CN101462746A - Method for preparing anhydrous magnesium chloride from bischofite - Google Patents
Method for preparing anhydrous magnesium chloride from bischofite Download PDFInfo
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- CN101462746A CN101462746A CNA2007101798659A CN200710179865A CN101462746A CN 101462746 A CN101462746 A CN 101462746A CN A2007101798659 A CNA2007101798659 A CN A2007101798659A CN 200710179865 A CN200710179865 A CN 200710179865A CN 101462746 A CN101462746 A CN 101462746A
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- bischofite
- ammoniate
- ammonia
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Abstract
The invention relates to a method for preparing anhydrous magnesium chloride from bischofite, which uses the bischofite as a raw material for preparing the anhydrous magnesium chloride. The method comprises the following technical processes: (1) firstly, drying the bischofite for dewatering most crystallization water; (2) dissolving the dried magnesium chloride in glycol for preparing a glycol solution of the magnesium chloride and using a vacuum distillation method for dewatering water in the glycol solution of the magnesium chloride; (3) reacting the dewatered glycol solution of the magnesium chloride with ammonia for crystallizing so as to generate magnesium chloride hexammoniate crystals; (4) washing, filtering and drying for obtaining the magnesium chloride hexammoniate crystals; and (5) heating, decomposing and deaminating the dried magnesium chloride hexammoniate crystals for preparing the anhydrous magnesium chloride. In each process, ammonia gas, detergent and a crystallization mother liquor are recycled. The process has the characteristics of convenient operation, easy large-scale production, low energy consumption, low product cost and no pollution to environment and the prepared anhydrous magnesium chloride can be used as a raw material for producing magnesium metal by an electrolysis method.
Description
Technical field
The present invention relates to a kind of method for preparing Magnesium Chloride Anhydrous by bischofite.
Background technology
The production method of MAGNESIUM METAL generally has two kinds: hot reducing method and electrolysis Magnesium Chloride Anhydrous method.Hot reducing method technology is simple, and cost of investment is low, but its energy consumption height, resource utilization is low and serious environment pollution.The method operation of electrolysis Magnesium Chloride Anhydrous is more, the cost height, but with hot reducing method comparatively speaking, energy consumption is lower, and is less to the pollution that environment brings, and is a green, environmental protection, the production method of continuable MAGNESIUM METAL.
The raw material of electrolytic process production MAGNESIUM METAL is highly purified Magnesium Chloride Anhydrous, and the Magnesium Chloride Anhydrous preparation is the key of electrolysis process production MAGNESIUM METAL.According to the difference of raw material and technology, Magnesium Chloride Anhydrous generally has four kinds of preparation methods:
(1) dewatering bischofite is produced Magnesium Chloride Anhydrous under the hydrogen chloride gas protection.Contain abundant magnesium chloride resource in salt lake brine and the salt pan bittern,, can obtain bischofite (MgCl through removal of impurities separation and purifying
26H
2O).Bischofite is under the protection of hydrogen chloride gas, and crystal water is sloughed in heating, obtains Magnesium Chloride Anhydrous.The subject matter that this method exists is: hydrogenchloride is corrosive gases, to having relatively high expectations of equipment material; Side reaction can only suppress, and can not prevent fully; Composition more complicated in salt lake brine and the salt pan bittern, impurity are difficult to separate fully or remove, and have influenced the purity of anhydrous chlorides of rase magnesium products, and Installed capital cost is very high simultaneously, the running cost height.
(2) magnesite calcining chlorination production Magnesium Chloride Anhydrous.The magnesite high-temperature calcination generates magnesium oxide, the following and chlorine reaction generation Magnesium Chloride Anhydrous of magnesium oxide high temperature.This method efficient is very low, and safety and problem of environmental pollution are outstanding, and in addition, the material lifetime of energy consumption and chlorination furnace also is the problem that merits attention, and therefore, this technology generally seldom is used now.
(3) the double salt method is produced Magnesium Chloride Anhydrous.Bischofite and ammonium chloride can form the ammonia carnallitite, and the ammonia carnallitite dewaters, takes off amine step by step promptly can obtain Magnesium Chloride Anhydrous.The recovery difficulty of ammonium chloride in this method, in addition, the purity of Magnesium Chloride Anhydrous is not high, still contains higher magnesium oxide.
