CN107381603A - The preparation method of picromerite based on adding halogen method - Google Patents
The preparation method of picromerite based on adding halogen method Download PDFInfo
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- CN107381603A CN107381603A CN201710630398.0A CN201710630398A CN107381603A CN 107381603 A CN107381603 A CN 107381603A CN 201710630398 A CN201710630398 A CN 201710630398A CN 107381603 A CN107381603 A CN 107381603A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/12—Preparation of double sulfates of magnesium with sodium or potassium
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
- C05D1/02—Manufacture from potassium chloride or sulfate or double or mixed salts thereof
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Abstract
The invention discloses a kind of preparation method of the picromerite based on adding halogen method, comprise the steps：S1, initial bittern evaporated brine, obtain the low high potassium type sulfuric acid salt mine of magnesium；S2, the high potassium type sulfuric acid salt mine of low magnesium and unsaturated magnesium chloride solution be subjected to mixed once dispensing, once converted after removing sodium chloride, one turn of solid low-sodium and high-potassium type sulfuric acid salt mine is obtained through separation of solid and liquid；S3, one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and water are carried out to secondary mix, progress secondary conversion, through the wet picromerite filter cake of separation of solid and liquid acquisition；S4, wet picromerite filter cake is dried, obtain picromerite.The present invention using Hoh Yanhu after sodium chloride produce caused discarded bittern or its similar to forming bittern as initial bittern, by once evaporating brine and converting twice halogen, the complex point can be used to produce picromerite in the Brine resources of saltcake phase region, the recycling of potassium magnesium resource is realized, further fully utilizes salt lake resources.
Description
Technical field
The invention belongs to technical field of comprehensive utilization of salt lake brine, specifically, is related to a kind of soft potassium based on adding halogen method
The preparation method of magnesium alum.
Background technology
China has abundant salt lake resources, the various sylvite of separation and Extraction, lithium salts from salt lake bittern, to meet country's hair
Exhibition and economic needs.For the Qinghai-xizang Plateau Region of China's salt lake resources preservation, it is clear that the salt lake bittern composition of different regions
Difference, correspondingly, that is, it is adapted to different preparation technologies.
Picromerite (also referred to as potash magnesium sulphate fertilizer) is a kind of important potash fertilizer, and the raw material of production potassium sulfate.China's sulphur
The main producing region Qinghai east West Taijinar Salt Lake of sour potassic-magnesian fertilizer, salt lake bittern are located at picromerite phase region, the system of shining in phasor
Potassium mixed salt picromerite can be directly generated in water conversion process is added.What it is such as patent CN 1482102A representatives is salt lake bittern
Be located at picromerite phase region in phasor, shine system potassium mixed salt can directly generate picromerite in water conversion process is added be
The technique that the good ore deposit of condition prepares potash magnesium sulphate fertilizer.Domestic salt lake production picromerite also has some other reports at present, such as specially
Sharp CN 101412639A, it discloses it is a kind of leach potassium after it is secondary into ore deposit, again convert production potash magnesium sulphate fertilizer method, still
The problem of there is technological process length in this method, control point is more.But except above-mentioned initial bittern composition be advantageous to prepare it is soft
The situation of leonite, substantial amounts of K is still suffered from other salt lake bitterns+、Mg2+、SO4 2-Plasma, if can be to other kinds of salt
Lake bittern water is utilized, and could really realize the comprehensive utilization of resource.
Hoh Yanhu positioned at Qinghai Province Wulan County, its resource is based on solid halite, and reserves are up to 10.3 hundred million tons, wherein table
Outer intercrystalline bittern belongs to sulfate type sulfuric acid magnesium hypotype solid-liquid and deposits salt lake, intercrystalline bittern contains largely up to 1.969 billion cubic meters
K+、Mg2+、SO4 2-Deng composition.For many years, the utilization to Hoh Yanhu realizes far away resource to produce based on sodium chloride
Comprehensive utilization, while go back by-product and largely discard bittern containing potassium.These discard bittern containing potassium to be reused, and not only waste
Resource, take up an area seriously, pollution is also caused to Salt Lake Area.
The content of the invention
To solve the above-mentioned problems of the prior art, the invention provides a kind of system of the picromerite based on adding halogen method
Preparation Method, the preparation method can caused discarded bittern be able to sufficiently recovery profit after sodium chloride is extracted to Hoh Yanhu
With.
