CN110372017A - Bittern mixes the separation method that alkaline process prepares basic magnesium carbonate and its natrium potassium salt - Google Patents
Bittern mixes the separation method that alkaline process prepares basic magnesium carbonate and its natrium potassium salt Download PDFInfo
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- CN110372017A CN110372017A CN201910811955.8A CN201910811955A CN110372017A CN 110372017 A CN110372017 A CN 110372017A CN 201910811955 A CN201910811955 A CN 201910811955A CN 110372017 A CN110372017 A CN 110372017A
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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
- C01D3/06—Preparation by working up brines; seawater or spent lyes
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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
- C01D3/14—Purification
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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
- C01F5/24—Magnesium carbonates
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Abstract
The present invention is the separation method that a kind of bittern mixes that alkaline process prepares basic magnesium carbonate and its natrium potassium salt.Method includes the following steps: prepared by (one) basic carbonate magnesium crystal: bittern being added in reactor, Na is then added2CO3Solution and NaOH solution, obtain slurry；Filtering, obtains filtrate and solid；Solid dries 8~10h, obtains basic carbonate magnesium crystal；(2) equivalent CaCl is added in obtained filtrate2Solution is filtered after reaction, obtains filtrate；Isothermal evaporation crystallization, is obtained by filtration related substances；(3) in remaining mother liquor KCl and NaCl separation and Extraction.Magnesium ion is complete close to conversion after present invention reaction, realizes the efficient utilization of bittern, simplifies later separation.Bittern is reacted with mixed alkali, and bicarbonate ion-containing, simplified reaction post mother liquor composition do not reduce the difficulty of later separation in reaction post mother liquor.
Description
Technical field
The present invention relates to a kind of separation of new method and subsequent mother liquor using mixed alkaline process synthesis basic magnesium carbonate.
Background technique
Mother liquor after seawater solar evaporation salt manufacturing is known as bittern, contains the inorganic salts such as a large amount of sodium, magnesium, potassium in mother liquor, is
Valuable resource treasure-house, annual 20000000 m of by-product bittern in China3, but the utilization rate of bittern is less than 20%, a large amount of bittern
Resource is discharged into sea or recycles in salt pan, not only caused the waste of resource but also affect the ecological balance of offshore sea waters.So bitter
The high-efficiency comprehensive utilization of halogen resource is always to be worth the project of explore and study.
Contain a large amount of magnesium salts in bittern, converts magnesium hydroxide (Tai C Y, Tai C T, Minghui for magnesium salts
ChangA,et al.Synthesis of Magnesium Hydroxide and Oxide Nanoparticles Using a
Spinning Disk Reactor[J].Industrial&Engineering Chemistry Research,2007,46
(17): 5536-5541.), basic magnesium carbonate (Ohkubo T, Suzuki S, Mitsuhashi K, et al.Preparation
of petaloid microspheres of basic magnesium carbonate[J].Langmuir,2007,23
(11): 5872-5874.), alkali magnesium sulfate (MiY, Chen J, SongY.Research on the preparation
ofbasic magnesium sulfate whisker with organic acid by hydrothermal method
[J] .Inorganic Chemicals Inoustry, 2007.) etc. the value of magnesium resource had not only can be improved in inorganic material product, but also
The separation for being conducive to other salt in bittern is the new way of bittern high-efficiency comprehensive utilization.But in actual production, due to magnesium salts
The magnesium hydroxide of precipitating is a kind of superfine colloidal powder-product, is separated by filtration extremely difficult, industrial industry difficult to realize
Change.For basic magnesium carbonate as magnesium salts fire retardant, performance is better than magnesium hydroxide, and also acts as paint, ink, coating, food
Additive and modifying agent of product and various chemical products etc. use.At present with Mg (NO3)2、MgSO4、MgCl2Equal chemical reagent are
Raw material, by with Na2CO3、NaHCO3、NH3·H2The alkali substance reactions such as O, which prepare basic magnesium carbonate, many document reports
Road, but these researchs is concerned with product appearance structure, and to feed stock conversion and reaction post mother liquor composition and how again
Utilize seldom research.Using bittern as raw material, Na2CO3Basic carbonate magnesium crystal is prepared as precipitating reagent, in recent years Zhang Shihang
(Zhang S.Preparation of Basic Magnesium Carbonate and Magnesium Oxide from
Mother Liquor of Salt Production[J].Shandong Chemical Industry,2017.)Wu Jiansong
(Wu Jiansong, Liang Haiqun, the Huang Xue clear Xuwen saltern bittern prepare Mg2(OH)2CO3·3H2O whisker [J] artificial lens journal,
2015,44 (6): 1713-1717.) Qi Hongbo (Qi H, Yang W.Production process of light
transparent basic magnesium carbonate[J].Inorganic Chemicals Industry,2008.)