(4) ammoniation process is produced Magnesium Chloride Anhydrous.It is medium with the organic solvent generally that ammino closes dehydration production Magnesium Chloride Anhydrous, and organic solvent commonly used has small molecule alcohols such as methyl alcohol, ethanol, ethylene glycol.The organic solution that at first prepares magnesium chloride feeds ammonia or liquefied ammonia then, then can obtain the magnesium chloride hex-ammoniate crystal, washs, calcines magnesium chloride hex-ammoniate at last, then can obtain purified anhydrous chlorides of rase magnesium products.This process is finished under mild conditions, does not produce poisonous and hazardous material, therefore, compares with other method, and the process that ammoniation process is produced Magnesium Chloride Anhydrous is the technology of a green, environmental protection.The patent No. is that the patent of CN94194221.X and CN01126495.0 is a raw material with the bischofite, directly prepares Magnesium Chloride Anhydrous by ammoniation process.Yet at present bischofite raw material ammonification legal system is equipped with Magnesium Chloride Anhydrous and has following problem: it is big that (1) unit product does not have aqueous organic media cycle consumption amount, the efficient raising of still needing; (2) unit product dehydration energy consumption is higher.
Summary of the invention
Purpose of the present invention: (1) reduces unit product does not have aqueous organic media cycle consumption amount, for this reason, at first adopt drying meanss such as fluidization that the combination water major part in the bischofite is sloughed, obtain crystal water content less than 27.5% magnesium chloride powder, adopt the organic medium distillating method to slough remainder water then; (2) improve the magnesium chloride output capacity of unit organic solvent, thereby cut down the consumption of energy.The corresponding like this dewatering efficiency that improved.
For achieving the above object, technical solution of the present invention provides and a kind ofly prepares the method for Magnesium Chloride Anhydrous by bischofite, comprising: the reaction distillation dehydration technique of the fluidized drying dehydration technique of bischofite, the preparation of Magnesium Chloride Anhydrous organic solution, the fluidization reactive crystallization technology and the deamination reaction technology of magnesium chloride hex-ammoniate preparation.This processing method is: (1) bischofite drying is sloughed most of crystal water; (2) dried magnesium chloride is dissolved in the ethylene glycol ethylene glycol solution of preparation magnesium chloride, adopts the vacuum distilling method to slough moisture in the magnesium chloride ethylene glycol solution simultaneously; (3) ethylene glycol solution of the magnesium chloride after the dehydration and ammonia react crystallization generate the magnesium chloride hex-ammoniate crystal; (4) filtration, washing, the dry magnesium chloride hex-ammoniate crystal that gets; (5) exsiccant magnesium chloride hex-ammoniate thermolysis deamination is made Magnesium Chloride Anhydrous.Ammonia, washing composition and crystalline mother solution recycles in each process.
Describedly prepare the method for Magnesium Chloride Anhydrous by bischofite, it comprises the following steps:
1) bischofite (MgCl
26H
2O) drying makes MgCl
26H
2O sloughs most crystal water, gets moisture low magnesium chloride powder.
2) with 1) the magnesium chloride powder that makes of step mixes with ethylene glycol, the ethylene glycol solution of preparation magnesium chloride simultaneously, adds an amount of ammonium chloride in the ethylene glycol solution of magnesium chloride, mix, adopt the vacuum distilling dewatering to make that water content is lower than 1% in the ethylene glycol solution of magnesium chloride simultaneously.
3) with 2) water content that makes of the step ethylene glycol solution that is lower than 1% magnesium chloride at first mixes with liquefied ammonia, introduces the fluidized-bed reaction crystallizer then, feeds ammonia simultaneously from the bottom, and reactive crystallization generates magnesium chloride hex-ammoniate and precipitates.
4) with 3) the magnesium chloride hex-ammoniate washing, filtration, the drying that make of step make the magnesium chloride hex-ammoniate crystal.