In order to reach foregoing invention purpose, present invention employs following technical scheme：
A kind of preparation method of the picromerite based on adding halogen method, including step：
S1, initial bittern evaporated brine, obtain the low high potassium type sulfuric acid salt mine of magnesium；Wherein, in the initial bittern, Na+Mass percent be 3.0%~5.0%, Mg2+Mass percent be 2.0%~4.5%, K+Mass percent be
0.5%~1.0%, Cl-Mass percent be 13.0%~16.0%, SO4 2-Mass percent be 3.0%~6.0%；
In the low high potassium type sulfuric acid salt mine of magnesium, Na+Mass percent be 18.0%~20.0%, Mg2+Mass percent be
1.5%~4.0%, K+Mass percent be 5.0%~8.0%, Cl-Mass percent be 32.5%~35.0%, SO4 2-
Mass percent be 18.0%~22.0%；
S2, by the low high potassium type sulfuric acid salt mine of magnesium and unsaturated magnesium chloride solution according to 2:1~2.5:1 mass ratio enters
Row mixed once dispensing, after mechanical grading removes sodium chloride, once converted, solid-liquid is carried out after reaching crystallization of the dissolution and precipitation balance
Separation, obtain one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and one turn of mother liquor；Wherein, in described one turn solid low-sodium and high-potassium type sulfate
In, Na+Mass percent be 4.5%~7.5%, Mg2+Mass percent be 4.0%~7.5%, K+Mass percent
For 11.0%~13.5%, Cl-Mass percent be 21.0%~25.0%, SO4 2-Mass percent for 17.0%~
20.0%；In one turn of mother liquor, Na+Mass percent be 2.0%~3.5%, Mg2+Mass percent be 18.0%
~22.0%, K+Mass percent be 4.5%~6.5%, Cl-Mass percent be 53.5%~58.0%, SO4 2-Matter
It is 14.0%~16.5% to measure percentage；
S3, by described one turn solid low-sodium and high-potassium type sulfuric acid salt mine and water according to 1:0.3~1:0.5 mass ratio carries out secondary
Mix, secondary conversion is carried out, carry out separation of solid and liquid after reaching crystallization of the dissolution and precipitation balance, obtain wet picromerite filter cake and two
Turn mother liquor；Wherein, in two turns of mother liquors, Na+Mass percent be 2.0%~3.5%, Mg2+Mass percent be
18.0%~22.0%, K+Mass percent be 4.3%~6.5%, Cl-Mass percent be 53.5%~58.0%,
SO4 2-Mass percent be 14.0%~16.5%；
S4, the wet picromerite filter cake is dried, obtain picromerite；Wherein, in the picromerite, with K2O is counted
K mass percent be not less than 18%.
Further, two turns of mother liquors are incorporated to progress mixed once dispensing in the step S2；Wherein, described two turns
The mass ratio of mother liquor and the unsaturated magnesium chloride solution is 0.5:1~1:1.
Further, the wet picromerite filter cake is incorporated in the step S3 and carries out secondary mix；Wherein, institute
The mass ratio for stating wet picromerite filter cake and described one turn solid low-sodium and high-potassium type sulfuric acid salt mine is 0.01:1~0.05:1；Described
In picromerite, with K2The K of O meters mass percent is more than 21%.
Further, in the unsaturated magnesium chloride solution, Mg2+Mass percent be 10.0%~12.0%.
Further, in the step S2,20min~30min is once converted at 20 DEG C~30 DEG C.
Further, in the step S3, secondary conversion 10min~30min is carried out at 20 DEG C~30 DEG C.
The present invention using Hoh Yanhu after sodium chloride produce caused discarded bittern or its similar bittern that forms as initially
Bittern, by once evaporating brine and converting twice halogen, you can the complex point (Na such as is helped into saltcake phase region with reference to gold+,K+,Mg2+//
Cl-,SO4 2--H225 DEG C of metastable phase diagrams of O systems) Brine resources be used to producing picromerite, abundant recycling is therein
Potassium magnesium resource, and the product can be further extended to other sylvite such as production potassium sulfate, further to comprehensively utilize the salt lake
Resource；And present invention process flow is simple, positive effect, preparation-obtained picromerite product particle is big, and quality is good；
Meanwhile when, when caused discarded bittern is as initial bittern after producing sodium chloride, also solving existing process using Hoh Yanhu
In, pollution environment big to the discarded bittern floor space in the presence of the utilization of Hoh Yanhu, the wasting of resources the problems such as.