Et al. studied respectively, although these documents discuss the conversion ratio of magnesium ion in raw material, but without investigating Na2CO3's
Conversion ratio, brine used are the bittern after dilution, and oxide spinel na concn is lower, and without research making from brine for basic carbonate
After magnesium, remaining mother liquor is formed and its how to be utilized, and for instructing actual production, there are also a certain distance for research work.
In view of the above analysis, it is contemplated that bittern or sea-air blowout method mention bromine technology (Guo-HuaH E, Chen Q
R.Effect of Bromine Production in Brine by Air Blowing method on Seasalt
Production [J] .Journal of Salt&Chemical Industry, 2016.) mature and industrialize, the present invention
Patent is simulation bittern with not brominated practical bittern, around raising raw material magnesium ion and Na2CO3Conversion ratio simplifies synthetic alkali formula
For the purpose of the separate design of magnesium carbonate post mother liquor composition and its subsequent sodium salt and sylvite, not brominated bittern and sodium carbonate and hydrogen are proposed
Sodium oxide molybdena mixed liquor reaction prepares the technique that basic magnesium carbonate and its remaining mother liquor sodium salt are separated with sylvite.
Summary of the invention:
Object of the present invention is to more difficult for the utilization of resources of China's bittern, and the enrichment of bittern coastal waters domain leads to marine ecology ring
The problems such as border is destroyed provides one kind and efficiently utilizes Mg in bittern2+Method, and design separation utilize residual ion technique stream
Journey.This method mixes alkali reaction by the bittern, sodium carbonate and sodium hydroxide of high concentration, passes through appropriate carbanion, hydrogen-oxygen
The proportion of magnesium ion in radical ion and bittern, realize simplify synthesis basic magnesium carbonate post mother liquor composition and its subsequent sodium salt with
The separation of sylvite.
The technical solution of the present invention is as follows:
A kind of mixed alkaline process of bittern prepares the separation method of basic magnesium carbonate and its natrium potassium salt, the following steps are included:
(1) prepared by basic carbonate magnesium crystal
(1) bittern is added in reactor, Na is then added2CO3Solution and NaOH solution, obtain mixed liquor, and 60~80
After being stirred to react 120s at DEG C, then 2.5~4.5h is stood, obtains slurry；
Wherein, bittern composition includes: MgCl2: 150~180gL-1；NaCl:60~110gL-1；KCl:18
~22gL-1；MgSO4: 60~75gL-1；The Na2CO3The concentration of solution is 2.0~2.5molL-1；NaOH solution
Concentration be 2.5~3molL-1；Molar ratio Mg in mixed liquor2+:CO3 2-:OH-=5:4.8:1.9~2.1；
(2) gained slurry in (1) step is filtered, obtains filtrate and solid；And solid is washed with deionized into
Property；
(3) dry: the solid after the washing of (2) step being dried into 8~10h at 100~110 DEG C, obtains basic magnesium carbonate crystalline substance
Body；
(2) NaCl and Na in basic carbonate magnesium crystal preparation post mother liquor2SO4·10H2O is extracted
(4) 0.3~0.5molL is added in obtained filtrate into (2) step-1CaCl2Solution carried out after reaction
Filter, obtains filtrate；Wherein, CO in filtrate3 2-With CaCl2Ca in solution+Equivalent；
(5) to filtrate isothermal evaporation under the conditions of 25 DEG C is obtained in step (4), every 1000g filtrate evaporates 571.4~588.8g
NaCl is precipitated in water, crystallization, stops evaporation, filters out NaCl；Filtrate is cooled to 0 DEG C again, and reduces moisture 114.0-119.0g
After stop, filtering out Na2SO4·10H2O；Continue for residual filtrate to be warming up to 25 DEG C of isothermal evaporations, evaporates 33.9-35.4g moisture
Afterwards, stop evaporation, filter out NaCl；Remaining mother liquor is finally cooled to 0 DEG C, is stopped when moisture reduces 24.70-25.78g, mistake
Filter out Na2SO4·10H2O；
(3) in remaining mother liquor KCl and NaCl separation and Extraction
(6) 0.3~0.5molL is added into (5) step finally obtained filtrate-1BaCl2Solution carries out after reaction
Filtering；(5) the last SO in obtained filtrate of step4 2-With BaCl2The Ba of solution+Equivalent；
(7) NaCl is precipitated in 100 DEG C of isothermal evaporations of gained filtrate in step (6), and every 1000g filtrate evaporates 649.9-661.1g
NaCl is precipitated in water, crystallization, stops evaporation, filters out the NaCl of 56.96-70.89g；Remaining mother liquor is cooled to 25 DEG C again, is precipitated
