CN107140663A - A kind of preparation technology of epsom salt - Google Patents
A kind of preparation technology of epsom salt Download PDFInfo
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- CN107140663A CN107140663A CN201710543598.2A CN201710543598A CN107140663A CN 107140663 A CN107140663 A CN 107140663A CN 201710543598 A CN201710543598 A CN 201710543598A CN 107140663 A CN107140663 A CN 107140663A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of preparation technology of epsom salt, comprise the following steps：S1100 removal of impurities, extraction magnesium hydroxide material step：The magnesium hydroxide filter cake formed in lithium technique is carried using salt lake bittern as raw material, removal of impurities processing is carried out to the magnesium hydroxide filter cake, to extract the magnesium hydroxide material in the magnesium hydroxide filter cake, makes Cl in the magnesium hydroxide material‑Mass fraction be less than 0.01%；S1200 magnesium sulfate synthesis steps：Sulfuric acid solution is added in the magnesium hydroxide material, is 1 according to the ratio between amount of material of magnesium hydroxide and sulfuric acid：1.7~1：1.8 mixing, occur neutralization reaction and form Adlerika；S1300 crystallizations, separation, drying steps：The first body of the crystallized process formation epsom salt crystallization of Adlerika, just, through separation circuit, drying process, epsom salt crystal is made in body for the epsom salt crystallization.
Description
Technical field
The present invention relates to technical field prepared by magnesium sulfate, and in particular to one kind is produced during carrying lithium using salt lake bittern
Discarded magnesium hydroxide filter cake produce epsom salt crystal preparation technology.
Background technology
Epsom salt (molecular formula MgSO47H2O) also known as magnesium sulphate, sal amarum, epsomite, Epsom salts, are white or colourless
Needle-like or batter post shape crystalline solid, odorless, cool and slight bitter, molecular weight：246.47, proportion 1.68 is soluble in water, be slightly soluble in ethanol and
Glycerine, in 67.5 DEG C of crystallizations water for being dissolved in itself.Thermally decomposed, 70,80-85 DEG C be to lose the tetramolecular crystallization water.About 200
DEG C all crystallizations water are lost into anhydride.Easy-weathering is powdery in air (drying), and crystallization water change is gradually sloughed during heating
For anhydrous magnesium sulfate, this product is free of any poisonous impurities.Epsom salt more holds because being not easily dissolved than anhydrous magnesium sulfate
Easily weigh, be easy to the quantitative control carried out in the industry.It is mainly used in fertilizer, process hides, printing and dyeing, catalyst, papermaking, plastics, porcelain
Device, pigment, match, the manufacture of explosive and fire proofing material.Available for the thin thin cotton of printing and dyeing, silk, as staple heavy weight additive and
The filler of kapok product；Pharmaceutically it is used as Epsom salts.
Main production process has：
Method one：Magnesia (containing magnesia more than 85%) 202kg is participated in into neutralization kettle, then participates in the running water that must be measured and is mixed
And instant, start that sulfuric acid 417kg is added dropwise, first quick and back slow, until color is changed into redness of the skin or complexion from native white.Repercussion 0.5h again after drop finishes.
Neutralizer is squeezed into blade rotary vacuum filter and filtered, filtrate is squeezed into crystallizer, pH value is adjusted to 4 with sulfuric acid, participates in appropriate sulphur
Sour magnesium crystal seed is to 30 DEG C, centrifugation difference, and finished product is obtained in dull at 50~60 DEG C.
Method two：Sulfuric acid is participated in natural magnesium magnesium (magnesite), is removed after carbon dioxide, recrystallizes and obtains.By sulphur
Magnesium vanadium is dissolved in hot water recrystallization and obtained.Produced by seawater.
Method three：This method of sulfuric acid process is using dolomite, serpentine, magnesia as data.Neutralize repercussion device in participate in water or
Mother liquor, then neutralizes sulfuric acid and the magnesia containing magnesia more than 85% instead by that must match progress in progressively participation repercussion device
Ring, manipulate Ph=5, concentration is 39~40 ° of B é.30 method min are mixed and stirred, repercussion is fully carried out.Its MgO+H2SO4+6H2O→
MgSO4·7H2Neutralizer is maintained at 80-85 DEG C by O, in the filtrate feeding crystallizer after filtering, plus the appropriate crystal seed of people, then through cold
But, filter, centrifuge difference, in 50~55 DEG C of dullnesses, produce magnesium sulfate.
