CN100379682C - Method for preparing anhydrous magnesium chloride - Google Patents
Method for preparing anhydrous magnesium chloride Download PDFInfo
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- CN100379682C CN100379682C CNB2004100097376A CN200410009737A CN100379682C CN 100379682 C CN100379682 C CN 100379682C CN B2004100097376 A CNB2004100097376 A CN B2004100097376A CN 200410009737 A CN200410009737 A CN 200410009737A CN 100379682 C CN100379682 C CN 100379682C
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Abstract
The present invention relates to a method for preparing anhydrous magnesium chloride, which is characterized in that the method comprises the steps that aqueous solution of magnesium chloride is used as raw material, a solvent extracting method is adopted to selectively extract magnesium in the solution of magnesium chloride, and in this way, water and other impurities are separated effectively; the extraction rate can reach more than 99%, alcoholic solution of hydrogen chloride is used for back extraction to obtain alcoholic solution of anhydrous magnesium chloride, and the back extraction rate can reach more than 99%; ammonia precipitating agents are adopted to generate complex compounds of hexammonate magnesium chloride, and the complex compounds are washed, dried and deaminated to obtain anhydrous magnesium chloride with the purity of 99.3% to 99.5%. The present invention has the advantages of favorable separating effect of water and impurities, simple operation, low consumption of extracting agents, cyclic usage of extracting agents, low cost, reliable technology, economy, reasonableness and industrialized production.
Description
Technical field
The present invention relates to a kind of method for preparing Magnesium Chloride Anhydrous, it is a raw material with the aqueous solution of magnesium chloride, produces the anhydrous magnesium chloride with high purity of electrolytic preparation MAGNESIUM METAL, belongs to chemical field.
Background technology
Magnesium is the lightest structural metal, can constitute the high-strength alloy of excellent property with other metal, has purposes and vast potential for future development widely.China's Qinghai Salt Lake Bittern solubility magnesium salts aboundresources, only the magnesium chloride reserves promptly reach 31.43 hundred million tons, and these developments of resources are good, make good use of, and bring into play it to greatest extent and be worth, be highly significant.Realize effective utilization of this precious resources, a maximum difficult problem is how to remove the crystal water that magnesium chloride has, and prepares highly purified Magnesium Chloride Anhydrous.
The production of metal current magnesium has the electrolytic process of electrolysis Magnesium Chloride Anhydrous and comprises the hot reducing method of Pidgeon process, synthesis by internal resistance electric melting and semi-continuous process, two kinds of methods relatively, electrolytic process is than the hot reducing method advanced technology, the resource utilization height, the product foreign matter content is few, is the developing direction of production MAGNESIUM METAL.
The technology of producing both at home and abroad Magnesium Chloride Anhydrous can be divided into two classes, and a class is to utilize the principle of chemical equilibrium, feeds the hydrolysis that hydrogen chloride gas or chlorine suppresses hydrated magnesium chloride when adding hot brine and obtains Magnesium Chloride Anhydrous thereby adopt.Another kind of is ammoniation process, is about to hydrated magnesium chloride and is dissolved in the organic solvent, removes from this solvent and anhydrates, and alcoholic solution and precipitation agent reaction formation magnesium chloride complex compound by this Magnesium Chloride Anhydrous heat this magnesium chloride complex compound and produce Magnesium Chloride Anhydrous.This method also claims " ammoniation process ".