After solid, the KCl of 29.23-29.96g is filtered out；NaCl, evaporation water is precipitated in 100 DEG C of isothermal evaporations in obtained filtrate
83.72-85.23g stopping evaporation, the NaCl of 22.41-22.86g is filtered out；Remaining mother liquor is cooled to 25 DEG C again, is precipitated solid
After body, the KCl of 14.15-14.44g is filtered out；Obtained remaining mother liquor repeat 1~3 time " 100 DEG C of isothermal evaporations analyse sodium chloride,
The process of 25 DEG C of analysis potassium chloride is cooled to again " so that sodium chloride, potassium chloride amount of precipitation are stopped when respectively reaching 97% and 93% or more
Only.
Substantive distinguishing features of the invention are as follows:
(1) bittern mixes alkali with sodium carbonate and sodium hydroxide and reacts, and alkali concentration and bittern concentration are higher, magnesium ion after reaction
Completely close to conversion, it realizes the efficient utilization of bittern, simplifies later separation.(2) bittern is reacted with mixed alkali, is reacted in post mother liquor not
Bicarbonate ion-containing simplifies reaction post mother liquor composition, reduces the difficulty of later separation.(3) present invention devises set of system
Technique, realize recycling for bittern, realize being kept completely separate for the elements such as sodium in mother liquor, potassium.
During preparing basic magnesium carbonate, due to the proportion of the magnesium ion in carbanion, hydroxide ion and bittern
The presence of bicarbonate ion in the conversion ratio and solution of magnesium ion is affected, therefore is the key factor of experiment.
Beneficial effects of the present invention:
The present invention is with the bittern of high concentration and sodium carbonate, sodium hydroxide reaction, raw glomerate basic carbonate magnesium crystal.It should
Method Mg2+Conversion ratio reach approximately 100%, lay the foundation for subsequent mother liquor separation, and shorten the reaction time, there is technique letter
It is single, it is easy to accomplish industrialization, economic advantages outstanding feature.Furthermore HCO is free of in remaining mother liquor3 -, significantly reduce mother liquor point
From difficulty, while the separating technology process of remaining mother liquor has also been devised in this experiment, improves the utilization rate of bittern, favorably avoids
Problem of environmental pollution caused by the enrichment of bittern coastal waters domain.
Above-mentioned beneficial effect is embodied in:
(1) basic magnesium carbonate of precipitation method production for a long time is mostly the reactant of low concentration, the reactant meeting of low concentration
Lead to react that post mother liquor concentration is too low, and repetition evaporates brine and evaporates the process of water, increases on the energy and temporal waste.This experiment
The bittern used is undiluted bittern, and the sodium carbonate and sodium hydroxide used similarly are high concentrations, and is reacted before
Object concentration compared to improve 50% or so, the present invention it is subsequent can reduce 50% or so evaporated water, economic advantages are significant, more accord with
Factory's practical operation is closed, is laid the foundation for later separation.
(2) basic magnesium carbonate of precipitation method production for a long time uses sodium carbonate as precipitating reagent mostly, but magnesium after reacting
The conversion ratio of ion is not high, and after reaction, there is bicarbonate ion residue in mother liquor, so that the solution separation after reaction
It complicates.This experiment mixes alkali reaction using bittern and sodium carbonate, sodium hydroxide and generates basic carbonate magnesium crystal, the conversion of magnesium ion
Rate close to 100% than before using sodium carbonate as precipitating reagent when magnesium ion conversion ratio improve 2%.Reaction time shortens than before
50% or so, and react and do not contain HCO in post mother liquor3 -Ion provides convenience for later separation,
(3) later-stage utilization of bittern is paid attention to by domestic and international all the time, is not yet reported that later separation so far
Method, remaining mother liquor it is random stacking will lead to coastal waters domain ecological environment destruction.After this experiment magnesium sinking, later period solution is used
Precipitating -- phasor separation -- reprecipitation -- method that phasor separates again separates each substance, and resource is made to obtain rational utilization,
The appearance for the problems such as avoiding the wasting of resources and marine eco-environment destruction.