Method four：Mother liquor returns to be used as dispensing.It is (thick that the natural transpiration of bittern obtained in recrystallization method salt lake is condensed into crude magnesium
Magnesium sulfate).Using crude magnesium as data, add water and dissolve at 80~90 DEG C, then understood fully at a temperature of 60~70 DEG C, at 20~25 DEG C
Crystallisation by cooling, distinguish through centrifugation, it is dull, industrial sulphuric acid magnesium finished product is made.Commercial sulphuric acid magnesium is immersed into distilled water, adjusted with sulfuric acid
Ph values are spent, pharmaceutical magnesium sulfate is made through recrystallization in centrifugation difference, dull dehydration.
Method five：Seawater bittern method seawater of evaporating brine is evaporated brine to obtain bittern, with adding halogen method it is rising after, output high temperature salt, it, which is organized, becomes
It is about that 7%, KCl is about 0.5% into MgSO4 ＞ 30%, NaCI ＜ 35%, MgCl2.Bittern can use 200g/L MgCl2 solution
Molten in 48 DEG C of leachings, NaCl dissolvings are less, and MgSO4 dissolvings are more.Respectively after, immersion liquid be cooled to 10 DEG C just separate it is thick
MgSO47H2O, finished product is obtained through secondary recrystallization.
Method six：Sulfuric acid process first progressively participates in magnesia in water and mother liquor in neutralizing tank, is then neutralized with sulfuric acid, color
It is color that redness of the skin or complexion interruption is changed into from ashen, manipulate Ph=5, relative density 1.37~1.38 (39~40 ° of B é).Filtered at 80-85 DEG C
Neutralizer, then dispatches Ph values to 4 with sulfuric acid, participates in appropriate crystal seed, and be cooled to 30 DEG C of crystallizations.At 50~55 DEG C after respectively
Lower dull finished product, mother liquor is returned neutralizing tank.
Method seven：Also it can use in the sulfuric acid of low concentration and the magnesia of content of magnesia 65% and repercussion, through filtering, accumulating,
Concentration, crystallization, centrifugation difference, dullness, are made epsom salt.
Although the production technology using solid material containing magnesium as raw material is compared to the production work using liquid material containing magnesium as raw material
Skill production cost is lower, but this kind of technique can form new acid soil discarded object, therefore does not meet environmental protection theory
It is required that, belong to the technique currently eliminated.
Due to the magnesium ion containing higher concentration in salt lake bittern, substantial amounts of magnesium ion is still had in lithium technique is put forward and is existed
In lithium desorption liquid, during lithium desorption liquid is handled, generally magnesium ion is converted into magnesium hydroxide and formed through press filtration and is filtered
Cake and remove.Although magnesium hydroxide material be have in rubber and plastic industry generally acknowledged at present fire-retardant, suppression cigarette, filling triple functions it is excellent
Elegant flame retardant materials, it is contour that it is widely used in rubber, chemical industry, building materials, plastics and electronics, unsaturated polyester (UP) and paint, coating
In molecular material, but obtained magnesium hydroxide filter cake is handled in the technique that salt lake bittern carries lithium because its content is not high, knot
Crystalline form looks and dispersiveness do not meet the requirement as filler and fire retardant and would generally directly discarded, and a large amount of discarded objects are covered
Bury, not only added burial cost but also caused the wasting of resources.Accordingly, it is desirable to provide a kind of by the discarded magnesium hydroxide filter cake profit
For producing epsom salt, the problem of discarded magnesium hydroxide filter cake is buried can be solved, can effectively reduce by seven water sulphur again
The preparation cost of sour magnesium.
The content of the invention
Therefore, the present invention proposes a kind of system at least one of new epsom salt that can be solved the above problems
Standby technique.
According to an aspect of the invention, there is provided a kind of preparation technology of epsom salt, comprises the following steps：
S1100 removal of impurities, extraction magnesium hydroxide material step：The magnesium hydroxide filter cake formed in lithium technique is carried with salt lake bittern
As raw material, removal of impurities processing is carried out to the magnesium hydroxide filter cake, to extract the magnesium hydroxide in the magnesium hydroxide filter cake
Material, makes Cl in the magnesium hydroxide material-Mass fraction be less than 0.01%；
S1200 magnesium sulfate synthesis steps：Sulfuric acid solution is added in the magnesium hydroxide material, according to magnesium hydroxide and sulphur
The ratio between amount of material of acid is 1：1.7~1：1.8 mixing, occur neutralization reaction and form Adlerika；
S1300 crystallizations, separation, drying steps：The crystallized process formation epsom salt crystallization of Adlerika is just
Body, just, through separation circuit, drying process, epsom salt crystal is made in body for the epsom salt crystallization.