5) with 4) go on foot the magnesium chloride hex-ammoniate crystal that makes, under 400-500 ℃ of condition, keep 30-120min. to slough ammonia, get Magnesium Chloride Anhydrous, the ammonia recycle of sloughing; Under temperature 714-800 ℃, Magnesium Chloride Anhydrous becomes liquid state, leaves standstill 30-60min., obtains the liquid anhydrous magnesium chloride, can directly introduce electrolyzer and smelt magnesium.
Describedly prepare the method for Magnesium Chloride Anhydrous by bischofite, it is described 1 years old) step bischofite (MgCl
26H
2O) drying and dehydrating adopts the fluidized drying technology, and it has heat transfer, mass transfer is fast, energy consumption is low, and temperature is even; The drying and dehydrating temperature obtains crystal water content less than 27.5% magnesium chloride powder under 170-220 ℃ of condition.
The described method for preparing Magnesium Chloride Anhydrous by bischofite, they are described 2 years old) dried bischofite of step is dissolved in the ethylene glycol solution of ethylene glycol magnesium chloride, adding is the ammonium chloride of basic 8wt%-12wt% with bischofite, to eliminate the magnesium oxide that generates because of hydrolysis; The ethylene glycol solution of the magnesium chloride of preparation adopts the method for vacuum distilling to slough wherein moisture, 100-160 ℃ of temperature, vacuum tightness 500mmHg-700mmHg, until the solution water content less than 1%.
The described method for preparing Magnesium Chloride Anhydrous by bischofite, they are described 3 years old) step crystalline mother solution at first use liquefied ammonia saturated, then with the ammonia counter-current operation, reaction generates the magnesium chloride hex-ammoniate crystal in the fluidized-bed reaction crystallizer, Tc is controlled at 15-20 ℃, and the residence time is controlled at 20-120min..
Describedly prepare the method for Magnesium Chloride Anhydrous by bischofite, they are described 4 years old) step selects by the saturated ethanol of ammonia as washing composition.
Describedly prepare the method for Magnesium Chloride Anhydrous by bischofite, they are described 5 years old) step under temperature 80-100 ℃ condition, the magnesium chloride hex-ammoniate crystal after the dry washing; Exsiccant magnesium chloride hex-ammoniate crystal under 400-500 ℃ of condition, keeps 30-120min. to slough ammonia and gets the Magnesium Chloride Anhydrous powder, the ammonia recycle of sloughing; Under temperature 714-800 ℃, Magnesium Chloride Anhydrous becomes liquid state, leaves standstill 30-60min., obtains the liquid anhydrous magnesium chloride, can directly introduce electrolyzer and smelt magnesium.
The invention has the advantages that: (1) bischofite drying and dehydrating process does not need painstakingly to prevent hydrolysis, easy to operate, processing condition wide ranges.(2) because bischofite has at first been sloughed most crystal water in the bischofite by drying, therefore reduced the consumption of the required organic solvent of preparation unit weight Magnesium Chloride Anhydrous (ethylene glycol) (with bischofite (MgCl
26H
2O) directly the dehydration of organic solvent method is compared, and has reduced consumption of organic solvent 35%-45%), reduce unit product and do not have the aqueous organic media internal circulating load, improve the magnesium chloride output capacity of unit organic solvent, cut down the consumption of energy.(3) reactive crystallization prepares before the magnesium chloride hex-ammoniate, adopts the method for dry and vacuum distilling, almost completely removes moisture, has eliminated the influence of moisture to the magnesium chloride hex-ammoniate crystal mass.(4) the magnesium chloride hex-ammoniate reaction crystallization process adopts fluidized-bed-reaction crystalizer, has strengthened mass transfer, the heat transfer of process, has improved the homogeneity that crystal particle diameter distributes.(5) molten state is cooled off the block Magnesium Chloride Anhydrous of preparation, easier preservation, transportation again.
Description of drawings
Fig. 1 forms and process flow diagram for the inventive method equipment used;
Fig. 2 is the crystal Electronic Speculum scintigram that obtained in 5.3% o'clock for water-content in the crystalline mother solution;
Fig. 3 is the magnesium chloride hex-ammoniate crystalline electron-microscope scanning figure that obtained in 0.2% o'clock for water-content in the crystalline mother solution;
Fig. 4 is magnesium chloride hex-ammoniate XRD figure spectrum;
Fig. 5 magnesium chloride hex-ammoniate in-situ high temperature X-ray diffraction spectrogram.