Disclose ammoniation process in the US2381995 patent of nineteen forty-two M.W.Kellogg company, the preferred primary isoamyl alcohol of this method as precipitation agent, generates magnesium chloride hex-ammoniate with ammonia as the solvent that is used to form hydrated magnesium chloride solution, and promptly molecular formula is MgCl
26NH
3, reheat promptly obtains Magnesium Chloride Anhydrous.But the magnesium chloride of this method is dehydration fully not, when its reason is the alcoholic solution of the hydrated magnesium chloride that heats in order to dewater, temperature about the boiling point of used alcohol can not be removed and anhydrate, and after this many people have adopted the different solvents and the different precipitator method, but effect is all undesirable.Reason is after the magnesium chloride that contains crystal water adds in the organic solvent, the coordination reaction that solvent molecule replaces water takes place, thereby slough the coordinated water molecule, but all alcohols to replace all unusual difficulties of latter two water molecules, if increase alcohol adding amount, then need a large amount of alcohol, anhydrate as adopting distillation method to remove from solution, its difficulty is very big, because alcohol and water evaporates together when boiling, also do not remove when very low at moisture, the boiling point of solution increases, this moment MgCl
2Again and the water that stays reaction and decomposing.On the other hand, dephlegmate not only needs big energy, also cause the alcoholic solution of magnesium chloride to become sticky thick, produce wax shape precipitation, and carry a large amount of alcohol secretly, precipitate and separate and washing are made troubles, after closing with ammino, the alcoholic solution of the magnesium chloride of band water can not obtain the high purity magnesium chloride hex-ammoniate, and hydrolysis in the deamination process, can not obtain meeting the Magnesium Chloride Anhydrous of electrolysis requirement behind the deamination, this shows that above-mentioned method realizes that industrialization has a lot of difficulties.
Summary of the invention
Purpose of the present invention is closed sedimentary a kind of method for preparing Magnesium Chloride Anhydrous from the aqueous solution of magnesium for the shortcoming that overcomes above-mentioned prior art provides with solvent extration, ammino with deficiency just, can produce the anhydrous chlorides of rase magnesium raw material that meets the electrolytic magnesium requirement, make the magnesium resource in the salt lake brine obtain development and use.
The objective of the invention is to realize by following technical proposal:
The method for preparing Magnesium Chloride Anhydrous is characterized in that being undertaken by following step:
A) be that the magnesium chloride brine of 50～120g/l carries out counter-current extraction with di (isooctyl) phosphate or 2-ethylhexyl ester extractant with Mg content, it is 10～50% organic phase that extraction agent is diluted to volumetric concentration with octane-iso or sulfonated kerosene, organic phase is carried out saponification according to a conventional method with ammoniacal liquor or the sodium hydroxide solution of 5～15M again, both consumptions are 8～12: 1 by volume, extraction phase is 1～2 than organic phase volume with water volume O/W, the extraction hop count is 8～12, the extraction time is 5～10 minutes, and the separation of extraction back obtains magniferous saturated organic phase and water;
B), with the hydrogenchloride strippant to the extraction of (a) after magniferous saturated organic phase strip, strippant is 0.5～8M reextraction organic phase with the mixture preparation hydrogen cloride concentration of methyl alcohol, ethanol, ethylene glycol, propyl alcohol, butanols, glycerol or above-mentioned any two or more arbitrary proportion, saturated organic phase is in a ratio of 1～5 with reextraction is organic, the reextraction hop count is 1～2, time is 5～8 minutes, separate after stripping, obtain the Magnesium Chloride Anhydrous alcoholic solution, the organic phase after the reextraction recycles after saponification;
C), the Magnesium Chloride Anhydrous alcoholic solution of (b) is packed in the airtight reactor, under-10～50 ℃ of temperature, feed ammonia and stirring, ammonia feeding amount is centinormal 1 8～12 times an of magnesium ion in the magnesium chloride alcoholic solution, generating post precipitation filters or centrifugation, obtain magnesium chloride hex-ammoniate precipitation and alcoholic solution, to precipitate with the saturated methyl alcohol of ammonia again and wash according to a conventional method 1～3 time, alcoholic solution reclaims through fractionation by distillation and is back to reextraction, and ammonia returns use;
D), again the magnesium chloride hex-ammoniate after (c) washing is deposited in-0.05～-vacuum condition of 0.1MPa down or under the protection of inert gas under 50～120 ℃ of temperature dry 1～3 hour, obtain magnesium chloride hex-ammoniate;
E), at last magnesium chloride hex-ammoniate was being heated deamination 1～3 hour under the protection of inert gas under 400～600 ℃ of temperature, obtain the anhydrous chlorides of rase magnesium products of purity 99.3～99.5%.