Alternatively, according to an embodiment of the invention, in S1100, the magnesium hydroxide filter cake remove and lived together
Reason comprises the following steps：
S1101 the first thick liquid steps of formation：Added water in the magnesium hydroxide filter cake, stir mixing, form first thick
Shape thing；
S1102 the second thick liquid steps of formation：First thick liquid is heated to 40~50 DEG C, 20~40min is stirred,
Form the second thick liquid；
S1103 the second filter cake steps of formation：Second thick liquid is through filter press to form the second filter cake；
S1104 washing steps：Using the second filter cake described in desalination water washing, so that the 3rd filter cake is formed, by the described 3rd
Filter cake is used as the magnesium hydroxide material.
Alternatively, according to an embodiment of the invention, in S1200 magnesium sulfate synthesis steps, neutralized described instead
The reaction temperature answered is controlled at 80-85 DEG C.
Alternatively, according to an embodiment of the invention, in S1300 steps, the drying process is pneumatic conveying drying, is done
Dry temperature is 50~55 DEG C, and pressure is less than 0.01MPa.
Alternatively, according to an embodiment of the invention, the sulfuric acid solution in S1200 steps is dense using mass percent
Spend the sulfuric acid for 90~98%.
Alternatively, according to an embodiment of the invention, the sulfuric acid solution in S1200 steps is the matter after recycling
Amount percent concentration is 75~95% Waste Sulfuric Acid.
Alternatively, according to an embodiment of the invention, in the Crystallization Procedure of S1300 steps, the temperature of the crystal solution
Degree control is at -1.8~48.18 DEG C.
Alternatively, according to an embodiment of the invention, the Crystallization Procedure in step S1300 is crystallisation by cooling,
Crystal solution in the crystallisation by cooling is cooled to 25~35 DEG C, and the separation circuit is centrifugation.
The preparation technology for the epsom salt that the present invention is provided can solve asking for discarded magnesium hydroxide filter cake burial
Topic, can effectively reduce the preparation cost of epsom salt, meet the theory of green circulation economy again.
Brief description of the drawings
By reading the detailed description of hereafter preferred embodiment, various other advantages and benefit is common for this area
Technical staff will be clear understanding.Accompanying drawing is only used for showing the purpose of preferred embodiment, and is not considered as to the present invention
Limitation.And in whole accompanying drawing, identical part is denoted by the same reference numerals.Wherein in the accompanying drawings, reference numeral
Alphabetic flag afterwards indicates multiple identical parts, when referring to these parts, will omit its last alphabetic flag.Attached
In figure：
Fig. 1 shows the preparation technology of the epsom salt of a preferred embodiment of the invention.And
Fig. 2 show a preferred embodiment of the invention to the magnesium hydroxide filter cake carry out removal of impurities processing
The step of.
Embodiment
The invention provides many applicable creative concepts, the creative concept can be reflected in a large number of on specific
Hereinafter.Specific embodiment described in following embodiments of the present invention is only as embodiment of the invention
Exemplary illustration, and be not meant to limit the scope of the invention.
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
According to Fig. 1, the invention provides a kind of preparation technology of epsom salt, comprise the following steps：
S1100 removal of impurities, extraction magnesium hydroxide material step：The magnesium hydroxide filter cake formed in lithium technique is carried with salt lake bittern
As raw material, removal of impurities processing is carried out to the magnesium hydroxide filter cake, to extract the magnesium hydroxide in the magnesium hydroxide filter cake
Material, makes Cl in the magnesium hydroxide material-Mass fraction be less than 0.01%.
Salt lake bittern puies forward lithium technique and refers to the process of extract lithium ion, the work using multistep process by raw material of salt lake bittern
Skill is well known to those skilled in the art, therefore will not be described in detail herein.
Due to containing substantial amounts of magnesium ion in salt lake bittern, in order to improve the purity of final lithium-containing compound, usual need pair
Magnesium ion in salt lake bittern, which is realized, to be removed, and the processing procedure to magnesium ion is to be handled to raw material salt lake bittern or through preliminary removal of impurities
Aqueous slkali is added in salt lake bittern afterwards, aqueous slkali is usually sodium hydroxide solution or potassium hydroxide solution, with anti-with magnesium ion
Magnesium hydrate precipitate should be formed, the magnesium hydroxide filter cake in the present embodiment is then made in filtering.
In the magnesium hydroxide filter cake, main matter is magnesium hydroxide, also containing partial oxidation sodium and a small amount of unreacted magnesium
The chlorination magnesium addition that ion is formed, therefore, the present embodiment realize that removal of impurities is handled to the magnesium hydroxide filter cake first.It should remove and live together
Reason can be using removal of impurities modes such as multistep washing and filterings, it is preferable that difference of the present embodiment by magnesium hydroxide and impurity in water
Solubility is handled it, the efficient quick and good impurity removing effect of the removal of impurities processing procedure.