Detailed description of the invention
Fig. 1 is process flow chart.
Fig. 2 is K+,Na+//Cl-,SO4 2--H2O quaternary system phasor.
Fig. 3 is NaCl-KCl-H2O ternary system phasor.
Fig. 4 is the SEM figure of product in embodiment 1.
Fig. 5 is the SEM figure of product in embodiment 2.
Fig. 6 is the SEM figure of product in embodiment 3.
Fig. 7 is the SEM figure of product in embodiment 4.
Fig. 8 is the SEM figure of product in embodiment 5.
Fig. 9 is the SEM figure of product in embodiment 6.
Specific embodiment:
Fig. 1 is the separating technology flow chart that bittern mixes that alkaline process prepares basic magnesium carbonate and its natrium potassium salt.
Fig. 2 is K+,Na+//Cl-,SO4 2--H2O quarternary phase diagram, wherein coordinate unit be Ye Neike index, abscissa:
100*2Cl/(2Cl-+SO4 2-), ordinate: 100*Na+/(Na++K+).EFGHB is the crystal region of NaCl, EFPN in 25 DEG C of phasors
For Na2SO4·10H2The crystal region of O, OPFGRQ are GLa (NaSO4·3K2SO4) crystal region.AMLKJSI is in 0 DEG C of phasor
Na2SO4·10H2The crystal region of O, ISUB are the crystal region of NaCl, LKJWV 3K2SO4·Na2SO4Crystal region.
Evaporating principle is as follows: after bittern magnesium sinking removes carbanion, system point is a point in Fig. 2, and a point has fallen in 25 DEG C
When quaternary system phasor the crystal region NaCl in, therefore the 25 DEG C of isothermal evaporation dehydrations of a mother liquor have NaCl precipitation, be precipitated NaCl after liquid
Phase point will be moved along Ba extended line direction, when liquidus point reaches the intersection point b of Ba extended line and EF line, Na2SO4Also reach full
With re-evaporation moisture will will appear Na2SO4With NaCl eutectoid, stop evaporation at this time.After solid phase NaCl is precipitated in separation, mother liquor b is fallen
The K at 0 DEG C+,Na+//Cl-,SO4 2--H2The Na of O phasor2SO4·10H2In the crystal region O, pass through the moisture of volatilization adjustment mother liquor b
And 0 DEG C is cooled to, Na can be made2SO4·10H2O crystallization is precipitated, and liquidus point reaches the intersection point c point of Ab extended line Yu IS line just, point
Isolate Na2SO4·10H2After O solid phase, mother liquor c point and the K when having fallen in 25 DEG C+,Na+//Cl-,SO4 2--H2O quaternary system is dry
In the crystal region NaCl of salt figure.Carry out 25 DEG C of isothermal evaporation dehydrations again to mother liquor c, it will have NaCl precipitation, after NaCl is precipitated
Liquidus point reaches the intersection point d point of Bc line extended line and FG line, after NaCl is precipitated in separation, K mother liquor d point has fallen in 0 DEG C again when+,Na+//Cl-,SO4 2--H2The Na of O phasor2SO4·10H2In the crystal region O, in this temperature isothermal volatilization moisture, there is Na2SO4·10H2O
Solid separation, liquidus point reach the intersection point e point of Ad extended line Yu JK line just, and NaCl's and KCl is total to when due to e point close to 25 DEG C
Full line GH, therefore stop evaporation.
NaCl-KCl-H when Fig. 3 is 100 DEG C and 25 DEG C2The dry salt figure of O ternary system is as shown in Figure 3.BMO is in 25 DEG C of phasors
The crystal region of NaCl, AMN are the crystal region KCl, and ABM is the crystal region NaCl and KCl.BEI is the crystallization of NaCl in 100 DEG C of phasors
Area, AEK are the crystal region KCl, and ABE is the crystal region NaCl and KCl.
(Fig. 2,3 are well-known technique, are seen: Stephen H, Stephen T.Solubilities ofinorganic and
organic compounds/editedby H.Stephen and T.Stephen[M].Pergamon Press,1963.)