Described magnesium chloride brine is the magnesium chloride brine that salt lake brine or magnesium ore make.
The present invention prepares the method for Magnesium Chloride Anhydrous, it is raw material with the magnesium chloride brine, the aqueous solution of the magnesium chloride that comprises salt lake brine or make from magnesium ore, use di (isooctyl) phosphate, be called for short P204 or 2-(ethyl hexyl) ester, be called for short P507 and extract the magnesium that optionally extracts in the magnesium chloride solution, thereby effectively separate with water and other impurity, percentage extraction can reach more than 99%, strip with the hydrogenchloride alcoholic solution again, can obtain anhydrous magnesium chloride alcoholic solution, stripping rate can reach more than 99%, select for use the ammonia precipitation agent to generate magnesium chloride hex-ammoniate complex, the alcohol that complex compound is carried secretly seldom, through washing, dry, it is 993～99.5% Magnesium Chloride Anhydrouss that deamination obtains purity.
Owing to take technique scheme to make the technology of the present invention compared with the prior art have following advantage and effect:
A) magnesium in the magnesium chloride brine produced of extraction of the present invention alternative extraction salt lake brine or magnesium ore, the mass-transfer efficiency height, simple to operate with water and impurity good separating effect, extraction agent consumption seldom and can be recycled, and cost is low;
B) this method and technology is reliable, and is reasonable economically, can realize suitability for industrialized production.
Embodiment
Embodiment 1
With Mg content is 10 liters of the salt lake brines of 50g/l; carry out counter-current extraction with the di (isooctyl) phosphate extraction agent; get 1 liter of di (isooctyl) phosphate with 10 liters of 9 liters of dilutions of octane-iso organic phases; organic phase is carried out saponification for 0.83 liter according to a conventional method with the sodium hydroxide solution of 5M again; extraction phase is 1 than O/W; the extraction hop count is 8; the extraction time is 5 minutes; the separation of extraction back obtains magniferous saturated organic phase and water; strip to extracting the magniferous saturated organic phase in back with the hydrogenchloride strippant; with hydrogenchloride is 10 liters of the reextraction organic phases of 0.5M with methyl alcohol preparation hydrogen cloride concentration; reextraction is in a ratio of 1; the reextraction hop count is 1; time is 5 minutes; separate after stripping; obtain the Magnesium Chloride Anhydrous methanol solution; organic phase after the reextraction recycles after saponification; the Magnesium Chloride Anhydrous methanol solution is packed in the airtight reactor; under-10 ℃ of temperature, feed ammonia and stirring; ammonia feeding amount is centinormal 1 12 times an of magnesium ion in the magnesium chloride methanol solution; generate post precipitation and carry out centrifugation; obtain magnesium chloride hex-ammoniate precipitation and methanol solution; to precipitate again with the saturated methyl alcohol of ammonia and wash according to a conventional method 1 time; methanol solution is back to reextraction through the distillation Separation and Recovery; ammonia returns use; magnesium chloride hex-ammoniate after will washing again is deposited in-vacuum condition of 0.08MPa under under 50 ℃ of temperature dry 3 hours; obtain magnesium chloride hex-ammoniate, at last magnesium chloride hex-ammoniate was being heated deamination 1 hour under the protection of inert gas under 600 ℃ of temperature, obtain the anhydrous chlorides of rase magnesium products of purity 99.3%.