Preferably, in S1100, removal of impurities processing is carried out to the magnesium hydroxide filter cake and is comprised the following steps：According to Fig. 2 institutes
Show, initially enter S1101 the first thick liquid steps of formation：Added water in the magnesium hydroxide filter cake, stir mixing, form first
Thick liquid.
Preferably, for the ease of the control of finishing operations, the mass fraction of the first thick liquid reclaimed water is 60~80%.
Enter S1102 the second thick liquid steps of formation afterwards：First thick liquid is heated to 40~50 DEG C, stirring 20
~40min, forms the second thick liquid.In this step, mode of heating is preferably steam heating, passes through the steam point set in equipment
Cloth device, to realize the heating to material in equipment, so that heating process is more economical and simple, for the control of temperature
It is more convenient.The feed temperature of first thick liquid remains 40~50 DEG C, if being in crystalline because temperature is too low, in filter cake
The sodium chloride and magnesium chloride of formula are difficult to be dissolved into liquid phase rapidly, and if temperature is too high, not only waste heat energy, and can be to rear
In phase step press filtration operation make troubles, easily cause operator scald, meanwhile, in the temperature range, sodium chloride it is molten
Xie Du is close to maximum, and therefore, control of the present embodiment to feed temperature can realize preferable impurity-eliminating effect, and after being beneficial to
The progress of continuous step.
Subsequently enter S1103 the second filter cake steps of formation：Second thick liquid is through filter press to form the second filter cake.Pressure
Filter is a kind of conventional solid-liquid separating equipment of chemical industry, and it is to utilize special filter medium, and one is applied to filtering object
A kind of fixed pressure so that plant equipment that liquid dialysis comes out.Specifically, the filter press in the present embodiment uses sheet frame
Filter press.
In order to further lift the purity of magnesium hydroxide in the second filter cake, the second filter cake is washed using industry water,
Further to reduce the content of chlorion in the second filter cake, so that the 3rd filter cake is made, the 3rd filter cake is used as magnesium hydroxide
Material, can further lift the purity of the water magnesium sulfate crystal of end-product six obtained by the later stage.Therefore, after S1103 steps,
Into S1104 the 3rd filter cake steps of formation：Using the second filter cake described in desalination water washing, so that the 3rd filter cake is formed, will be described
3rd filter cake is used as the magnesium hydroxide material.
S1200 magnesium sulfate synthesis steps：Sulfuric acid solution is added in the magnesium hydroxide material, according to magnesium hydroxide and sulphur
The ratio between amount of material of acid is 1：1.7~1：1.8 mixing, occur neutralization reaction and form Adlerika.The reaction equation of this reaction
For：According to reaction equation：Mg(HO)2+H2SO4=MgSO4+2H2O。
Preferably, in S1200 magnesium sulfate synthesis steps, the reaction temperature of the neutralization reaction is controlled 80~85
DEG C, when the pH value of the Adlerika of formation is 5, then above-mentioned neutralization reaction terminates.
During above-mentioned neutralization reaction occurs, if reaction temperature is too low, the viscosity of reaction solution is larger, if conversely, anti-
Answer temperature too high, then when meeting or exceeding the boiling point of reaction solution, with the evaporation of solvent, the viscosity of reaction solution can equally increase,
And if reaction fluid viscosity is too big in the present embodiment, the viscosity that reaction terminates the Adlerika formed is also very big, in the later stage
The more mother liquor for being difficult to remove can be sticked in Crystallization Procedure, on the outer surface of the magnesium sulfate crystals of formation, is unfavorable for the later stage to sulphur
The processing of sour magnesium crystal, can also reduce the purity of final product epsom salt crystal.It is therefore preferred that reaction solution will be controlled
Temperature be 80-85 DEG C, now reaction solution is that the viscosity of reaction solution is minimum close to the state of boiling, in Crystallization Procedure, can be had
Effect reduces the content of the sodium chloride adhered on crystalline solid and magnesium chloride, so that the purity of epsom salt crystal is improved, and it is more sharp
In the progress of drying process.
Specifically, because the neutralization reaction in this step is exothermic reaction, the present embodiment is used sets folder on reactor
Set, uses and allows cooling water by way of chuck to control the reaction temperature in this step.
This step is in neutralization reaction terminal, and the pH value of the Adlerika formed is 5, because, when pH value is less than this
During scope, show that solution has free sulfuric acid, and when pH value is higher than this scope, be unfavorable for the place of later stage epsom salt
Reason.