Evaporating principle is as follows: most Na is isolated by step two2SO4·10H2After O and NaCl, removed with barium chloride surplus
After remaining sulfate radical, system point is the point m in Fig. 3, and at phasor midpoint, m has been fallen in 100 DEG C of regions IEKW, indicates that point m is not
Saturation point.NaCl is precipitated in 100 DEG C of isothermal evaporations of the first step, and system point is moved on the intersection point F of BE and Wm by m, liquidus point E,
Total saturation point E has been fallen in simultaneously in 25 DEG C of crystal regions KCl；Point E is cooled to 25 DEG C by second step, and E point is system point at this time, is precipitated
KCl, liquidus point are point D.This is for 100 DEG C of NaCl-KCl-H as can be seen from Figure2For O ternary system phasor, D point is not
NaCl is precipitated in saturation point, 100 DEG C of isothermal evaporations of third step, and system point is moved on the intersection point H of point BE and WD by point D, liquidus point
For point E.4th two or three steps of multiplicating, until by NaCl and KCl completely separable.
The raw material that the present invention is said are the liquid after seawater is evaporated brine, the composition of this liquid are as follows: MgCl2: 150~180g
L-1；NaCl:60~110gL-1；KCl:18~22gL-1；MgSO4: 60~75gL-1、Br:6.5-8.0g·L-1.Pass through
Air blows out method for after the removing of a small amount of bromide ion, and obtained bittern group becomes MgCl2: 150~180gL-1；NaCl:60~
110g·L-1；KCl:18~22gL-1；MgSO4: 60~75gL-1。
Embodiment 1: concrete operations are as follows:
One, prepared by basic carbonate magnesium crystal
Bittern raw material used in the present invention basic composition is: MgCl2: 165gL-1；NaCl:85gL-1；KCl:20g
L-1；MgSO4: 67.5gL-1。
(1) it takes bittern 250ml to be placed in 500ml three neck round bottom flask, and is placed in 60 DEG C of water-baths, company stirs
Device is mixed, 2.5molL is added to the inside-1Na2CO3And 3molL-1NaOH, guarantee Mg2+:CO3 2-:OH-Mol ratio
For 5:4.8:2, after being stirred to react 120s, 2.5h is stood, slurry is obtained.
(2) gained slurry in (1) step is filtered, obtains 533.5g filtrate and 52.8g solid, and with deionized water into
Row washing solid to neutrality, filtrate quality forms are as follows: Na+: 7.29%；K+: 0.49%；Cl-: 8.64%；SO4 2-: 2.53%；
CO3 2-: 0.99%；H2O:80.06%.
(3) dry: the solid product that (2) step obtains being dried into 8h at 110 DEG C, obtains basic carbonate magnesium crystal, product
SEM figure see Fig. 4, be spheric granules.
Two, NaCl and Na in basic carbonate magnesium crystal preparation post mother liquor2SO4·10H2O is extracted
(4) it is added in obtained filtrate into (2) step and CO in filtrate3 2-The 0.5molL of equivalent-1CaCl2It is molten
Liquid, by CO in mother liquor3 2-It completely removes, is filtered after reaction, obtain 704.9g mother liquor, quality group becomes: Na+:
5.52%；K+: 0.37%；Cl-: 7.43%；SO4 2-: 1.92%；H2O:84.76%.
(5) gained 704.9g filtrate isothermal evaporation under the conditions of 25 DEG C in step (4) after steaming 410.0g water, stops evaporation, mistake
Filter out NaCl；Filtrate is cooled to 0 DEG C, stops after moisture reduces 81.7g, filters out Na2SO4·10H2O；By residual filtrate
25 DEG C of isothermal evaporations are warming up to, after evaporating 24.3g water, stops evaporation, filters out NaCl；Remaining mother liquor is cooled to 0 DEG C, works as water
Divide after reducing 17.7g and stop, filtering out Na2SO4·10H2O；Filtrate 54.8g is obtained, quality group becomes: Na+: 6.75%；K+:
4.74%；Cl-: 13.50%；SO4 2-: 1.64%；H2O:73.37%.