Embodiment
As shown in Figure 1, for present method equipment used is formed synoptic diagram, wherein, and sulfuration bed dryer 1, dissolving tank 2, distillation tower 3, crystallizer 4, strainer 5, washer 6, sulfuration bed dryer 7, sulfuration bed calcining kiln 8, each parts connects routinely.
From Fig. 1 as seen, the concrete enforcement of the inventive method comprises that step is as follows:
(1) chloromagnesite (MgCl
26H
2O) drying and dehydrating
Bischofite adopts fluidized drying device 1 with chloromagnesite (MgCl
26H
2O) six most of dryings of crystal water are sloughed in, and promptly the 1mol bischofite is sloughed the crystal water of 4mol at least, makes water-content less than 27.5%.In the inventive method, the drying and dehydrating temperature is 170-220 ℃, and bischofite drying and dehydrating process does not need painstakingly to prevent hydrolysis that operating restraint is wide.
(2) underpressure distillation of magnesium chloride ethylene glycol solution dehydration
Under heated and stirred, magnesium chloride that in dissolving tank 2 step (1) is obtained and ammonium chloride are dissolved in ethylene glycol solvent and make the magnesium chloride ethylene glycol solution.The ammonium chloride add-on is the 8wt%-12wt% of base with the bischofite.
The magnesium chloride ethylene glycol solution of above-mentioned preparation is sloughed surplus water in vacuum tower 3,100-160 ℃ of temperature, vacuum tightness 500mmHg-700mmHg, the selection reflux ratio is 3:1---5:1, until the solution water content less than 1%.Carry out the vacuum distilling operation.Distillation tower can be selected periodical operation, also can select the operate continuously mode.
When selecting periodical operation, when beginning to reflux, cat head can access almost purified moisture, along with the carrying out of vacuum distilling operation, the rising gradually of trim the top of column liquid temp.Under fixing vacuum tightness operational condition, when the trim the top of column liquid temp is constant, can conclude that the moisture distillation in the solution finishes, the solution in the tower still is the ethylene glycol solution of the magnesium chloride that can be used for reactive crystallization.Also can adopt the karl Fischer method in operating process, regularly to measure the water content of solution in the tower still, thereby solution water content is less than 1% in the tower still of judgement distillation tower.
(3) reactive crystallization of magnesium chloride hex-ammoniate
Experiment shows that water-content generally should be greater than 1% in the crystalline mother solution, and the water content in the crystalline mother solution is greater than 1% o'clock, the crystalline growth and the crystal morphology of magnesium chloride hex-ammoniate is had remarkably influenced, thereby can influence the quality product of Magnesium Chloride Anhydrous.Fig. 2 is that water content is the magnesium chloride hex-ammoniate crystalline electron-microscope scanning figure that obtained in 0.2% o'clock in the crystalline mother solution, and magnesium chloride hex-ammoniate has good crystal formation, the purity height; Fig. 3 is that moisture content is the electron-microscope scanning figure of the product that obtained in 5.3% o'clock in the crystalline mother solution, visible magnesium chloride hex-ammoniate impure (the magnesium chloride hex-ammoniate crystal formation is an octahedral structure).
Step 2) the almost completely dehydration magnesium chloride ethylene glycol solution that obtains mixes with liquefied ammonia, make that crystalline mother solution, temperature drop to the suitable temp of crystallization operation after, introduce fluidized-bed crystallizer 4.Entered crystallizer by the saturated magnesium chloride ethylene glycol solution of ammonia by the top of fluidized-bed reaction crystallizer, ammonia is pressed into crystallizer by the bottom, ammonia and magnesium chloride ethylene glycol solution in wherein countercurrent flow of fluidized-bed reaction crystallization, mix, reactive crystallization.Unreacted ammonia is overflowed by the crystallizer top, can recirculation use then; The magnesium chloride hex-ammoniate crystal leaves crystallizer by bottommost, and is collected the importing strainer.