Brief description of the drawings
The following description carried out in conjunction with the accompanying drawings, above and other aspect, feature and the advantage of embodiments of the invention
It will become clearer, in accompanying drawing：
Fig. 1 is the process chart of the preparation method of the picromerite according to an embodiment of the invention based on adding halogen method.
Embodiment
Hereinafter, with reference to the accompanying drawings to embodiments of the invention are described in detail.However, it is possible to come in many different forms real
Apply the present invention, and the specific embodiment of the invention that should not be construed as limited to illustrate here.Conversely, there is provided these implementations
Example is in order to explain the principle and its practical application of the present invention, so that others skilled in the art are it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.
It will be appreciated that although term " once ", " secondary " etc. can be used to describe various technological operations herein, still
These technological operations should not be limited by these terms.These terms are only used for a technological operation and another identical work
Skill operation makes a distinction.
The invention provides a kind of preparation method of the picromerite based on adding halogen method, referring in particular to Fig. 1, the preparation method
Comprise the steps：
Step S1, initial bittern is evaporated brine, obtains the low high potassium type sulfuric acid salt mine of magnesium.
Specifically, the initial bittern refers to wherein Na+Mass percent for 3.0%~5.0%, Mg2+Quality hundred
Fraction is 2.0%~4.5%, K+Mass percent for 0.5%~1.0%, Cl-Mass percent for 13.0%~
16.0%th, SO4 2-Mass percent be 3.0%~6.0% salt lake bittern or produced during the utilization of salt lake bittern
Discarded bittern or middle bittern etc.；In embodiments of the invention preferably by Hoh Yanhu after sodium chloride has been produced it is caused useless
Bittern is abandoned as the initial bittern.
Above-mentioned initial bittern is evaporated brine by normal temperature (generally 20 DEG C~30 DEG C), obtains wherein Na+Mass percent
For 18.0%~20.0%, Mg2+Mass percent for 1.5%~4.0%, K+Mass percent for 5.0%~8.0%,
Cl-Mass percent for 32.5%~35.0%, SO4 2-Mass percent be 18.0%~22.0% the high potassium type of low magnesium
Sulfuric acid salt mine；Pass through said components, it can be seen that the complex point of the low high potassium type sulfuric acid salt mine of magnesium is located at gold and the Na such as helps+,K+,
Mg2+//Cl-,SO4 2--H225 DEG C of metastable phase diagrams of O systems (are helped, Xiao Xianzhi, beam type plum (Na referring to gold+,K+,Mg2+),(Cl-,
SO4 2-),H2Research [J] chemistry journals of O quinary system metastable equilibriums, 1980,38 (4):In saltcake phase region 313-321),
If only simply being evaporated brine to the low high potassium type sulfuric acid salt mine of magnesium, the mixture of NaCl and saltcake can only be typically produced, and nothing
Method is utilized to potassium magnesium resource therein.Therefore, with reference to following step successively converted halogen twice, by potassium magnesium therein from
Son is recycled in the form of double salt.
Step S2, by the high potassium type sulfuric acid salt mine of low magnesium and unsaturated magnesium chloride solution according to 2:1~2.5:1 mass ratio enters
Row mixed once dispensing, after mechanical grading removes sodium chloride, once converted, solid-liquid is carried out after reaching crystallization of the dissolution and precipitation balance
Separation, obtain one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and one turn of mother liquor.
Specifically, when the high potassium type sulfuric acid salt mine of low magnesium and unsaturated magnesium chloride solution carry out mixed once dispensing, by
Cause sodium chloride to separate out in the salting out of magnesium chloride, therefore this partial oxidation sodium is removed by mechanical grading first, to enter
Sodium content in one step reduction system；Then liquid system continues once to convert, will after crystallization of the dissolution and precipitation balance is reached
The precipitation of low-sodium and high-potassium type sulfuric acid salt mine is had, after carrying out separation of solid and liquid, that is, obtains wherein Na+Mass percent for 4.5%~
7.5%th, Mg2+Mass percent for 4.0%~7.5%, K+Mass percent for 11.0%~13.5%, Cl-Quality
Percentage is 21.0%~25.0%, SO4 2-Mass percent be one turn of 17.0%~20.0% solid low-sodium and high-potassium type sulfuric acid
Salt mine and wherein Na+Mass percent for 2.0%~3.5%, Mg2+Mass percent for 18.0%~22.0%, K+
Mass percent for 4.3%~6.5%, Cl-Mass percent for 53.5%~58.0%, SO4 2-Mass percent be
14.0%~16.5% one turn of mother liquor.