The sulfuric acid solution used in above-mentioned neutralization reaction use mass percent concentration for 90~98% sulfuric acid, in addition,
Experiments verify that, the mass percent concentration that the sulfuric acid is alternatively after recycling is 75~95% Waste Sulfuric Acid, can equally be reached
To the purpose of the present embodiment.
Preferably, the sulfuric acid solution in S1200 steps use mass percent concentration for 90~98% sulfuric acid.
Preferably, the sulfuric acid solution in S1200 steps is 75~95% for the mass percent concentration after recycling
Waste Sulfuric Acid.
S1300 crystallizations, separation, drying steps：The crystallized process formation epsom salt crystallization of Adlerika is just
Body, just, through separation circuit, drying process, epsom salt crystal is made in body for the epsom salt crystallization.
For the crystallization beneficial to epsom salt, by adding seven appropriate water into Adlerika in Crystallization Procedure
Magnesium sulfate crystal seed, and cause Adlerika to be cooled to 25~35 DEG C or so, so as to constantly form seven water in Adlerika
The first body of magnesium sulfate crystallization.Separated using centrifugal separation process so as to which epsom salt is crystallized into just body, after separation circuit
Liquid can be discharged or returned it in reactor, then participate in neutralization reaction.
It is noted that the various operating modes of the first body of crystallization are formed in crystallization process with reference to magnesium sulfate, it is full in magnesium sulfate
In solution, it can crystallize out and be respectively provided with 1, the crystalline hydrate thing of 2,3,4,5,6,12 water, in -3.9~1.8 DEG C of saturation waters
In solution, ten sulfate dihydrate magnesium are separated out, in -1.8~48.18 DEG C of saturated aqueous solutions, epsom salt are separated out, 48.1~
In 67.5 DEG C of saturated aqueous solutions, six water magnesium sulfates are separated out, magnesium sulfate monohydrate is separated out during higher than 67.5 DEG C, it is therefore preferred that in order to
The formation of other crystals is avoided, the temperature control of crystal solution is at -1.8~48.18 DEG C.It is highly preferred that by the temperature of crystal solution
Control is at 25~35 DEG C.
Preferably, in S1300 steps, the drying process is pneumatic conveying drying, and drying temperature is 50~55 DEG C, and pressure is less than
0.01MPa。
Just body realizes drying process by the way of pneumatic conveying drying to it for isolated epsom salt crystallization, and air-flow is done
Dry mode is to disperse scattered particulate solid material to be suspended in velocity heated gas, one kind side being dried under Geldart-D particle
Method.
This step is during pneumatic conveying drying, and drying temperature control is 50~55 DEG C, and pressure is less than 0.01MPa.Properly
Drying temperature can improve the discharging purity of epsom salt crystal.If drying temperature is less than the design temperature in the present embodiment,
Then it is insufficient to allow the moisture of the first external surface of epsom salt crystallization thorough by evaporation, and if drying temperature is higher than in the present embodiment
Design temperature, then causing epsom salt crystallization again, just body removes partially crystallizable water during drying, and at this
During easily cause epsom salt crystallization just body melt be liquid, cause drying process not to be normally carried out.
Preferably, in S1300 steps, the separation circuit is centrifugation.
Embodiment 1
According to Fig. 1, a kind of preparation technology of epsom salt initially enters S1100 removal of impurities, extracts magnesium hydroxide thing
Expect step：The magnesium hydroxide filter cake formed in lithium technique is carried using salt lake bittern and is used as raw material.In wherein S1100, to the hydrogen-oxygen
Change the progress removal of impurities processing of magnesium filter cake to comprise the following steps：According to Fig. 2, S1101 the first thick liquid steps of formation are initially entered：
Added water in the magnesium hydroxide filter cake, stir mixing, form the first thick liquid；S1102 the second thick liquid steps of formation：By institute
State the first thick liquid and be heated to 40 DEG C, stir 20min, form the second thick liquid；S1103 the second filter cake steps of formation：Described
Two thick liquids are through filter press to form the second filter cake；S1104 the 3rd filter cake steps of formation：Using the second filter described in desalination water washing
Cake, so as to form the 3rd filter cake, the 3rd filter cake is used as the magnesium hydroxide material.By above-mentioned to the hydrogen-oxygen
Change the removal of impurities processing of magnesium filter cake, extract the magnesium hydroxide material in the magnesium hydroxide filter cake, make the magnesium hydroxide material
Middle Cl-Mass fraction be less than 0.01%.
Subsequently into S1200 magnesium sulfate synthesis steps：Sulfuric acid solution is added in the magnesium hydroxide material, according to hydrogen-oxygen
It is 1 to change the ratio between amount of material of magnesium and sulfuric acid：1.7 mixing, occur neutralization reaction and form Adlerika.Wherein, neutralization reaction
Reaction temperature control at 80 DEG C.Sulfuric acid solution for recycling after mass percent concentration be 75% Waste Sulfuric Acid.