Embodiment 2
With Mg content is 10 liters of the salt lake brines of 70g/l; carry out counter-current extraction with 2-ethylhexyl ester extractant; get 2.4 liters of 2-(ethyl hexyl) esters with 12 liters of 9.6 liters of dilutions of sulfonated kerosene organic phases; organic phase is carried out saponification for 1.2 liters according to a conventional method with the ammoniacal liquor of 8M again; extraction phase is 1.2 than O/W; the extraction hop count is 9; the extraction time is 6 minutes; the separation of extraction back obtains magniferous saturated organic phase and water; strip to extracting the magniferous saturated organic phase in back with the hydrogenchloride strippant; with hydrogenchloride spent glycol preparation hydrogen cloride concentration is 6 liters of the reextraction organic phases of 2.0M; reextraction is in a ratio of 2; the reextraction hop count is 2; time is 8 minutes; separate after stripping; obtain Magnesium Chloride Anhydrous ethylene glycol alcoholic solution; organic phase after the reextraction recycles after saponification; the Magnesium Chloride Anhydrous ethylene glycol solution is packed in the airtight reactor; under 25 ℃ of temperature, feed ammonia and stirring; ammonia feeding amount is centinormal 1 10 times an of magnesium ion in the magnesium chloride ethylene glycol solution; generate post precipitation and carry out centrifugation; obtain magnesium chloride hex-ammoniate precipitation and ethylene glycol solution; to precipitate again with the saturated methyl alcohol of ammonia and wash according to a conventional method 1 time; ethylene glycol solution is back to reextraction through the distillation Separation and Recovery; ammonia returns use; magnesium chloride hex-ammoniate after will washing again is deposited in-vacuum condition of 0.1MPa under under 80 ℃ of temperature dry 2 hours; obtain magnesium chloride hex-ammoniate, at last magnesium chloride hex-ammoniate was being heated deamination 1.5 hours under the protection of inert gas under 500 ℃ of temperature, obtain the anhydrous chlorides of rase magnesium products of purity 99.5%.
Embodiment 3
With Mg content is 10 liters of the magnesium chloride brines that make of the magnesium ore of 100g/l; carry out counter-current extraction with the di (isooctyl) phosphate extraction agent; get 4.5 liters of di (isooctyl) phosphates with 15 liters of 10.5 liters of dilutions of sulfonated kerosene organic phases; organic phase is carried out saponification for 1.67 liters according to a conventional method with the sodium hydroxide solution of 12M again; extraction phase is 1.5 than O/W; the extraction hop count is 10; the extraction time is 8 minutes; the separation of extraction back obtains magniferous saturated organic phase and water; strip to extracting the magniferous saturated organic phase in back with the hydrogenchloride strippant; with hydrogenchloride is 5 liters of the reextraction organic phases of 4M with the mixing solutions preparation hydrogen cloride concentration of the propyl alcohol of 1: 1 volume ratio and butanols; reextraction is in a ratio of 3; the reextraction hop count is 1; time is 8 minutes; separate after stripping; obtain the propyl alcohol of Magnesium Chloride Anhydrous and the mixing solutions of butanols; organic phase after the reextraction recycles after saponification; the propyl alcohol of Magnesium Chloride Anhydrous and butanol solution are packed in the airtight reactor; under 50 ℃ of temperature, feed ammonia and stirring; ammonia feeding amount is centinormal 19 times an of magnesium ion in the magnesium chloride alcoholic solution; generate post precipitation and carry out centrifugation; obtain magnesium chloride hex-ammoniate precipitation and propyl alcohol; butanol solution; to precipitate again with the saturated methyl alcohol of ammonia and wash according to a conventional method 3 times; propyl alcohol and butanols mixing solutions are back to reextraction through the distillation Separation and Recovery; ammonia returns use; magnesium chloride hex-ammoniate after will washing again is deposited in-vacuum condition of 0.05MPa under under 120 ℃ of temperature dry 1 hour; obtain magnesium chloride hex-ammoniate; at last magnesium chloride hex-ammoniate is heated deamination 3 hours under the protection of inert gas under 400 ℃ of temperature, obtaining the anhydrous chlorides of rase magnesium products of purity 99.4%.
