CN106395867B - A kind of method that high-purity six water magnesium sulfate is extracted from bittern - Google Patents
A kind of method that high-purity six water magnesium sulfate is extracted from bittern Download PDFInfo
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- CN106395867B CN106395867B CN201610795499.9A CN201610795499A CN106395867B CN 106395867 B CN106395867 B CN 106395867B CN 201610795499 A CN201610795499 A CN 201610795499A CN 106395867 B CN106395867 B CN 106395867B
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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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to the production technology of high-purity six water magnesium sulfate, a kind of method that high-purity six water magnesium sulfate is extracted from bittern is particularly belonged to.Described method flow is the component in salt pond using old halogen, bischofite or saltcake regulation bittern, gypsum is added in bittern and settled, then bittern natural evaporation under sunshine condition is made, the salt of bittern after being evaporated to a certain degree and deposition is transported in heating response kettle, separation of solid and liquid after temperature control stirring, liquid phase bittern is incubated, finally takes its salt separated out to be dehydrated, obtains six high-purity water magnesium sulfates.The method have the characteristics that directly extracting six high-purity water magnesium sulfates from bittern, eliminate dissolving and the refined link recrystallized, avoid using mechanical vapor equipment so that technique is simple and direct, energy-efficient, it is easy to industrialized production.
Description
Technical field
The present invention relates to the production technology of high-purity six water magnesium sulfate, particularly belong to one kind and high-purity six water sulphur is extracted from bittern
The method of sour magnesium.
Background technology
Sulfuric acid a set of magnesium products can be obtained using the method for salt pan natural evaporation bittern, but purity is relatively low, its product master
If epsom salt crystal salt.High-purity magnesium sulfate class product of the purity more than 99% generally by crude magnesium product again
It is secondary it is refined obtained from, typical technique is dissolving and recrystallization.Crude magnesium product is obtained by Bittern of Salt Pan evaporation, its quilt
Course of dissolution when refined is carried out under conditions of generally requiring more than 60 DEG C, and it also requires clarifying one section under heat-retaining condition
Time, then evaporate and crystallize in the environment more than 45 DEG C, obtained product is mainly six water magnesium sulfates.Due to subtractive process
Need to use heater meanses and forced evaporation equipment, it is desirable to provide energy be used for a large amount of gasification latent heats consumption, therefore energy consumption and
Equipment cost is higher, and operation and technology controlling and process are also more complicated, and this causes the production cost of high-purity magnesium sulfate type products to compare
It is high.
Therefore, when preparing the high-purity magnesium sulfate class product of purity >=99%, it is necessary to take into account technically innovated
And improvement.According to these states of the art, it may be considered that directly extract six high-purity water magnesium sulfates from bittern, omit dissolving crude magnesium and
Recrystallizing and refining link, the technique that simplifies, and make full use of solar energy source come the condensing crystallizing for bittern, avoid using pressure
The equipment of evaporation is to be effectively reduced energy consumption.
The content of the invention
It is an object of the invention to provide a kind of method that high-purity six water magnesium sulfate is extracted from bittern, this method can be from halogen
Six high-purity water magnesium sulfates are directly extracted in water, tradition can be omitted and prepare high-purity six water magnesium sulfate and use and dissolve and recrystallize
Refined link, and avoid use mechanical vapor equipment.
The present invention is achieved through the following technical solutions.