In the present invention, the application target of magnesium chloride solution is in introducing Mg into system2+, on the one hand it is increase system
Middle Mg2+Relative amount, finally to obtain magnesium salts, on the other hand cause NaCl in Mg2+Salting out under separate out remove；Cause
This, does not make special provision for the concentration of magnesium chloride solution, is typically avoided saturation magnesium chloride solution, this is due to saturation chlorine
The viscosity of change magnesium solution is very big, will influence the practical operation of mixed once dispensing；If but the unsaturated magnesium chloride solution is dense
Degree is too low, it will causes next potassium magnesium ion for turning to dissolve into mother liquor of equal conditions etc. excessive, and causes one turn of solid low-sodium and high-potassium
Type sulfate mineral products amount is relatively low.It is therefore preferred that control Mg in the unsaturated magnesium chloride solution2+Mass percent be
10.0%~12.0%.
Preferably, on the one hand consider aforesaid operations treating capacity it is very large, on the other hand consider reduce energy consumption, save into
This factor, the above-mentioned operation once converted carry out 20min~30min under 20 DEG C~30 DEG C of normal temperature environment.
Step S3, by one turn of solid low-sodium and high-potassium type sulfuric acid salt mine with water according to 1:0.3~1:0.5 mass ratio carries out secondary
Mix, secondary conversion is carried out, carry out separation of solid and liquid after reaching crystallization of the dissolution and precipitation balance, obtain wet picromerite filter cake and two
Turn mother liquor.
Specifically, after one turn of solid low-sodium and high-potassium type sulfuric acid salt mine being carried out into secondary mix, secondary conversion with water, treat
After reaching crystallization of the dissolution and precipitation balance, i.e., can separate out picromerite solid phase, through separation of solid and liquid, then can obtain wet picromerite filter cake and
Wherein Na+Mass percent for 2.0%~3.5%, Mg2+Mass percent for 18.0%~22.0%, K+Quality hundred
Fraction is 4.5%~6.5%, Cl-Mass percent for 53.5%~58.0%, SO4 2-Mass percent for 14.0%~
16.5% 2 turn of mother liquor.
Secondary conversion carries out 10min~30min preferably at 20 DEG C~30 DEG C.
Step S4, wet picromerite filter cake is dried, is obtained wherein with K2The K of O meters mass percent is not less than 18%
Picromerite.
What deserves to be explained is typically during the comprehensive utilization of Brine resources, it can be related to the operation of separation of solid and liquid, and
Improve utilization ratio for further, promote the purpose of crystallization, solid phase caused by correspondence or mother liquor can be subjected to reuse, to
Reach line balancing after several circulations, improving production efficiency, steady production simultaneously ensure product quality to greatest extent；Therefore,
Preferably, two turns of mother liquors caused by above-mentioned steps S3 are back in step S2, and potassium type sulfuric acid salt mine high with low magnesium and not
Saturation magnesium chloride solution carries out mixed once dispensing jointly, and controls the high potassium type sulfuric acid salt mine of low magnesium, unsaturated magnesium chloride molten
Liquid, the mass ratio of two turns of mother liquor threes are 2~2.5:1:0.5~1；Additionally preferably, by caused portion in above-mentioned steps S3
Wet picromerite filter cake is divided to be back in step S3, using the crystal seed crystallized as picromerite, with one turn of solid low-sodium and high-potassium type sulphur
Hydrochlorate ore deposit and water carry out secondary mix and secondary conversion jointly, and control one turn of solid low-sodium and high-potassium type sulfuric acid salt mine, water,
The mass ratio of wet picromerite filter cake three is 1:0.3~0.5:0.01~0.05.In this way, treat that above-mentioned complete preparation technology reaches
To after line balancing, you can obtain with K2The wherein K mass percent of O meters is more than 21% picromerite product.
Especially it is noted that statement on K contents in above-mentioned picromerite product, " with K2The wherein K matter of O meters
Measure percentage " although referring in picromerite product and K being not present2This materials of O, but wherein K mass percent is rolled over
Synthesize K2O form represents.