Finally enter S1300 crystallizations, separation, drying steps：Seven water sulfuric acid of the crystallized process formation of Adlerika
The first body of magnesium crystallization, just body is centrifuged process, drying process for the epsom salt crystallization, and epsom salt crystal is made.
Wherein, in Crystallization Procedure, the temperature control of the crystal solution is at 25 DEG C.The separation circuit is centrifugation；The back tender
Sequence is pneumatic conveying drying, and drying temperature is 50 DEG C, and pressure is less than 0.01MPa.
Embodiment 2
According to Fig. 1, a kind of preparation technology of epsom salt initially enters S1100 removal of impurities, extracts magnesium hydroxide thing
Expect step：The magnesium hydroxide filter cake formed in lithium technique is carried using salt lake bittern and is used as raw material.In wherein S1100, to the hydrogen-oxygen
Change the progress removal of impurities processing of magnesium filter cake to comprise the following steps：According to Fig. 2, S1101 the first thick liquid steps of formation are initially entered：
Added water in the magnesium hydroxide filter cake, stir mixing, form the first thick liquid；S1102 the second thick liquid steps of formation：By institute
State the first thick liquid and be heated to 50 DEG C, stir 40min, form the second thick liquid；S1103 the second filter cake steps of formation：Described
Two thick liquids are through filter press to form the second filter cake；S1104 the 3rd filter cake steps of formation：Using the second filter described in desalination water washing
Cake, so as to form the 3rd filter cake, the 3rd filter cake is used as the magnesium hydroxide material.By above-mentioned to the hydrogen-oxygen
Change the removal of impurities processing of magnesium filter cake, extract the magnesium hydroxide material in the magnesium hydroxide filter cake, make the magnesium hydroxide material
Middle Cl-Mass fraction be less than 0.01%.
Subsequently into S1200 magnesium sulfate synthesis steps：Sulfuric acid solution is added in the magnesium hydroxide material, according to hydrogen-oxygen
It is 1 to change the ratio between amount of material of magnesium and sulfuric acid：1.8 mixing, occur neutralization reaction and form Adlerika.Wherein, neutralization reaction
Reaction temperature control at 85 DEG C.Sulfuric acid solution for recycling after mass percent concentration be 95% Waste Sulfuric Acid.
Finally enter S1300 crystallizations, separation, drying steps：Seven water sulfuric acid of the crystallized process formation of Adlerika
The first body of magnesium crystallization, just body is centrifuged process, drying process for the epsom salt crystallization, and epsom salt crystal is made.
Wherein, in Crystallization Procedure, the temperature control of the crystal solution is at 35 DEG C.The separation circuit is centrifugation；The back tender
Sequence is pneumatic conveying drying, and drying temperature is 50 DEG C, and pressure is less than 0.01MPa.
Embodiment 3
A kind of preparation technology of epsom salt according to Fig. 1, initially enters S1100 removal of impurities, extracts magnesium hydroxide thing
Expect step：The magnesium hydroxide filter cake formed in lithium technique is carried using salt lake bittern and is used as raw material.In wherein S1100, to the hydrogen-oxygen
Change the progress removal of impurities processing of magnesium filter cake to comprise the following steps：According to Fig. 2, S1101 the first thick liquid steps of formation are initially entered：
Added water in the magnesium hydroxide filter cake, stir mixing, form the first thick liquid；S1102 the second thick liquid steps of formation：By institute
State the first thick liquid and be heated to 45 DEG C, stir 25min, form the second thick liquid；S1103 the second filter cake steps of formation：Described
Two thick liquids are through filter press to form the second filter cake；S1104 the 3rd filter cake steps of formation：Using the second filter described in desalination water washing
Cake, so as to form the 3rd filter cake, the 3rd filter cake is used as the magnesium hydroxide material.By above-mentioned to the hydrogen-oxygen
Change the removal of impurities processing of magnesium filter cake, extract the magnesium hydroxide material in the magnesium hydroxide filter cake, make the magnesium hydroxide material
Middle Cl-Mass fraction be less than 0.01%.
Subsequently into S1200 magnesium sulfate synthesis steps：Sulfuric acid solution is added in the magnesium hydroxide material, according to hydrogen-oxygen
It is 1 to change the ratio between amount of material of magnesium and sulfuric acid：1.75 mixing, occur neutralization reaction and form Adlerika.Wherein, neutralization reaction
Reaction temperature control at 82 DEG C.Sulfuric acid solution for recycling after mass percent concentration be 80% Waste Sulfuric Acid.
