CN106517250A - Method for preparing potassium chloride and magnesium sulfate from kainite - Google Patents
Method for preparing potassium chloride and magnesium sulfate from kainite Download PDFInfo
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- CN106517250A CN106517250A CN201610996729.8A CN201610996729A CN106517250A CN 106517250 A CN106517250 A CN 106517250A CN 201610996729 A CN201610996729 A CN 201610996729A CN 106517250 A CN106517250 A CN 106517250A
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- water
- concentrated water
- nanofiltration membrane
- kainite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
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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
Abstract
The invention discloses a method for preparing potassium chloride and magnesium sulfate from kainite. The method comprises the following steps: dissolving the kainite in water to obtain a kainite solution, and performing primary nanofiltration: performing primary nanofiltration treatment on the kainite solution by adopting a nanofiltration membrane system to obtain primary concentrated water and primary producing water, wherein the nanofiltration membrane system comprises a first nanofiltration membrane assembly and a first concentrated water tank and a first producing water tank which are connected to the first nanofiltration membrane assembly, the primary concentrated water is stored in the first primary concentrated water tank, and the primary producing water is stored in the first producing water tank; performing evaporative crystallization on the primary producing water to obtain potassium chloride; performing evaporative crystallization on the primary concentrated water to obtain magnesium sulfate, or performing secondary nanofiltration to obtain secondary concentrated water, and performing evaporative crystallization on the secondary concentrated water to obtain the magnesium sulfate. The invention provides a novel method for producing the potassium chloride and the magnesium sulfate from the kainite serving as a raw material; and furthermore, the method has the advantages of simple process, high product purity and high yield.
Description
Technical field
The invention belongs to inorganic salt preparing technical field, specifically, is related to one kind and prepares potassium chloride using kainite
With the method for magnesium sulfate.
Background technology
Potassium is one of three big nutrient (nitrogen, phosphorus, potassium) necessary to crop growth, and wherein potassium chloride is used as main
Potash fertilizer kind, account for more than the 90% of potash fertilizer total amount.China is a serious soil potassium deficiency country, with crop yield and
The continuous improvement of Nitrogen and phosphate application rate, the potassium amount that crop is removed from soil gradually increase, and with fertilizer, straw-returning and apply
Remove amount of the crop from soil can not be supplied with the potassium amount for giving back soil containing forms such as potassium fertilizers, soil potassium element is exhausted increasingly
Seriously, potassium deficiency area gradually expands, become restriction agricultural production continue, one of the major reason of stable development；Therefore, greatly
Power develops China's potassium resource, produces potassium chloride, improves grain yield, significant to maintaining social stability.
At present, the Technology of potassium chloride is produced with carnallite or sylvite as raw material, according to carnallite and sylvite
Composition it is different, and adopt various processes preparing potassium chloride.
Kainite (KCl MgSO4·3H2O it is) a kind of natural chloride-sulfate type double salt containing potassium, magnesium, often
With the symbiosis in the form of potassium mixed salt such as sylvite, carnallite, halite, picromerite, it is higher than 35 DEG C to form temperature, its dissolution velocity
Relatively slow, the technique rear for needing Jing numerous and diverse can be used as chemical fertilizer.
At this stage, the main process and utilization technology of kainite is to add water thereto to be converted into potash magnesium sulphate fertilizer (K2SO4·
MgSO4·6H2O), then with chlorination nak response, further prepare potassium sulfate.
At present, the Technology for preparing potassium chloride and/or magnesium sulfate using kainite not yet has relevant report.
The content of the invention
For solving the problems, such as above-mentioned prior art, the invention discloses one kind using kainite prepare potassium chloride and
The method of magnesium sulfate, there is provided it is a kind of using kainite as raw material producing the new method of potassium chloride and magnesium sulfate, and the party
Method has the advantages that process is simple, product purity height, high income.