As can be seen that the preparation method of the picromerite based on adding halogen method of the present invention, is preferably producing Hoh Yanhu
Potassium magnesium resource after complete sodium chloride in caused discarded bittern has carried out further recycling, produces economic benefit more
High picromerite product；And in whole technical process, other raw materials only relate to unsaturated magnesium chloride solution and water, chlorination
Magnesium is Salt Lake Area another kind excess by-product, cheap, and its recycling is also solved into its a large amount of stacking, pollution ring
Border, destroy the problem of Salt Lake Area balance.
Hereinafter, the preparation method of the above-mentioned picromerite based on adding halogen method, but this will be illustrated by specific embodiment
The offer of a little embodiments is only the wherein a certain specific example of above-mentioned preparation method, is not the specific limit of above-mentioned preparation method
It is fixed.Also, following embodiments represent process after technique reaches line balancing, therefore above-mentioned two turns of mother liquors and wet soft be present
The situation of leonite reusing filter cake.
Embodiment 1
In the present embodiment, it is caused discarded after sodium chloride has been produced to derive from Hoh Yanhu for the initial bittern used in it
Bittern, its leading ion composition are shown in Table 1.
The leading ion composition of 1 initial bittern of table
After step S1, the leading ion composition of the high potassium type sulfuric acid salt mine of low magnesium of acquisition is shown in Table 2.
The leading ion composition of the high potassium type sulfuric acid salt mine of 2 low magnesium of table
In step s 2, the high potassium type sulfuric acid salt mine of low magnesium, unsaturated magnesium chloride solution, the quality of two turns of mother liquor threes are controlled
Ratio is 2:1:1,15min or so is stirred after mixed once dispensing and carries out mechanical grading removing sodium chloride；Then at normal temperatures
30min is once converted, separation of solid and liquid obtains one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and one turn of mother liquor.
In the unsaturated magnesium chloride solution, Mg2+Mass percent be 10.0%~12.0%.
Wherein, the leading ion composition of one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and one turn of mother liquor is shown in Table 3, with quality percentage
Number meter.
The leading ion composition of the solid low-sodium and high-potassium type sulfuric acid salt mine of 3 one turns of table and one turn of mother liquor
In step s3, one turn of solid low-sodium and high-potassium type sulfuric acid salt mine, water, mass ratio of wet picromerite filter cake three are controlled
Example is 1:0.5:0.05,30min is stirred after secondary mix to carry out secondary conversion, separation of solid and liquid obtains wet picromerite filter
Cake and two turns of mother liquors.
Wherein, the leading ion composition of two turns of mother liquors is shown in Table 4.
The leading ion composition of 4 two turns of mother liquors of table
The wet picromerite filter cake that step S3 is obtained is obtained with K through drying2O meter wherein K mass percent be
21.4% picromerite product.
Embodiment 2
It in the description of embodiment 2, will not be repeated here, only described with embodiment 1 not with the something in common of embodiment 1
Same part.The difference of embodiment 2 and embodiment 1 is that in step sl, the leading ion composition of initial bittern is shown in Table 5.
The leading ion composition of 5 initial bittern of table
After step S1, the leading ion composition of the high potassium type sulfuric acid salt mine of low magnesium of acquisition is shown in Table 6.
The leading ion composition of the high potassium type sulfuric acid salt mine of 6 low magnesium of table
In step s 2, the high potassium type sulfuric acid salt mine of low magnesium, unsaturated magnesium chloride solution, the quality of two turns of mother liquor threes are controlled
Ratio is 2.5:1:0.7,10min or so is stirred after mixed once dispensing and carries out mechanical grading removing sodium chloride；Then normal
Temperature is lower once to be converted 25min, and separation of solid and liquid obtains one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and one turn of mother liquor.
Wherein, the leading ion composition of one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and one turn of mother liquor is shown in Table 7, with quality percentage
Number meter.
The leading ion composition of the solid low-sodium and high-potassium type sulfuric acid salt mine of 7 one turns of table and one turn of mother liquor
In step s3, one turn of solid low-sodium and high-potassium type sulfuric acid salt mine, water, mass ratio of wet picromerite filter cake three are controlled
Example is 1:0.4:0.03,20min is stirred after secondary mix to carry out secondary conversion, separation of solid and liquid obtains wet picromerite filter
Cake and two turns of mother liquors.