Embodiment 4
With Mg content is 10 liters of the salt lake brines of 120g/l; carry out counter-current extraction with 2-ethylhexyl ester extractant; get 10 liters of 2-(ethyl hexyl) esters with 20 liters of 10 liters of dilutions of octane-iso organic phases; organic phase is carried out saponification for 2.5 liters according to a conventional method with the ammoniacal liquor of 15M again; extraction phase is 2 than O/W; the extraction hop count is 12; the extraction time is 10 minutes; the separation of extraction back obtains magniferous saturated organic phase and water; strip to extracting the magniferous saturated organic phase in back with the hydrogenchloride strippant; with the methyl alcohol of hydrogenchloride with 1: 0.5: 0.5 volume ratio; ethanol and glycerol alcohol mixture preparation hydrogen cloride concentration is 4 liters of the reextraction organic phases of 8M; reextraction is in a ratio of 5; the reextraction hop count is 2; time is 7 minutes; separate after stripping; obtain Magnesium Chloride Anhydrous methyl alcohol; ethanol and glycerol alcohol mixture solution; organic phase after the reextraction recycles after saponification; Magnesium Chloride Anhydrous methyl alcohol; ethanol; glycerol solution is packed in the airtight reactor; under 0 ℃ of temperature, feed ammonia and stirring; ammonia feeding amount is centinormal 18 times an of magnesium ion in the magnesium chloride alcoholic solution; generate post precipitation and carry out centrifugation; obtain magnesium chloride hex-ammoniate precipitation and methyl alcohol; ethanol and glycerol alcohol mixture solution; to precipitate again with the saturated methyl alcohol of ammonia and wash according to a conventional method 2 times; methyl alcohol; ethanol and glycerol alcohol mixture solution are back to reextraction through the distillation Separation and Recovery; ammonia returns use; magnesium chloride hex-ammoniate after will washing again is deposited in-vacuum condition of 0.1MPa under under 100 ℃ of temperature dry 1.2 hours; obtain magnesium chloride hex-ammoniate; at last magnesium chloride hex-ammoniate is heated deamination 1.2 hours under the protection of inert gas under 550 ℃ of temperature, obtaining the anhydrous chlorides of rase magnesium products of purity 99.3%.
Claims (2)
1. method for preparing Magnesium Chloride Anhydrous is characterized in that being undertaken by following step:
(a) be that the magnesium chloride brine of 50～120g/l carries out counter-current extraction with di (isooctyl) phosphate or 2-ethylhexyl ester extractant with Mg content, it is 10～50% organic phase that extraction agent is diluted to volumetric concentration with octane-iso or sulfonated kerosene, organic phase is carried out saponification according to a conventional method with ammoniacal liquor or the sodium hydroxide solution of 5～15M again, both consumptions are 8～12: 1 by volume, extraction phase is 1～2 than organic phase volume with water volume ratio O/w, the extraction hop count is 8～12, the extraction time is 5～10 minutes, and the separation of extraction back obtains magniferous saturated organic phase and water:
B), with the hydrogenchloride strippant to the extraction of (a) after magniferous saturated organic phase strip, strippant is 0.5～8M reextraction organic phase with the mixture preparation hydrogen cloride concentration of methyl alcohol, ethanol, ethylene glycol, propyl alcohol, butanols, glycerol or above-mentioned any two or more arbitrary proportion, saturated organic phase is in a ratio of 1～5 with reextraction is organic, the reextraction hop count is 1～2, time is 5～8 minutes, separate after stripping, obtain the Magnesium Chloride Anhydrous alcoholic solution, the organic phase after the reextraction recycles after saponification:
C), the Magnesium Chloride Anhydrous alcoholic solution of (b) is packed in the airtight reactor, under-10～50 ℃ of temperature, feed ammonia and stirring, ammonia feeding amount is centinormal 1 8～12 times an of magnesium ion in the magnesium chloride alcoholic solution, generating post precipitation filters or centrifugation, obtain magnesium chloride hex-ammoniate precipitation and alcoholic solution, to precipitate with the saturated methyl alcohol of ammonia again and wash according to a conventional method 1～3 time, alcoholic solution reclaims through fractionation by distillation and is back to reextraction, and ammonia returns use;
D), again the magnesium chloride hex-ammoniate after (c) washing is deposited in-0.05～-vacuum condition of 0.1MPa down or under the protection of inert gas under 50～120 ℃ of temperature dry 1～3 hour, obtain magnesium chloride hex-ammoniate;
E), at last magnesium chloride hex-ammoniate was being heated deamination 1～3 hour under the protection of inert gas under 400～600 ℃ of temperature, obtain the anhydrous chlorides of rase magnesium products of purity 99.3～99.5%.