In order to reach foregoing invention purpose, following technical scheme is present invention employs：
A kind of method that utilization kainite prepares potassium chloride and magnesium sulfate, including step：By the kainite in water
Middle dissolving, obtains kainite solution；One section of nano-filtration step：One section is carried out to the kainite solution using nanofiltration membrane system
Nanofiltration is processed, and obtains one section of concentrated water and one section of product water；Wherein, the nanofiltration membrane system includes the first nanofiltration membrane component, Yi Jilian
The first concentrated water case being connected on first nanofiltration membrane component and first produces water tank；It is dense that one section of concentrated water is stored in described first
In water tank, described one section is produced water and is stored in the first product water tank；Water is produced to described one section and is evaporated crystallization, obtain described
Potassium chloride；Crystallization is evaporated to one section of concentrated water, obtains the magnesium sulfate.
Further, the nanofiltration membrane system also includes the first booster pump before being arranged on first nanofiltration membrane component.
Further, the pressure of first booster pump is 0.6MPa～1.5MPa.
Further, the nanofiltration membrane system is concentrated water internal-circulation type membranous system.
Another object of the present invention is to the method that another kind prepares potassium chloride and magnesium sulfate using kainite is provided, bag
Include step：The kainite is dissolved in water, kainite solution is obtained；One section of nano-filtration step：Using nanofiltration membrane system
Carry out one section of nanofiltration to process to the kainite solution, obtain one section of concentrated water and one section of product water；Wherein, the nanofiltration membrane system
Water tank is produced including the first nanofiltration membrane component and the first concentrated water case being connected on first nanofiltration membrane component and first；Institute
State one section of concentrated water to be stored in the first concentrated water case, described one section is produced water and is stored in the first product water tank；To described one
Section is produced water and is evaporated crystallization, obtains the potassium chloride；Two-stage nitration nano-filtration step：The nanofiltration membrane system is also described including being connected to
The second nanofiltration membrane component and the second concentrated water case and second being connected on second nanofiltration membrane component on first concentrated water case
Produce water tank；After one section of nano-filtration step, two-stage nitration is carried out to first concentrated water using second nanofiltration membrane component and is received
Filter is processed, and obtains two-stage nitration concentrated water and two-stage nitration produces water；The two-stage nitration concentrated water is stored in the second concentrated water case, and the two-stage nitration produces water
It is stored in described second to produce in water tank；Crystallization is evaporated to the two-stage nitration concentrated water, obtains the magnesium sulfate.
Further, the nanofiltration membrane component also includes being arranged on the first supercharging before first nanofiltration membrane component
Pump and the second booster pump being arranged between the first concentrated water case and second nanofiltration membrane component.
Further, the pressure of first booster pump is 0.6MPa～1.5MPa, and the pressure of second booster pump is
1.2MPa～2.5MPa.
Further, the two-stage nitration produces water and is incorporated in one section of product water.
Further, the nanofiltration membrane system is concentrated water internal-circulation type membranous system.
Further, the part two-stage nitration concentrated water is incorporated in the kainite solution.
Beneficial effects of the present invention：
(1) consumption for dissolving kainite fresh water is defined by the setting concentration of potassium chloride in saline solution and magnesium sulfate, is prevented
The only excessive consumption of fresh water；
(2) method of the present invention is preferably separated using two sections of nanofiltration membrane systems, is further separated in one section of concentrated water
Magnesium sulfate and potassium chloride, improve the separation yield of potassium chloride；
(3) every section of nanofiltration membrane component loads reflux inlet, realizes each section of concentrated water interior circulation, maintains water inlet in nanofiltration membrane component
Flow velocity is stablized, while not receiving the change of leading portion nanofiltration membrane component pollution level or water inlet composition and changing；
(4) present invention adopts concentrated water part outer circulation membranous system, part two-stage nitration concentrated water to be back in kainite solution, increases
The relative scale of magnesium sulfate in big kainite solution, so that further improve the nanofiltration separation efficiency of magnesium sulfate and potassium chloride；
In combination with each section of evaporation mother solution and the composition of washing mother solution, the circulating load of two-stage nitration concentrated water is adjusted, kainite solution is met
Concentration requirement；The two-stage nitration concentrated water for being introduced into outer circulation is used for preparing sulphuric acid magnesium products, so as to realize the comprehensive utilization of two-stage nitration concentrated water；
(5) each section of evaporation mother solution, washing mother solution and recycle-water are recycled in being back to kainite solution, are improved
The cyclic utilization rate of fresh water and salt；
(6), in evaporation and crystal process, theoretical direction and calculating are carried out using Phase Diagram for Aqueous Salt Solutions, it is ensured that in crystalline solid phase
The high-purity of product, beneficial to the quality standard of control product.