Finally enter S1300 crystallizations, separation, drying steps：Seven water sulfuric acid of the crystallized process formation of Adlerika
The first body of magnesium crystallization, just body is centrifuged process, drying process for the epsom salt crystallization, and epsom salt crystal is made.
Wherein, in Crystallization Procedure, the temperature control of the crystal solution is at 40 DEG C.It is highly preferred that the crystal solution quilt in the crystallisation by cooling
It is cooled to 30 DEG C.The separation circuit is centrifugation；The drying process is pneumatic conveying drying, and drying temperature is 52 DEG C, pressure
Less than 0.01MPa.
Epsom salt crystal can directly be prepared according to the embodiment 1-3 preparation technologies provided, and preparation technology is saved significantly
Spent heat energy is saved.The preparation technology for the epsom salt that the present invention is provided can not only produce seven water sulphur best in quality
Sour magnesium crystal, use suitable for industry and agriculturally, and also the preparation technology of epsom salt produced by the invention utilizes salt lake
Bittern carries the discarded object magnesium hydroxide filter cake in lithium production process, solves the problems, such as the burial of the discarded object magnesium hydroxide filter cake,
And the preparation cost of epsom salt crystal is effectively saved, meanwhile, the preparation technology of epsom salt provided by the present invention,
Process is simple, and power consumption is few, meets the theory of green circulation economy.
The preparation-obtained epsom salt crystal of technique that the present invention is provided, its white in appearance or colourless crystallization particle
Or powder, the mass fraction of epsom salt is 99.0~99.5%, and the mass fraction of water-insoluble is 0.005~0.01%,
The mass fraction of chloride is 0.01~0.02%, and the mass fraction of iron ion is less than 0.001%, heavy metal mass fraction (with
Pb is counted) it is less than 0.001%.
The preparation technology for the epsom salt that the present embodiment is provided carries the hydrogen-oxygen discarded in lithium technique using salt lake bittern
Change magnesium filter cake as raw material, relative to the preparation technology of traditional epsom salt crystal, be effectively saved raw material into
This, concrete analysis process is as follows：
The calculating of raw material is on the basis of producing 1t epsom salts in following two technique.
1. the calculating of raw material in the present embodiment technique
Reaction equation is as follows：
It is computed, X=58/246=0.234t Y=98/246=0.398t
Raw material sulphuric acid solution used in the technique that the present invention is provided is the work that mass percent concentration is 75~98%
Industry sulfuric acid, if being calculated by 98%, the acid amount consumed is：0.398/0.98=0.406t.
Magnesium hydroxide raw material used in the technique that the present invention is provided carries the magnesium hydroxide discarded in lithium technique for salt lake
Filter cake, the content of its general solid magnesium hydroxide is 40~60% (content of butt magnesium hydroxide is generally 80~90%), if
Calculated by 85%, then the required discarded object quality containing magnesium hydroxide is：0.234/0.85=0.275t.
2. the calculating of raw material in traditional handicraft
According to chemical industry standard HG/T 2680-95, reaction equation is as follows：
According to can be calculated：
X=40/246=0.162t Y=98/246=0.398t
Raw material sulphuric acid solution used in this technique is the industrial sulphuric acid that mass percent concentration is 75~98%, if pressing
98% calculates, then the acid amount consumed is：0.398/0.98=0.406t
The technique that the present invention is provided compares with traditional handicraft, and the consumption of sulfuric acid is 0.406t, the work of the present embodiment
The magnesium raw material that skill is utilized is discarded object, therefore is not counted in the consumption of raw material, and traditional handicraft need to consume 0.162t oxygen
Change magnesium, and the magnesia is outsourcing or calcining generation, therefore, the cost of raw material of traditional handicraft is significantly higher than in the present embodiment
The cost of raw material of technique.
Meanwhile, by analysis, the preparation technology that the present invention is provided can directly prepare epsom salt crystal, and traditional
Method uses using solid material containing magnesium as raw material in order to save cost and prepares magnesia, after it is anti-with sulfuric acid by magnesia
Evaporating, concentrating and crystallizing separation should need to be used when extracting epsom salt crystal dry so as to produce the technique of epsom salt crystal
The process such as dry, it is similar to the technique in the present embodiment, therefore the energy contrast consumed can be based on the technique before magnesium sulfate generation
To consider, the present invention only heats the first thick liquid to consuming heat at 40~50 DEG C before magnesium sulfate generation in step S1101
Amount, other steps carry out at normal temperatures, and production technology of the conventional method using solid material containing magnesium as raw material need to first to containing
The ore of magnesium carbonate is calcined, and magnesium carbonate therein is converted into magnesia, and the heat needed for calcining is very big, is far longer than
Spent heat in the present invention.By above-mentioned analysis, the preparation technology of the epsom salt in the present embodiment is greatlyd save
Spent heat energy.