2. method according to claim 1 is characterized in that described magnesium chloride brine is the magnesium chloride brine that salt lake brine or magnesium ore make.
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| CNB2004100097376A CN100379682C (en) | 2004-11-01 | 2004-11-01 | Method for preparing anhydrous magnesium chloride |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336422B (en) * | 2010-07-14 | 2013-08-21 | 中国科学院过程工程研究所 | Method for circulating fluidized bed pyrolysis and deamination of magnesium chloride hexammoniate and equipment thereof |
| CN101983922B (en) * | 2010-11-16 | 2012-05-09 | 华东理工大学 | Method for preparing anhydrous magnesium chloride by calcining and deaminating magnesium chloride hexammoniate |
| CN103818942B (en) * | 2014-01-22 | 2015-03-18 | 中国科学院上海硅酸盐研究所 | Method for preparing high-purity anhydrous strontium iodide |
| CN105256151B (en) * | 2015-10-14 | 2017-07-21 | 上海大学 | The method that the magnesium chloride in serpentine is extracted with ethanol |
| CN106673028A (en) * | 2015-11-09 | 2017-05-17 | 虔东稀土集团股份有限公司 | Preparation method of alkaline earth metal compound |
| CN106348321B (en) * | 2016-08-30 | 2017-10-24 | 荆门市格林美新材料有限公司 | The method that magnesium prepares high-purity fire retardant is reclaimed from the industrial magnesium solution containing cobalt of cobalt nickel |
| CN114014346B (en) * | 2021-12-21 | 2024-03-26 | 深圳市美凯特科技有限公司 | Preparation method of anhydrous magnesium chloride |
| CN116969489A (en) * | 2022-04-21 | 2023-10-31 | 中国科学院过程工程研究所 | Method for removing magnesium from salt lake brine |
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|---|---|---|---|---|
| CN1135743A (en) * | 1993-10-28 | 1996-11-13 | 联邦科学及工业研究组织 | Anhydrous magnesium chloride |
| CN1333183A (en) * | 2001-08-17 | 2002-01-30 | 华东理工大学 | Methodf or preparing anhydrous magnesium chloride |
| CN1412114A (en) * | 2001-10-08 | 2003-04-23 | 谷亮 | New process for preparing anhydrous magnesium chloride |
| JP2004083298A (en) * | 2002-08-23 | 2004-03-18 | Toho Titanium Co Ltd | Method for manufacturing magnesium chloride anhydride and extracting apparatus for fused magnesium chloride |
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2004
- 2004-11-01 CN CNB2004100097376A patent/CN100379682C/en not_active Expired - Fee Related
Patent Citations (4)
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|---|---|---|---|---|
| CN1135743A (en) * | 1993-10-28 | 1996-11-13 | 联邦科学及工业研究组织 | Anhydrous magnesium chloride |
| CN1333183A (en) * | 2001-08-17 | 2002-01-30 | 华东理工大学 | Methodf or preparing anhydrous magnesium chloride |
| CN1412114A (en) * | 2001-10-08 | 2003-04-23 | 谷亮 | New process for preparing anhydrous magnesium chloride |
| JP2004083298A (en) * | 2002-08-23 | 2004-03-18 | Toho Titanium Co Ltd | Method for manufacturing magnesium chloride anhydride and extracting apparatus for fused magnesium chloride |
Non-Patent Citations (2)
| Title |
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| 高纯度无水氯化镁生产工艺评述. 陈荣等.江苏化工，第29卷第6期. 2001 * |
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Assignee: Zhongxinguoan Mengguli Power Supply Technology Co., Ltd. Assignor: Zhongxin Guoan Mengguli New Energy Sources Science and Technology Co., Ltd. Contract record no.: 2011110000118 Denomination of invention: Method for preparing anhydrous magnesium chloride Granted publication date: 20080409 License type: Exclusive License Open date: 20050406 Record date: 20110720 |
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