Description of the drawings
By combining the following description that accompanying drawing is carried out, above and other aspect of embodiments of the invention, feature and advantage
Will become clearer from, in accompanying drawing：
Fig. 1 is the technique of the method that the utilization kainite of embodiments in accordance with the present invention 2 prepares potassium chloride and magnesium sulfate
Flow chart；
Fig. 2 is the step of utilization kainite of embodiments in accordance with the present invention 2 prepares the method for potassium chloride and magnesium sulfate
Flow chart.
Specific embodiment
Hereinafter, with reference to the accompanying drawings to describing embodiments of the invention in detail.However, it is possible to come real in many different forms
Apply the present invention, and the present invention should not be construed as limited to the specific embodiment that illustrates here.On the contrary, there is provided these enforcements
Example is for the principle and its practical application of explaining 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.In the accompanying drawings, for the sake of clarity, element can be exaggerated
Shape and size, and identical label will be used to indicate same or analogous element all the time.
It will be appreciated that although various elements can be described using term " first ", " second " etc. here, these
Element should not be limited by these terms.These terms are only used for making a distinction an element and another element.
Embodiment 1
Present embodiment discloses a kind of method that utilization kainite prepares potassium chloride and magnesium sulfate, according to the present embodiment
The method that potassium chloride and magnesium sulfate are prepared using kainite comprises the steps：
S1, kainite is dissolved in water, obtain kainite solution.
In kainite solution, the concentration of KCl is 15g/L～35g/L, MgSO4Concentration be 30g/L～60g/L.
S2, one section of nano-filtration step：One section of nanofiltration is carried out using nanofiltration membrane system to process to kainite solution, one section is obtained
Concentrated water and one section of product water.
Specifically, nanofiltration membrane system include the first nanofiltration membrane component and be connected on the first nanofiltration membrane component
One concentrated water case and first produces water tank；First concentrated water case is used for storing one section of concentrated water, and first produces water tank for storing one section of product water.
Preferably, the nanofiltration membrane system also includes being arranged on the first booster pump before the first nanofiltration membrane component.
In the present embodiment, the pressure for controlling the first booster pump is 0.6MPa～1.5MPa.
Preferably, the nanofiltration membrane system adopted by the present embodiment is concentrated water internal-circulation type membranous system；That is, in nanofiltration
Load reflux inlet in membranous system, one section of part concentrated water can by reflux inlet be returned directly to the first nanofiltration membrane component import and with
Kainite solution merges, and is again introduced into the first nanofiltration membrane component and is separated.Concentrated water interior circulation can make the first NF membrane
Water inlet flow rate kept constant in component, the first nanofiltration membrane component import are consistent to the pressure between exporting, so that the
The desalination rate of one nanofiltration membrane component is improved, and which greatly enhances separation efficiency and the system response rate, reduces the level of nanofiltration
Number.
S3, water is produced to one section be evaporated crystallization, acquisition potassium chloride；Crystallization is evaporated to one section of concentrated water, obtains sulphuric acid
Magnesium.
Because still suffering from the potassium chloride of 10%～20% (wt%) in one section of concentrated water, in order to further improve the receipts of potassium chloride
Rate, there is provided the technical scheme in embodiment 2.
Embodiment 2
Present embodiment discloses the method that another kind preferably prepares potassium chloride and magnesium sulfate using kainite, concrete to join
According to Fig. 1, its based on device include the dissolving tank 1 being sequentially connected and nanofiltration membrane system；Specifically, nanofiltration membrane system includes first
Nanofiltration membrane component 21, the first concentrated water case (not shown) being connected on the first nanofiltration membrane component 21 and first produce water tank (figure
Not shown in), the second nanofiltration membrane component 22 for being connected on the first concentrated water case, and be connected on the second nanofiltration membrane component 22
Second concentrated water case (not shown) and second produces water tank (not shown).