The temperature of magnesium chloride hex-ammoniate reactive crystallization is selected 10-20 ℃.
The residence time of magnesium chloride hex-ammoniate reaction crystallization process is controlled at 20-120min..
In the magnesium chloride hex-ammoniate reaction crystallization process, reactive crystallization is carried out in recycles such as liquefied ammonia, ammonia, ethylene glycol, magnesium chloride, does not almost lose, and has improved the utilization ratio of ammonia and organic solvent, has improved the productive rate of magnesium chloride.
(4) the magnesium chloride hex-ammoniate crystalline filters, washs and be dry
The magnesium chloride hex-ammoniate magma of fluidized-bed-reaction crystalizer is introduced strainer 5 filter, filtrate imports its top feed mouth recycle of crystallizer again; After filter cake washed through two to three times, fluidized bed dryer 7 remained on the 80-100 ℃ of dry down magnesium chloride hex-ammoniate that gets in temperature.
Washings is selected micromolecular alcohol for use, preferentially selects ethanol for use.Ethanol as washing at first needs by liquefied ammonia saturated.1 kilogram of magnesium chloride hex-ammoniate filter cake needs 0.8-2.5 to rise by the saturated washing with alcohol liquid of ammonia.
Contain the ethylene glycol of ethanol, dissolved ammonia, the thin crystalline substance of magnesium chloride hex-ammoniate and minute quantity in the washings, can be by the distillatory method with each separating substances, recycle then.
(5) roasting of magnesium chloride hex-ammoniate deamination prepares Magnesium Chloride Anhydrous
8 roastings of exsiccant magnesium chloride hex-ammoniate crystal process fluidized-solids roaster remove ammonia and make the Magnesium Chloride Anhydrous powder, under 400-500 ℃ of condition, keep 30-120min. to slough ammonia, the ammonia recycle of sloughing.Making the Magnesium Chloride Anhydrous powder, can directly to enter temperature be that Magnesium Chloride Anhydrous becomes liquid state, leaves standstill 30-60min. in 714-800 ℃ the melt pool, and supernatant liquid can directly import electrolyzer system magnesium, also can cool off to be prepared into block Magnesium Chloride Anhydrous.
Example 1
Get 500g bischofite (MgCl
26H
2O), drying and dehydrating under 180 ℃ of temperature, dry back weight 245g, weightless 255g.Bischofite is dry under 180 ℃ of temperature, and partial hydrolysis takes place, and it is MgCl that desciccate is formed
2H
2O and Mg (OH) Cl, wherein MgCl
2H
2O accounts for 71.2wt%.
Example 2
Bischofite sealing after 180 ℃ of dryings is preserved.Get the dried bischofite of 150g and be dissolved in the 1000ml ethylene glycol solvent, add 33g ammonium chloride simultaneously.Adopt karl-Fischer method to measure the water content of solution, measurement result shows that water content is 1.60%.The solution of preparation is presented in three mouthfuls of matrasss of 2000ml, in vacuum tightness is 660mmHg, 150 ℃ of temperature, reflux ratio are to carry out intermittent vacuum distillation dehydration operation 200min. under the 5:1 condition in distillation tower, and the water content of measuring the solution after vacuum distilling is dewatered is 0.20%.From the tower still, take out the ethylene glycol solution cooling of 800ml magnesium chloride, add 100ml liquefied ammonia, feed ammonia then, in the fluidized-bed reaction crystallizer, generate the magnesium chloride hex-ammoniate white precipitate, after it is filtered, use under 80 ℃ of environment dry 2 hours then by the saturated washing with alcohol of liquefied ammonia three times, weighing obtains 120.4g magnesium chloride hex-ammoniate crystal, and the yield of magnesium chloride is 82.7%.Crystalline electron-microscope scanning figure and XRD figure see respectively shown in accompanying drawing 2 and the accompanying drawing 4 that magnesium chloride hex-ammoniate has good crystal formation (octahedra crystalline structure).