A kind of method that high-purity six water magnesium sulfate is extracted from bittern that the present invention is provided, comprises the following steps：
A) bittern is poured into salt pond, Mg in detection bittern2+And SO4 2-Deng the mass content of two kinds of ions, control in bittern
Mass of ion compares Mg2+:SO4 2-=1:1.20-1.91, if mass ratio Mg2+:SO4 2-<1:1.91 add into bittern and contain
If the old halogen or bischofite of magnesium chloride component, mass ratio Mg2+:SO4 2->1:1.20 add sulfur acid sodium group into bittern
Point saltcake, afterwards bittern stand 24-72 hours and shovel out the carnallite of bittern bottom deposit；
B) the gypsum consumption being equably sprinkled into bittern in the gypsum for being ground to 100-200 mesh, every cubic metre of bittern is
1-10 kilograms, continue standing sedimentation 24-72 hours, then shovel out the miscellaneous mud of bittern bottom deposit；
C) make bittern natural evaporation under sunshine condition, moisture is gradually steamed and monitor Na in bittern+And SO4 2-Two kinds
The mass content change of ion, as bittern intermediate ion mass ratio Na+:SO4 2-=1:2.25-2.70 when shovel out bittern bottom deposit
Carnallite and miscellaneous mud；
D) natural evaporation is then proceeded to, when bittern intermediate ion mass ratio reaches Na+:SO4 2-=1:During 2.71-4.34, collect
It is simultaneously transported in heating response kettle by carnallite that bittern bottom is deposited again together with bittern；
E) in heating response kettle, control bittern and carnallite mixture temperature is between 45-55 DEG C and to stir 4-6 small
When, then separate and discharge the carnallite of heating response kettle bottom deposit；
F) brine temperature is reduced to 20-35 DEG C in heating response kettle and is incubated 6-36 hours；
G) bittern in heating response kettle is discharged, the salt for now separating out and depositing again in heating response kettle, warp is collected
High-purity six water magnesium sulfate is obtained after centrifugal dehydration, drying.
The bittern that above-mentioned steps a) pours into salt pond should be Na+,K+,Mg2+//Cl-,SO4 2--H2O salt-water system type bittern, and
And the mass ratio Cl of bittern intermediate ion-:Na+=1:0.16-0.57, mass ratio K+:Na+<1:20。
Advantage of the invention is that technique is simple, easily operated；Steamed due to being not present in the operational phase of heating response kettle
Hair ring section, so the consumption of gasification latent heat is also not present, therefore energy of the invention compared with conventional six water magnesium sulfate process for refining
Consumption is greatly lowered；The thermal source of heating response kettle can be from solar pond, solar thermal collector, underground heat, industrial exhaust heat,
The heat energy of the various grades such as Industrial Boiler, energy-saving benefit is notable；Crude magnesium salt is prepared with conventional salt pan and prepared by recrystallizing and refining
The technology of six water magnesium sulfates or epsom salt is compared, and the present invention can omit dissolving and recrystallization link, from bittern directly
High-purity six water magnesium sulfate is extracted, is significantly simplified and shortens technological process, and improves the added value of production process；From heating
The bittern discharged in reactor can still return to that conventional day solar salt flow is continued with salt pond is therein various to extract
Inorganic salts, or be cyclically back to be mixed into salt pond and convert the effect of halogen to play, can also on the basis of production high purity product
Enough be effectively prevented from the waste of material, on the basis of conventional Solar pond production obtain high purity product income.
To sum up, flow of the present invention is simple and direct, be capable of high-purity product salt of output high added value, and power savings advantages are substantially, in fact
It is strong with property.
Embodiment
By the following specific examples further illustrate the invention.
Embodiment 1：
Bittern is derived from the seawater in Hebei province Qinhuangdao marine site.The bittern belongs to Na+,K+,Mg2+//Cl-,SO4 2--H2O water
Salt system type bittern, and in bittern leading ion mass content Na+For 1.08%, K+For 0.04%, Mg2+For 0.13%,
Cl-For 1.94%, SO4 2-For the mass ratio Cl of 0.27%, i.e. ion-:Na+=1:0.56th, mass ratio K+:Na+=1:27.