Preferably, above-mentioned nanofiltration membrane system also include being arranged on the first booster pump 23 before the first nanofiltration membrane component and
The second booster pump 24 being arranged between the first concentrated water case and the second nanofiltration membrane component 22.
In the description of embodiment 2, will not be described here with the something in common of embodiment 1, only describe with embodiment 1 not
Same part.Referring in particular to Fig. 1 and Fig. 2, in example 2, step Q1, Q2 phase corresponding with step S1, S2 in embodiment 1 respectively
Together；Include step Q3, two-stage nitration nano-filtration step after step Q2：Two-stage nitration is carried out using 22 pairs of the first concentrated waters of the second nanofiltration membrane component to receive
Filter is processed, and obtains two-stage nitration concentrated water and two-stage nitration produces water.
One section of concentrated water is stored in the first concentrated water case, and one section is produced water and is stored in the first product water tank；And the storage of two-stage nitration concentrated water
In the second concentrated water case, two-stage nitration produces water and is stored in the second product water tank.
In the present embodiment, the pressure for controlling the first booster pump 23 is 0.6MPa～1.5MPa, controls the second booster pump 24
Pressure be 1.2MPa～2.5MPa.
Preferably, the nanofiltration membrane system adopted by the present embodiment is similarly concentrated water internal-circulation type membranous system；That is,
Load reflux inlet (not shown) in nanofiltration membrane system, part concentrated water can be returned directly to nanofiltration membrane component by reflux inlet
Import is simultaneously merged with water inlet (i.e. kainite solution, one section of concentrated water), is again introduced into corresponding nanofiltration membrane component and is separated.
Concentrated water interior circulation can make the water inlet flow rate kept constant in nanofiltration membrane component, pressure of the nanofiltration membrane component import between exporting
It is consistent, so that the desalination rate of nanofiltration membrane component is improved, which greatly enhances separation efficiency and the system response rate, subtract
The series of nanofiltration is lacked.
NF membrane in above-mentioned first nanofiltration membrane component 21 and the second nanofiltration membrane component 22 can select any ripe production,
Using rolling nanofiltration membrane component, such as DOW companies NF90, NF270 series NF membrane, the DK of GE companies, DL, CK,
The series NF membrane such as Duraslick, HL, MUNi NF.DK, DL series NF membrane of the preferred GE companies of the present embodiment.
What deserves to be explained is, in the present embodiment, replacement step of step Q3 for step S3 in embodiment 1；Namely
Say, in the present embodiment, do not carry out step S3 in embodiment 1, but one section of concentrated water is carried out into two-stage nitration nanofiltration process.
Q4, the mixing to one section of product water and two-stage nitration product water are produced water and are evaporated crystallization, obtain potassium chloride.
Usually, mixing is produced water to be evaporated after crystallization, the first mixed slurry, the first mixed slurry Jing solid-liquids can be produced
Separate, obtain rich potassium evaporation mother solution and wet potassium chloride；Wherein, in rich potassium evaporation mother solution, K+Concentration be 90g/L～100g/L,
Mg2+Concentration be 30g/L～40g/L, SO4 2-Concentration be 90g/L～100g/L.
Preferably, it is molten that the water and rich potassium evaporation mother solution for producing in product water evaporation crystallization process is mixed is incorporated to kainite
In liquid.
Wet potassium chloride Jing water washings are refined, that is, obtain potassium chloride.The total recovery of KCl is 90%～95%.
Preferably, wash during refining wet potassium chloride, the rich potassium of generation washs mother liquor fraction, and to be incorporated to kainite molten
In liquid, partly it is incorporated to mixing and produces in water, be evaporated crystallization again.
Q5, process two-stage nitration concentrated water, obtain magnesium sulfate.