Three, in remaining mother liquor KCl and NaCl separation and Extraction
(6) it is added into (5) step finally obtained filtrate and SO in filtrate4 2-The 0.3molL of equivalent-1BaCl2
Solution, by the SO in mother liquor4 2-It completely removes, is filtered after reaction, obtain filtrate 84.8g, quality group becomes: Na+:
4.36%；K+: 3.07%；Cl-: 9.55%；H2O:83.02%.
(7) 100 DEG C of isothermal evaporation 55.9g moisture of gained 84.8g filtrate (mother liquor forms m in Fig. 3) in step (6), are precipitated
After 5.78g solid, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, 2.5g is precipitated
After solid, KCl is filtered out；Again by 100 DEG C of isothermal evaporation 7.1g moisture of obtained 20.6g filtrate (mother liquor forms D in Fig. 3), analysis
Out after 1.9g solid, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, is precipitated
After 1.2g solid, KCl is filtered out.Obtained 10.42g residue mother liquor (mother liquor forms D in Fig. 3) repeats 100 DEG C of isothermal evaporation analysis
Sodium chloride 0.97g out, then cool to 25 DEG C of precipitation potassium chloride 0.66g.Obtaining 5.67g residue mother liquor again, (mother liquor forms in Fig. 3
D 100 DEG C of isothermal evaporations) are repeated and analyse sodium chloride 0.52g, then cool to 25 DEG C of precipitation potassium chloride 0.34g.It is recycled by four times, it can
So that sodium chloride amount of precipitation reaches stopping when 97.45%, potassium chloride amount of precipitation reaches 94.00%.
Embodiment 2: concrete operations are as follows:
One, prepared by basic carbonate magnesium crystal
Bittern raw material used in the present invention basic composition is: MgCl2: 165gL-1；NaCl:85gL-1；KCl:20g
L-1；MgSO4: 67.5gL-1。
(1) it takes bittern 250ml to be placed in 500ml three neck round bottom flask, and is placed in 60 DEG C of water-baths, company stirs
Device is mixed, 2.5molL is added to the inside-1Na2CO3And 3molL-1NaOH, guarantee Mg2+:CO3 2-:OH-Mol ratio
For 5:4.8:1.9, after being stirred to react 120s, 2.5h is stood, slurry is obtained.
(2) gained slurry in (1) step is filtered, obtains 531.3g filtrate and 50.5g solid, and with deionized water into
Row washing solid to neutrality, filtrate quality forms are as follows: Na+: 7.25%；K+: 0.49%；Cl-: 8.68%；SO4 2-: 2.54%；
CO3 2-: 0.90%；H2O:80.14%
(3) dry: the solid product that (2) step obtains being dried into 10h at 100 DEG C, obtains basic carbonate magnesium crystal, product
SEM figure see Fig. 5, be spheric granules.
Two, NaCl and Na in basic carbonate magnesium crystal preparation post mother liquor2SO4·10H2O is extracted
(4) it is added in obtained filtrate into (2) step and CO in filtrate3 2-The 0.5molL of equivalent-1CaCl2It is molten
Liquid, by CO in mother liquor3 2-It completely removes, is filtered after reaction, obtain 686.5g mother liquor, quality group becomes: Na+:
5.61%；K+: 0.38%；Cl-: 7.55%；SO4 2-: 1.97%；H2O:84.49%.
(5) gained 686.5g filtrate isothermal evaporation under the conditions of 25 DEG C in step (4) after steaming 392.3g water, stops evaporation, mistake
Filter out NaCl；Filtrate is cooled to 0 DEG C, stops after moisture reduces 81.7g, filters out Na2SO4·10H2O；By residual filtrate
25 DEG C of isothermal evaporations are warming up to, after evaporating 24.3g water, stops evaporation, filters out NaCl；Remaining mother liquor is cooled to 0 DEG C, works as water
Divide after reducing 17.7g and stop, filtering out Na2SO4·10H2O；Filtrate 54.1g is obtained, quality group becomes: Na+: 6.10%；K+:
4.81%；Cl-: 12.62%；SO4 2-: 1.66%；H2O:74.81%
Three, in remaining mother liquor KCl and NaCl separation and Extraction
(6) it is added into (5) step finally obtained filtrate and SO in filtrate4 2-The 0.3molL of equivalent-1BaCl2
Solution, by the SO in mother liquor4 2-It completely removes, is filtered after reaction, obtain filtrate 84.1g, quality group becomes: Na+:
3.92%；K+: 3.09%；Cl-: 8.92%；H2O:84.07%.