Example 3
Get the 100g bischofite, drying directly is not dissolved in the dissolving of 1000ml ethylene glycol, adopts karl-Fischer method to measure the water content of solution, and measurement result shows that water content is 5.3%.The hydrated magnesium chloride ethylene glycol solution of preparation directly carries out reaction crystallization process without the step of vacuum distilling dehydration.Other step (reactive crystallization, filtration, washing and drying process) is identical with example 2, the crystalline electron-microscope scanning figure that the result obtains as shown in Figure 3, visible magnesium chloride hex-ammoniate impure (the magnesium chloride hex-ammoniate crystal formation is an octahedral structure).
Example 4
The magnesium chloride hex-ammoniate crystal that example 2 obtains is got 50g and is placed in the quartz glass, places by thyristor controlled electric furnace progressively to heat up under nitrogen protection.Under 450 ℃ of conditions, keep 60min. to remove ammonia; Temperature is elevated to 780 ℃, obtains the liquid anhydrous magnesium chloride, obtains block Magnesium Chloride Anhydrous after the cooling, and magnesium chloride purity is 99.6% by analysis.Fig. 5 is the magnesium chloride hex-ammoniate in-situ high temperature X-ray diffraction spectrogram of example 2 preparations, and experiment shows that magnesium chloride hex-ammoniate decomposes fully substantially at 250 ℃, has formed the Magnesium Chloride Anhydrous crystal formation at 650 ℃.
Claims (7)
1 one kinds prepare the method for Magnesium Chloride Anhydrous by bischofite, it is characterized in that: comprise step:
(1) the bischofite drying is sloughed most of crystal water;
(2) dried magnesium chloride is dissolved in the ethylene glycol solution of preparation magnesium chloride in the ethylene glycol, and employing vacuum distilling method is sloughed the moisture in the magnesium chloride ethylene glycol solution;
(3) ethylene glycol solution of the magnesium chloride after the dehydration and ammonia react crystallization generate the magnesium chloride hex-ammoniate crystal;
(4) washing, filtration, the dry magnesium chloride hex-ammoniate crystal that gets;
(5) exsiccant magnesium chloride hex-ammoniate thermolysis deamination makes Magnesium Chloride Anhydrous;
Ammonia, washing composition and crystalline mother solution recycle during the course.
2 the method for claim 1 is characterized in that: in described (1) step, bischofite by the fluidized drying technology, obtains crystal water content less than 27.5% magnesium chloride powder under temperature 170-220 ℃; Bischofite drying and dehydrating process does not need painstakingly to prevent hydrolysis, easy to operate, processing condition wide ranges.
3 the method for claim 1, it is characterized in that: in described (2) step, dried bischofite is dissolved in the ethylene glycol solution of ethylene glycol magnesium chloride, and adding with bischofite is the ammonium chloride of basic 8wt%-12wt%, to eliminate the by product that generates because of hydrolysis.
4 the method for claim 1, it is characterized in that: in described (2) step, the method for the ethylene glycol solution employing vacuum distilling of the magnesium chloride of preparation is sloughed moisture wherein, 100-160 ℃ of temperature, vacuum tightness 500mmHg-700mmHg, until the solution water content less than 1%.
5 the method for claim 1, it is characterized in that: in described (3) step, crystalline mother solution at first uses liquefied ammonia saturated, then with the ammonia counter-current operation, reaction generates the magnesium chloride hex-ammoniate crystal in the fluidized-bed reaction crystallizer, Tc is controlled at 10-20 ℃, and the residence time is controlled at 20-120min..
6 the method for claim 1 is characterized in that: the washing in described (4) step, select by the saturated ethanol of ammonia as washing composition; Under temperature 80-100 ℃ condition, to the magnesium chloride hex-ammoniate crystal drying after the washing.
7 the method for claim 1 is characterized in that: in described (5) step, exsiccant magnesium chloride hex-ammoniate crystal under 400-500 ℃ of condition, keeps 30-120min. to slough ammonia and gets Magnesium Chloride Anhydrous, the ammonia recycle of sloughing; Under temperature 714-800 ℃, Magnesium Chloride Anhydrous becomes liquid state, leaves standstill 30-60min., obtains the liquid anhydrous magnesium chloride, directly introduces electrolyzer smelting magnesium or cooling and is prepared into block Magnesium Chloride Anhydrous.
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