Specifically, crystallization is evaporated to two-stage nitration concentrated water, obtains the second mixed slurry, the second mixed slurry Jing solid-liquids point
From the wet magnesium sulfate of acquisition evaporates mother solution with rich magnesium；Wherein, in rich magnesium evaporation mother solution, MgSO4Concentration be 300g/L～330g/
The concentration of L, KCl is 40g/L～45g/L.
Simultaneously rich magnesium evaporation mother solution is incorporated in kainite solution.
Preferably, it is molten that the water and rich magnesium evaporation mother solution for producing in two-stage nitration concentrated water evaporation and crystal process is incorporated to kainite
In liquid, using the solvent as kainite, fresh water usage amount is reduced.
Wet magnesium sulfate Jing water washings are refined, that is, obtain magnesium sulfate.MgSO4Purity reach 92%～95%.
Preferably, wash during refining wet magnesium sulfate, the rich magnesium of generation washs mother liquor fraction, and to be incorporated to kainite molten
In liquid, partly it is incorporated in the secondary concentrated water for carrying out evaporative crystallization, is evaporated crystallization again.
In two-stage nitration concentrated water, the high price ion concentration such as magnesium, sulfate radical is higher, using part concentrated water outer circulation, returns it to potassium
The relative scale of magnesium salt in kainite solution in salt magnesium alum solution, can be increased, so as to further in one section of nano-filtration step
Improve the nanofiltration separation efficiency of the monovalent ions such as high valence ion and potassium, sodium such as magnesium, sulfate radical.
What deserves to be explained is, in above-mentioned steps Q4 and Q5, the conventional evaporation mode of twice evaporation crystallization is solar energy salt
Pond, forced evaporation or reverse osmosiss combine forced evaporation etc.；Wherein the mode in solar energy salt pond can make full use of abundant solar energy
Resource, but recycle-water resource capability is limited；Forced evaporation, reverse osmosiss can realize substantial amounts of fresh water with reference to the mode of forced evaporation
Recycle, but certain energy consumption need to be consumed.During water and two-stage nitration product water are produced due to one section, total dissolved solid (abbreviation TDS) is relative
It is higher, therefore when the mode of forced evaporation is combined from reverse osmosiss, the preferred seawater reverse osmosis membrane of reverse-osmosis membrane element therein
Element, to improve the response rate of fresh water.
The concentration of the liquid in each stage and separating effect in the present embodiment are listed below by way of table 1, to illustrate according to this
Bright utilization kainite prepares the beneficial effect of the method for potassium chloride and magnesium sulfate.
The liquid composition in 1 each stage of table and separating effect
The composition of kainite solution in 2 step Q1 of table
Each liquid composition in 3 step Q2 of table
Each liquid composition in 4 step Q3 of table
The composition for producing water is mixed in 5 step Q4 of table
With reference to table 3 and table 4, from table 1 it follows that kainite solution is through continuous two sections of nanofiltration separations, KCl's
Total transmitance is 88%～98%, MgSO4Total rejection be 92%～97%；Thus, in kainite the monovalence such as potassium, chlorine from
The high valence ion such as son and magnesium, sulfate radical obtains excellent separating effect.
Adopt nanofiltration skill with preparing the method innovation of potassium chloride and magnesium sulfate according to the utilization kainite of the present embodiment
Art, on the premise of without any other salt raw material, realizes that kainite produces high-quality potassium chloride and sulphuric acid magnesium products, tool
Have the advantages that process condition is gentle, separating effect is excellent, other components influences are little, product purity is high, high income；Meanwhile,
Technological process is simple, reasonable, and equipment is easy to configure, clean, install and shift, easily popularization and application.
Although illustrating and describing the present invention with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case of without departing from the spirit and scope of the present invention limited by claim and its equivalent, can here carry out form and
Various change in details.