Therefore, the preparation technology for the epsom salt that the present invention is provided can not only produce epsom salt best in quality
Crystal, use suitable for industry and agriculturally, and also the preparation technology of epsom salt produced by the invention utilizes salt lake bittern
The discarded object magnesium hydroxide filter cake in lithium production process is carried, the burial of the discarded object magnesium hydroxide filter cake is solved the problems, such as, and had
Effect saves the preparation cost of epsom salt crystal, meanwhile, the preparation technology of epsom salt provided by the present invention, process
Simply, consume energy few, meet the theory of green circulation economy.
It should be noted that the present invention will be described rather than limits the invention for above-described embodiment, and this
Art personnel can design alternative embodiment without departing from the scope of the appended claims.In claim
In, any reference symbol between bracket should not be configured to limitations on claims.Word "comprising" is not excluded for depositing
In element or step not listed in the claims.Word "a" or "an" before element do not exclude the presence of it is multiple this
The element of sample.The use of word first, second, and third does not indicate that any order.These words can be construed to title.
Claims (9)
1. a kind of preparation technology of epsom salt, comprises the following steps：
S1100 removal of impurities, extraction magnesium hydroxide material step：Carried using salt lake bittern the magnesium hydroxide filter cake that is formed in lithium technique as
Raw material, removal of impurities processing is carried out to the magnesium hydroxide filter cake, to extract the magnesium hydroxide material in the magnesium hydroxide filter cake,
Make Cl in the magnesium hydroxide material-Mass fraction be less than 0.01%；
S1200 magnesium sulfate synthesis steps：Sulfuric acid solution is added in the magnesium hydroxide material, according to magnesium hydroxide and sulfuric acid
The ratio between amount of material is 1：1.7~1：1.8 mixing, according to reaction equation：Mg(HO)2+H2SO4=MgSO4+2H2O, in generation
Adlerika is formed with reaction；
S1300 crystallizations, separation, drying steps：The first body of the crystallized process formation epsom salt crystallization of Adlerika, institute
Stating epsom salt crystallization, just, through separation circuit, drying process, epsom salt crystal is made in body.
2. the preparation technology of epsom salt according to claim 1, wherein, in S1100, to the magnesium hydroxide filter cake
Removal of impurities processing is carried out to comprise the following steps：
S1101 the first thick liquid steps of formation：Added water in the magnesium hydroxide filter cake, stir mixing, form the first thick liquid；
S1102 the second thick liquid steps of formation：First thick liquid is heated to 40~50 DEG C, 20~40min is stirred, is formed
Second thick liquid；
S1103 the second filter cake steps of formation：Second thick liquid described in press filtration is to form the second filter cake；
S1104 the 3rd filter cake steps of formation：Using the second filter cake described in desalination water washing, so that the 3rd filter cake is formed, will be described
3rd filter cake is used as the magnesium hydroxide material.
3. the preparation technology of epsom salt according to claim 1, will be described in S1200 magnesium sulfate synthesis steps
The reaction temperature of neutralization reaction is controlled at 80-85 DEG C.
4. in the preparation technology of epsom salt according to claim 1, S1300 steps, the drying process is air-flow
Dry, drying temperature is 50~55 DEG C, and pressure is less than 0.01MPa.
5. the sulfuric acid solution in the preparation technology of epsom salt according to claim 1, S1200 steps uses quality hundred
Divide the sulfuric acid that specific concentration is 90~98%.
6. the sulfuric acid solution in the preparation technology of epsom salt according to claim 1, S1200 steps is recycling
Mass percent concentration afterwards is 75~95% Waste Sulfuric Acid.
7. in the preparation technology of epsom salt according to claim 1, the Crystallization Procedure of S1300 steps, the crystallization
The temperature control of liquid is at -1.8~48.18 DEG C.
8. the Crystallization Procedure in the preparation technology of epsom salt according to claim 7, step S1300 is cooling
Crystal solution in crystallization, the crystallisation by cooling is cooled to 25~35 DEG C.
9. it is described in the preparation technology of the epsom salt according to any one in claim 1~8, step S1300
Separation circuit is centrifugation.
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| CN111135773A (en) * | 2020-01-03 | 2020-05-12 | 河北佰斯特药业有限公司 | Method for removing iron and manganese in raw material medicine magnesium sulfate |
| CN115159579A (en) * | 2022-08-01 | 2022-10-11 | 贵州金瑞新材料有限责任公司 | Method for deeply separating calcium and magnesium impurities in manganese sulfate |
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