(7) 100 DEG C of isothermal evaporation 55.0g moisture of gained 84.1g filtrate (mother liquor forms m in Fig. 3) in step (6), are precipitated
After 4.79g solid, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, is precipitated
After 2.51g solid, KCl is filtered out.Again by 100 DEG C of isothermal evaporation 7.1g water of obtained 21.8g filtrate (mother liquor forms D in Fig. 3)
Point, after 1.9g solid is precipitated, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, analysis
Out after 1.2g solid, KCl is filtered out.Obtained 11.6g residue mother liquor (mother liquor forms D in Fig. 3) repeats 100 DEG C of isothermal evaporation analysis
Sodium chloride 0.97g out, then cool to 25 DEG C of precipitation potassium chloride 0.66g.Obtaining 6.67g residue mother liquor again, (mother liquor forms in Fig. 3
D 100 DEG C of isothermal evaporations) are repeated and analyse sodium chloride 0.52g, then cool to 25 DEG C of precipitation potassium chloride 0.34g.It is recycled by four times, it can
So that sodium chloride amount of precipitation reaches 97.50%, stopping when potassium chloride amount of precipitation reaches 94.15%.
Embodiment 3: concrete operations are as follows:
One, prepared by basic carbonate magnesium crystal
Bittern raw material used in the present invention basic composition is: MgCl2: 165gL-1；NaCl:85gL-1；KCl:20g
L-1；MgSO4: 67.5gL-1。
(1) it takes bittern 250ml to be placed in 500ml three neck round bottom flask, and is placed in 60 DEG C of water-baths, company stirs
Device is mixed, 2.5molL is added to the inside-1Na2CO3And 3molL-1NaOH, guarantee Mg2+:CO3 2-:OH-Mol ratio
For 5:4.8:2.1, after being stirred to react 120s, 2.5h is stood, slurry is obtained.
(2) gained slurry in (1) step is filtered, obtains 538.7g filtrate and 52.8g solid, and with deionized water into
Row washing solid to neutrality, filtrate quality forms are as follows: Na+: 7.24%；K+: 0.48%；Cl-: 8.56%；SO4 2-: 2.51%；
CO3 2-: 1.02%；H2O:80.19%.
(3) dry: the solid product that (2) step obtains being dried into 9h at 105 DEG C, obtains basic carbonate magnesium crystal, product
SEM figure see Fig. 6, be spheric granules.
Two, NaCl and Na in basic carbonate magnesium crystal preparation post mother liquor2SO4·10H2O is extracted
(4) it is added in obtained filtrate into (2) step and CO in filtrate3 2-The 0.5molL of equivalent-1CaCl2It is molten
Liquid, by CO in mother liquor3 2-It completely removes, is filtered after reaction, obtain 716.5g mother liquor, quality group becomes: Na+:
5.44%；K+: 0.36%；Cl-: 7.34%；SO4 2-: 1.88%；H2O:84.98%.
(5) gained 716.5g filtrate isothermal evaporation under the conditions of 25 DEG C in step (4) after steaming 421.9g water, stops evaporation, mistake
Filter out NaCl；Filtrate is cooled to 0 DEG C, stops after moisture reduces 81.7g, filters out Na2SO4·10H2O；By residual filtrate
25 DEG C of isothermal evaporations are warming up to, after evaporating 24.3g water, stops evaporation, filters out NaCl；Remaining mother liquor is cooled to 0 DEG C, works as water
Divide after reducing 17.7g and stop, filtering out Na2SO4·10H2O；Filtrate 54.5g is obtained, quality group becomes: Na+: 6.97%；K+:
4.77%；Cl-: 13.87%；SO4 2-: 1.65%；H2O:72.74%.
Three, in remaining mother liquor KCl and NaCl separation and Extraction
(6) it is added into (5) step finally obtained filtrate and SO in filtrate4 2-The 0.3molL of equivalent-1BaCl2
Solution, by the SO in mother liquor4 2-It completely removes, is filtered after reaction, obtain filtrate 84.5g, quality group becomes: Na+:
4.50%；K+: 3.08%；Cl-: 9.70%；H2O:82.72%.