High-purity six water magnesium sulfate is extracted from the bittern, salt pond conventional in salt industry and Chemical Manufacture and heating response is used
Kettle, comprises the following steps：
A) bittern is poured into salt pond, Mg in detection bittern2+And SO4 2-Deng the mass content of two kinds of ions, bittern intermediate ion
Mass ratio Mg2+:SO4 2-=1:2.08, i.e. mass ratio Mg2+:SO4 2-<1:1.91, then it is mixed into bittern containing magnesium chloride component
Bischofite, make bittern intermediate ion mass ratio control in Mg2+:SO4 2-=1:1.90, afterwards bittern stand and 36 hours and shovel out
The carnallite of bittern bottom deposit；
B) the gypsum consumption being equably sprinkled into bittern in the gypsum for being ground to 160-200 mesh, every cubic metre of bittern is 1
Kilogram, continue standing sedimentation 36 hours, then shovel out the miscellaneous mud of bittern bottom deposit；
C) make bittern natural evaporation under sunshine condition, moisture is gradually steamed and monitor Na in bittern+And SO4 2-Deng two
Plant the mass content change of ion；
D) as bittern intermediate ion mass ratio Na+:SO4 2-=1:The carnallite miscellaneous mud of bittern bottom deposit is shoveled out when 2.50, then
Continuing natural evaporation makes bittern intermediate ion mass ratio reach Na+:SO4 2-=1:3.01, collect now bittern bottom and deposit again
Carnallite and be transported to together with bittern in heating response kettle；
E) in heating response kettle, control bittern and carnallite mixture temperature between 50 DEG C and stir 4 hours, then
Separate and discharge the carnallite of heating response kettle bottom deposit；
F) brine temperature is reduced to 30 DEG C in heating response kettle and is incubated 30 hours；
G) bittern in heating response kettle is discharged, the salt for now separating out and depositing again in heating response kettle, warp is collected
High-purity six water magnesium sulfate is obtained after centrifugal dehydration and drying.
2 kilograms of high-purity six water magnesium sulfate can be finally made in the bittern of raw material per ton in step a), equivalent to magnesium in bittern
The rate of recovery of element is 16% or so, and resulting high-purity six water magnesium sulfates purity has reached 99.9%, from heating response kettle
The bittern discharged, which is returned in salt pond, to be continued with conventional day solar salt flow to extract various inorganic salts therein.
Embodiment 2
Method flow is same as Example 1, Shanxi Province Yuncheng when difference is to be derived from spring as the bittern of raw material
The bittern shone in salt pond in salt lake, the bittern belongs to Na+,K+,Mg2+//Cl-,SO4 2--H2O salt-water system type bittern, and bittern
The mass content Na of middle leading ion+For 0.26%, K+For 0, Mg2+For 0.59%, Cl-For 1.61%, SO4 2-For 0.71%, i.e.,
The mass ratio Cl of ion-:Na+=1:0.16th, mass ratio K+:Na+=0；The bittern intermediate ion mass ratio Mg of raw material2+:SO4 2-=1:
1.19, i.e. mass ratio Mg2+:SO4 2->1:1.20, therefore the saltcake of sulfur acid sodium component is mixed into bittern so that halogen in step a)
Water intermediate ion mass ratio is controlled in Mg2+:SO4 2-=1:1.21.
6.2 kilograms of high-purity six water magnesium sulfate can be finally made in the bittern of raw material per ton in step a), equivalent in bittern
The rate of recovery of magnesium elements is 11% or so, and resulting high-purity six water magnesium sulfates purity has reached 99.6%, from heating response kettle
In the bittern that discharges return in salt pond and continue with conventional day solar salt flow to extract various inorganic salts therein.
Embodiment 3
Method flow is same as Example 1, and difference is to be derived from Yuncheng salt lake as the bittern of raw material
In bittern, the bittern belongs to Na+,K+,Mg2+//Cl-,SO4 2--H2O salt-water system type bittern, and leading ion in bittern
Mass content Na+For 4.44%, K+For 0, Mg2+For 3.92%, Cl-For 12.38%, SO4 2-For the mass ratio of 7.98%, i.e. ion
Cl-:Na+=1:0.36th, mass ratio K+:Na+=0；The bittern intermediate ion mass ratio Mg of raw material2+:SO4 2-=1:2.04, i.e. quality
Compare Mg2+:SO4 2-<1:1.91, then the old halogen containing magnesium chloride component is mixed into bittern, the control of bittern intermediate ion mass ratio is existed
Mg2+:SO4 2-=1:1.89.