Wherein, the leading ion composition of two turns of mother liquors is shown in Table 8.
The leading ion composition of 8 two turns of mother liquors of table
The wet picromerite filter cake that step S3 is obtained is obtained with K through drying2O meter wherein K mass percent be
22.3% picromerite product.
Embodiment 3
It in the description of embodiment 3, will not be repeated here, only described with embodiment 1 not with the something in common of embodiment 1
Same part.The difference of embodiment 3 and embodiment 1 is that in step sl, the leading ion composition of initial bittern is shown in Table 9.
The leading ion composition of 9 initial bittern of table
After step S1, the leading ion composition of the high potassium type sulfuric acid salt mine of low magnesium of acquisition is shown in Table 10.
The leading ion composition of the high potassium type sulfuric acid salt mine of 10 low magnesium of table
In step s 2, the high potassium type sulfuric acid salt mine of low magnesium, unsaturated magnesium chloride solution, the quality of two turns of mother liquor threes are controlled
Ratio is 2:1:0.5,5min or so is stirred after mixed once dispensing and carries out mechanical grading removing sodium chloride；Then at normal temperatures
20min is once converted, separation of solid and liquid obtains one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and one turn of mother liquor.
Wherein, the leading ion composition of one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and one turn of mother liquor is shown in Table 11, with quality hundred
Fraction meter.
The leading ion composition of the solid low-sodium and high-potassium type sulfuric acid salt mine of 11 1 turns of table and one turn of mother liquor
In step s3, one turn of solid low-sodium and high-potassium type sulfuric acid salt mine, water, mass ratio of wet picromerite filter cake three are controlled
Example is 1:0.3:0.01,10min is stirred after secondary mix to carry out secondary conversion, separation of solid and liquid obtains wet picromerite filter
Cake and two turns of mother liquors.
Wherein, the leading ion composition of two turns of mother liquors is shown in Table 12.
The leading ion composition of 12 2 turns of mother liquors of table
The wet picromerite filter cake that step S3 is obtained is obtained with K through drying2O meter wherein K mass percent be
22.8% picromerite product.
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where not departing from the spirit and scope of the present invention limited by claim and its equivalent, can carry out herein form and
Various change in details.
Claims (6)
1. a kind of preparation method of the picromerite based on adding halogen method, it is characterised in that including step：
S1, initial bittern evaporated brine, obtain the low high potassium type sulfuric acid salt mine of magnesium；Wherein, in the initial bittern, Na+Matter
Amount percentage is 3.0%~5.0%, Mg2+Mass percent be 2.0%~4.5%, K+Mass percent for 0.5%~
1.0%, Cl-Mass percent be 13.0%~16.0%, SO4 2-Mass percent be 3.0%~6.0%；Described low
In the high potassium type sulfuric acid salt mine of magnesium, Na+Mass percent be 18.0%~20.0%, Mg2+Mass percent for 1.5%~
4.0%, K+Mass percent be 5.0%~8.0%, Cl-Mass percent be 32.5%~35.0%, SO4 2-Quality
Percentage is 18.0%~22.0%；
S2, by the low high potassium type sulfuric acid salt mine of magnesium and unsaturated magnesium chloride solution according to 2:1~2.5:1 mass ratio carries out one
Secondary mix, after mechanical grading removes sodium chloride, once converted, separation of solid and liquid carried out after reaching crystallization of the dissolution and precipitation balance,
Obtain one turn of solid low-sodium and high-potassium type sulfuric acid salt mine and one turn of mother liquor；Wherein, in described one turn solid low-sodium and high-potassium type sulfate, Na+Mass percent be 4.5%~7.5%, Mg2+Mass percent be 4.0%~7.5%, K+Mass percent be
11.0%~13.5%, Cl-Mass percent be 21.0%~25.0%, SO4 2-Mass percent for 17.0%~
20.0%；In one turn of mother liquor, Na+Mass percent be 2.0%~3.5%, Mg2+Mass percent be 18.0%
~22.0%, K+Mass percent be 4.3%~6.5%, Cl-Mass percent be 53.5%~58.0%, SO4 2-Matter
It is 14.0%~16.5% to measure percentage；
S3, by described one turn solid low-sodium and high-potassium type sulfuric acid salt mine and water according to 1:0.3~1:0.5 mass ratio carries out secondary mixing
Dispensing, secondary conversion is carried out, carry out separation of solid and liquid after reaching crystallization of the dissolution and precipitation balance, obtain wet picromerite filter cake and two turns of mothers
Liquid；Wherein, in two turns of mother liquors, Na+Mass percent be 3.5%~4.5%, Mg2+Mass percent be 2.0%
~3.5%, K+Mass percent be 2.0%~4.0%, Cl-Mass percent be 11.5%~13.5%, SO4 2-Matter
It is 5.0%~6.5% to measure percentage；
S4, the wet picromerite filter cake is dried, obtain picromerite；Wherein, in the picromerite, with K2The K's of O meters
Mass percent is not less than 18%.
