum Retard, refilter the process that obtains lithium carbonate product.Drying process is filtration cakes torrefaction to be dewatered obtain the process of high-purity magnesium oxide product.
Method of the present invention not only efficiently solves the gordian technique difficult problem of Mg and Li from high-Mg Li-contained bittern separation of produced Quilonum Retard, and the valency that obtained again high Quilonum Retard and high-purity magnesium oxide product of fine quality, again by-product technical hydrochloric acid, thereby effectively reduce production cost, resource has obtained effective utilization, and good economic benefits and social benefit are arranged.
Four, description of drawings:
Fig. 1 is a process flow diagram of the present invention.The front is described further, here no longer narration.
Five, embodiment:
Embodiment 1: be raw material with the high-Mg Li-contained bittern, after precipitating the insolubles of removing in the bittern, the feeding temperature of spraying drying operation is a room temperature, the inlet temperature of spray-drying tower is 450 ℃, air outlet temperature is 240 ℃ a condition drying, output contains the lithium magnesium chloride solids, calcined 2.5 hours under 554 ℃ calcining temperature with rotary calciner during calcining, obtain solid otide containing lighium magnesium, wherein the pyrolysis rate of magnesium chloride can reach 96%, and the rate of recovery of lithium reaches 96.5%, with fresh water countercurrent washing 3 times, the filter cake drying dewaters and obtains MgO content is 99% high-purity magnesium oxide, and revaporization was concentrated to Li in the bittern after washing lotion was removed impurity
+During for 14g/l, behind the disgorging, concentrated solution is added soda ash precipitation Quilonum Retard, at last the precipitation solid-liquid separation is just obtained lithium carbonate product, hydrochloric acid absorbs and can make the technical hydrochloric acid product with the processing of hydrochloric acid absorption unit again after operation cools to 150 ℃ with mixed gas earlier.
Embodiment two: with high-Mg Li-contained bittern is raw material, precipitation is removed in the bittern behind the water-insoluble, spray-dired feeding temperature is 130 ℃, the inlet temperature of spray-drying tower is 200 ℃, air outlet temperature is dry under 150 ℃ of conditions, obtain containing the lithium magnesium chloride solids, calcined 0.5 second under 1200 ℃ of temperature condition with eddy flow dynamic calcining stove during calcining, obtain solid otide containing lighium magnesium, use the fresh water countercurrent washing again 6 times, the filter cake drying dewaters and obtains MgO content is 99.4% high-purity magnesium oxide product, and washing lotion revaporization after removal of impurities is concentrated to Li in the bittern
+During for 21g/l, disgorging, concentrated solution is added excessive soda ash precipitation Quilonum Retard, precipitated solid is separated obtaining lithium carbonate product at last, handle just obtaining the technical hydrochloric acid product after hydrochloric acid absorption operation cools to mixed gas about 199 ℃ earlier again with the hydrochloric acid absorption unit.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100858329A CN1313373C (en) | 2005-07-17 | 2005-07-17 | Process for producing lithium carbonate magnesium oxide and hydrogen chloride by high magnesium lithium-containing halogen water |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100858329A CN1313373C (en) | 2005-07-17 | 2005-07-17 | Process for producing lithium carbonate magnesium oxide and hydrogen chloride by high magnesium lithium-containing halogen water |
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|---|---|
| CN1724372A CN1724372A (en) | 2006-01-25 |
| CN1313373C true CN1313373C (en) | 2007-05-02 |
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| CNB2005100858329A Expired - Lifetime CN1313373C (en) | 2005-07-17 | 2005-07-17 | Process for producing lithium carbonate magnesium oxide and hydrogen chloride by high magnesium lithium-containing halogen water |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100453463C (en) * | 2006-12-21 | 2009-01-21 | 青海中信国安科技发展有限公司 | Process and apparatus for preparing magnesium oxide and hydrogen chloride mixed gas by two-stage dynamic calcining of magnesium chloride |
| CN104577243B (en) * | 2014-11-24 | 2017-05-10 | 北京化工大学 | Method for recovering lithium resource from lithium-ion-containing solution by using lithium ion carrier |
| CN106430258B (en) * | 2016-12-13 | 2017-11-17 | 宜春银锂新能源有限责任公司 | Byproduct collecting apparatus in a kind of lithium carbonate preparation process |
| CN114477772B (en) * | 2022-01-30 | 2023-07-25 | 山东国瓷功能材料股份有限公司 | High-strength high-permeability glass ceramic structure, preparation method thereof and obtained product |
| CN117699740A (en) * | 2023-12-01 | 2024-03-15 | 安徽金禾实业股份有限公司 | A method for recovering hydrochloric acid from magnesium oxide production tail gas |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454843A (en) * | 2003-03-21 | 2003-11-12 | 钟辉 | Magnesium sulfate hypotype salt lake brine magnesium lithium separation method |
| CN1502557A (en) * | 2002-11-22 | 2004-06-09 | 王 军 | Method for one-step extracting lithium carbonate from high magnesium lithium ratio salt lake bittern |
| US6764584B2 (en) * | 2002-10-22 | 2004-07-20 | Industrial Technology Research Institute | Process for producing lithium concentrate from brine or seawater |
-
2005
- 2005-07-17 CN CNB2005100858329A patent/CN1313373C/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6764584B2 (en) * | 2002-10-22 | 2004-07-20 | Industrial Technology Research Institute | Process for producing lithium concentrate from brine or seawater |
| CN1502557A (en) * | 2002-11-22 | 2004-06-09 | 王 军 | Method for one-step extracting lithium carbonate from high magnesium lithium ratio salt lake bittern |
| CN1454843A (en) * | 2003-03-21 | 2003-11-12 | 钟辉 | Magnesium sulfate hypotype salt lake brine magnesium lithium separation method |
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Effective date of registration: 20171213 Address after: 816099 Building No. 24, Golmud City, Qinghai Province, No. 1 Patentee after: QINGHAI ZHONGXIN GUOAN LITHIUM DEVELOPMENT CO.,LTD. Address before: 816000 Qaidam West Road, Golmud, Qinghai Province, No. 16 Patentee before: QINGHAI CITIC GUOAN SCIENCE AN |
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