40.95 kilograms of high-purity six water magnesium sulfate can be finally made in the bittern of raw material per ton in step a), equivalent to bittern
The rate of recovery of middle magnesium elements is 11% or so, and resulting high-purity six water magnesium sulfates purity has reached 99.9%, from heating response
The bittern discharged in kettle, which is returned in salt pond, to be continued with conventional day solar salt flow to extract various inorganic salts therein.
Claims (2)
1. a kind of method that high-purity six water magnesium sulfate is extracted from bittern, it is characterised in that comprise the following steps：
A) bittern is poured into salt pond, Mg in detection bittern2+And SO4 2-The mass content of two kinds of ions, controls bittern intermediate ion matter
Amount compares Mg2+:SO4 2-=1:1.20-1.91, stands 24-72 hours, shovels out the carnallite of bittern bottom deposit；
B) the gypsum consumption being equably sprinkled into bittern in the gypsum for being ground to 100-200 mesh, every cubic metre of bittern is 1-10
Kilogram, continue standing sedimentation 24-72 hours, then shovel out the miscellaneous mud of bittern bottom deposit；
C) make bittern natural evaporation under sunshine condition, moisture is gradually steamed and monitor Na in bittern+And SO4 2-Two kinds of ions
Mass content changes, as bittern intermediate ion mass ratio Na+:SO4 2-=1:2.25-2.70 when shovel out the carnallite of bittern bottom deposit
With miscellaneous mud；
D) natural evaporation is then proceeded to, when bittern intermediate ion mass ratio reaches Na+:SO4 2-=1:2.71-4.34 when, collect bittern
It is simultaneously transported in heating response kettle by carnallite that bottom is deposited again together with bittern；
E) in heating response kettle, control bittern and carnallite mixture temperature is between 45-55 DEG C and stirs 4-6 hours, so
The carnallite of heating response kettle bottom deposit is separated and discharged afterwards；
F) brine temperature is reduced to 20-35 DEG C in heating response kettle and is incubated 6-36 hours；
G) bittern in heating response kettle is discharged, the salt for now separating out and depositing again in heating response kettle is collected, through centrifugation
High-purity six water magnesium sulfate is obtained after dehydration, drying.
2. a kind of method that high-purity six water magnesium sulfate is extracted from bittern as claimed in claim 1, it is characterised in that the step
The rapid bittern for a) pouring into salt pond is Na+,K+,Mg2+//Cl-,SO4 2--H2O salt-water system type bittern, and the matter of bittern intermediate ion
Amount compares Cl-:Na+=1:0.16-0.57, mass ratio K+:Na+<1:20。
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| CN107935003B (en) * | 2017-11-22 | 2019-09-17 | 中国科学院青海盐湖研究所 | A method of high-purity magnesium sulfate is prepared by magnesium sulfate waste |
| CN107758707B (en) * | 2017-11-22 | 2019-09-17 | 中国科学院青海盐湖研究所 | From the rough middle method for preparing high-purity magnesium sulfate of magnesium sulfate |
| CN107739042B (en) * | 2017-11-22 | 2019-09-17 | 中国科学院青海盐湖研究所 | The method that high-purity magnesium sulfate is prepared by magnesium sulfate waste |
| CN115465874B (en) * | 2022-11-15 | 2023-03-07 | 山西大学 | Device and method for preparing micron-sized crystalline magnesium sulfate hollow tube |
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| CN101497453B (en) * | 2008-01-30 | 2010-08-04 | 中国科学院过程工程研究所 | Method for preparing ammonium magnesium sulfate hexahydrate from giobertite |
| CN102030350B (en) * | 2010-11-11 | 2012-07-11 | 北京科技大学 | Method for preparing magnesium sulfate heptahydrate by taking magnesium chloride bittern from salt lake as raw material |
| CN103112908A (en) * | 2013-01-26 | 2013-05-22 | 刘晓钟 | Method for treating magnesium-sulfate-containing wastewater in hydrometallurgy |
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