Claims (10)
1. a kind of method that utilization kainite prepares potassium chloride and magnesium sulfate, it is characterised in that including step：
The kainite is dissolved in water, kainite solution is obtained；
One section of nano-filtration step：One section of nanofiltration is carried out using nanofiltration membrane system to process to the kainite solution, one section of acquisition is dense
Water and one section of product water；Wherein, the nanofiltration membrane system includes the first nanofiltration membrane component and is connected to the first NF membrane group
The first concentrated water case on part and first produces water tank；One section of concentrated water is stored in the first concentrated water case, one section of product water
It is stored in described first to produce in water tank；
Water is produced to described one section and is evaporated crystallization, obtain the potassium chloride；
Crystallization is evaporated to one section of concentrated water, obtains the magnesium sulfate.
2. method according to claim 1, it is characterised in that the nanofiltration membrane system also includes that being arranged on described first receives
The first booster pump before filter membrane component.
3. method according to claim 2, it is characterised in that the pressure of first booster pump be 0.6MPa～
1.5MPa。
4. according to the arbitrary described method of claim 1-3, it is characterised in that the nanofiltration membrane system is concentrated water internal-circulation type film
System.
5. a kind of method that utilization kainite prepares potassium chloride and magnesium sulfate, it is characterised in that including step：
The kainite is dissolved in water, kainite solution is obtained；
One section of nano-filtration step：One section of nanofiltration is carried out using nanofiltration membrane system to process to the kainite solution, one section of acquisition is dense
Water and one section of product water；Wherein, the nanofiltration membrane system includes the first nanofiltration membrane component and is connected to the first NF membrane group
The first concentrated water case on part and first produces water tank；One section of concentrated water is stored in the first concentrated water case, one section of product water
It is stored in described first to produce in water tank；
Water is produced to described one section and is evaporated crystallization, obtain the potassium chloride；
Two-stage nitration nano-filtration step：The nanofiltration membrane system also include being connected to the second nanofiltration membrane component on the first concentrated water case,
And the second concentrated water case and second being connected on second nanofiltration membrane component produces water tank；Using second nanofiltration membrane component
Two-stage nitration nanofiltration process is carried out to first concentrated water, obtains two-stage nitration concentrated water and two-stage nitration produces water；The two-stage nitration concentrated water is stored in described
In second concentrated water case, the two-stage nitration produces water and is stored in the second product water tank；
Crystallization is evaporated to the two-stage nitration concentrated water, obtains the magnesium sulfate.
6. method according to claim 5, it is characterised in that the nanofiltration membrane component also includes that being arranged on described first receives
The first booster pump before filter membrane component and be arranged between the first concentrated water case and second nanofiltration membrane component
Two booster pumps.
7. method according to claim 6, it is characterised in that the pressure of first booster pump be 0.6MPa～
1.5MPa, the pressure of second booster pump is 1.2MPa～2.5MPa.
8. method according to claim 5, it is characterised in that the two-stage nitration produces water and is incorporated to described a section and produces in water.
9. according to the arbitrary described method of claim 5-8, it is characterised in that the nanofiltration membrane system is concentrated water internal-circulation type film
System.
10. method according to claim 5, it is characterised in that it is molten that the part two-stage nitration concentrated water is incorporated to the kainite
In liquid.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1542147A (en) * | 2003-04-30 | 2004-11-03 | 中国科学院青海盐湖研究所 | Nano-filtration method for separating magnesium and enriching lithium from salt lake brine |
| CN103723875A (en) * | 2013-12-31 | 2014-04-16 | 朱江 | Seawater full recycling process |
| CN106082284A (en) * | 2016-06-08 | 2016-11-09 | 北京清源创智科技有限公司 | The production method of LITHIUM BATTERY pure Lithium Carbonate |
-
2016
- 2016-11-11 CN CN201610996729.8A patent/CN106517250B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1542147A (en) * | 2003-04-30 | 2004-11-03 | 中国科学院青海盐湖研究所 | Nano-filtration method for separating magnesium and enriching lithium from salt lake brine |
| CN103723875A (en) * | 2013-12-31 | 2014-04-16 | 朱江 | Seawater full recycling process |
| CN106082284A (en) * | 2016-06-08 | 2016-11-09 | 北京清源创智科技有限公司 | The production method of LITHIUM BATTERY pure Lithium Carbonate |
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