2. preparation method according to claim 1, it is characterised in that be incorporated in the step S2 by two turns of mother liquors
Row mixed once dispensing；Wherein, the mass ratio of two turns of mother liquors and the unsaturated magnesium chloride solution is 0.5:1~1:1.
3. preparation method according to claim 2, it is characterised in that the wet picromerite filter cake is incorporated to the step
Secondary mix is carried out in S3；Wherein, the wet picromerite filter cake consolidates low-sodium and high-potassium type sulfuric acid salt mine with described one turn
Mass ratio is 0.01:1~0.05:1；In the picromerite, with K2The K of O meters mass percent is more than 21%.
4. according to any described preparation methods of claim 1-3, it is characterised in that in the unsaturated magnesium chloride solution,
Mg2+Mass percent be 10.0%~12.0%.
5. preparation method according to claim 1, it is characterised in that in the step S2, enter at 20 DEG C~30 DEG C
Row once converts 20min~30min.
6. preparation method according to claim 1, it is characterised in that in the step S3, enter at 20 DEG C~30 DEG C
Row secondary conversion 10min~30min.
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| CN201710630398.0A CN107381603A (en) | 2017-07-28 | 2017-07-28 | The preparation method of picromerite based on adding halogen method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052432A (en) * | 2018-11-07 | 2018-12-21 | 河北工业大学 | The method for preparing picromerite with salt-mixture |
| CN109354042A (en) * | 2018-11-22 | 2019-02-19 | 青海蓝湖善成生物技术有限公司 | The preparation method and picromerite feed of picromerite |
| CN109368669A (en) * | 2018-11-22 | 2019-02-22 | 青海蓝湖善成生物技术有限公司 | A kind of preparation method and picromerite feed of picromerite |
| CN111362284A (en) * | 2020-05-18 | 2020-07-03 | 天津君瑞和科技有限公司 | Method for preparing magnesium potassium sulfate from bittern obtained by preparing salt from seawater |
| CN115465874A (en) * | 2022-11-15 | 2022-12-13 | 山西大学 | Device and method for preparing micron-sized crystalline magnesium sulfate hollow tube |
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| CN101412639A (en) * | 2008-10-30 | 2009-04-22 | 中国科学院青海盐湖研究所 | Method for preparing potash magnesium sulphate fertilizer from potassium-containing solid mine by separation and extraction |
| WO2017108876A1 (en) * | 2015-12-22 | 2017-06-29 | Yara Dallol Bv | Method for the control of sulphate forming compounds in the preparation of potassium sulphate from potassium-containing ores at high ambient temperatures |
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| CN101412639A (en) * | 2008-10-30 | 2009-04-22 | 中国科学院青海盐湖研究所 | Method for preparing potash magnesium sulphate fertilizer from potassium-containing solid mine by separation and extraction |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052432A (en) * | 2018-11-07 | 2018-12-21 | 河北工业大学 | The method for preparing picromerite with salt-mixture |
| CN109354042A (en) * | 2018-11-22 | 2019-02-19 | 青海蓝湖善成生物技术有限公司 | The preparation method and picromerite feed of picromerite |
| CN109368669A (en) * | 2018-11-22 | 2019-02-22 | 青海蓝湖善成生物技术有限公司 | A kind of preparation method and picromerite feed of picromerite |
| CN111362284A (en) * | 2020-05-18 | 2020-07-03 | 天津君瑞和科技有限公司 | Method for preparing magnesium potassium sulfate from bittern obtained by preparing salt from seawater |
| CN115465874A (en) * | 2022-11-15 | 2022-12-13 | 山西大学 | Device and method for preparing micron-sized crystalline magnesium sulfate hollow tube |
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