(7) 100 DEG C of isothermal evaporation 55.41g moisture of gained 84.5g filtrate (mother liquor forms m in Fig. 3) in step (6), are precipitated
After 5.99g solid, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, is precipitated
After 2.47g solid, KCl is filtered out.Again by 100 DEG C of isothermal evaporation 7.1g water of obtained 20.63g filtrate (mother liquor forms D in Fig. 3)
Point, after 1.9g solid is precipitated, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, analysis
Out after 1.2g solid, KCl is filtered out.Obtained 10.43g residue mother liquor (mother liquor forms D in Fig. 3) repeats 100 DEG C of isothermal evaporations
Sodium chloride 0.97g is analysed, then cools to 25 DEG C of precipitation potassium chloride 0.66g.Obtaining 5.7g residue mother liquor again, (mother liquor forms in Fig. 3
D 100 DEG C of isothermal evaporations) are repeated and analyse sodium chloride 0.52g, then cool to 25 DEG C of precipitation potassium chloride 0.34g.It is recycled by four times, it can
So that sodium chloride amount of precipitation reaches stopping when 97.00%, potassium chloride amount of precipitation reaches 93.96%.
Embodiment 4: concrete operations are as follows:
One, prepared by basic carbonate magnesium crystal
Bittern raw material used in the present invention basic composition is: MgCl2: 165gL-1；NaCl:85gL-1；KCl:20g
L-1；MgSO4: 67.5gL-1。
(1) it takes bittern 250ml to be placed in 250ml three neck round bottom flask, and is placed in 60 DEG C of water-baths, company stirs
Device is mixed, 2.5molL is added to the inside-1Na2CO3And 3molL-1NaOH, guarantee Mg2+:CO3 2-:OH-Mol ratio
For 5:4.8:2, after being stirred to react 120s, 3h is stood, slurry is obtained.
(2) gained slurry in (1) step is filtered, obtains 533.5g filtrate and 52.8g solid, and with deionized water into
Row washing solid to neutrality, filtrate quality forms are as follows: Na+: 7.27%；K+: 0.49%；Cl-: 8.64%；SO4 2-: 2.53%；
CO3 2-: 0.99%；H2O:80.08%.
(3) dry: the solid product that (2) step obtains being dried into 8h at 110 DEG C, obtains basic carbonate magnesium crystal, product
SEM figure see Fig. 7, be spheric granules.
Two, NaCl and Na in basic carbonate magnesium crystal preparation post mother liquor2SO4·10H2O is extracted
(4) it is added in obtained filtrate into (2) step and CO in filtrate3 2-The 0.5molL of equivalent-1CaCl2It is molten
Liquid, by CO in mother liquor3 2-It completely removes, is filtered after reaction, obtain 704.9g mother liquor, quality group becomes: Na+:
5.50%；K+: 0.37%；Cl-: 7.43%；SO4 2-: 1.92%；H2O:84.78%.
(5) gained 704.9g filtrate isothermal evaporation under the conditions of 25 DEG C in step (4) after steaming 411.5g water, stops evaporation, mistake
Filter out NaCl；Filtrate is cooled to 0 DEG C, stops after moisture reduces 81.7g, filters out Na2SO4·10H2O；By residual filtrate
25 DEG C of isothermal evaporations are warming up to, after evaporating 24.3g water, stops evaporation, filters out NaCl；Remaining mother liquor is cooled to 0 DEG C, works as water
Divide after reducing 17.7g and stop, filtering out Na2SO4·10H2O；Filtrate 53.3g is obtained, quality group becomes: Na+: 6.94%；K+:
4.88%；Cl-: 13.94%；SO4 2-: 1.69%；H2O:72.55%.
Three, in remaining mother liquor KCl and NaCl separation and Extraction
(6) it is added into (5) step finally obtained filtrate and SO in filtrate4 2-The 0.3molL of equivalent-1BaCl2
Solution, by the SO in mother liquor4 2-It completely removes, is filtered after reaction, obtain filtrate 83.3g, quality group becomes: Na+:
4.44%；K+: 3.12%；Cl-: 9.72%；H2O:82.72%.
(7) 100 DEG C of isothermal evaporation 54.14g moisture of gained 83.3g filtrate (mother liquor forms m in Fig. 3) in step (6), are precipitated
After 5.76g solid, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, is precipitated
After 2.48g solid, KCl is filtered out.Again by 100 DEG C of isothermal evaporation 7.1g water of obtained 20.92g filtrate (mother liquor forms D in Fig. 3)
Point, after 1.9g solid is precipitated, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, analysis
Out after 1.2g solid, KCl is filtered out.Obtained 10.72g residue mother liquor (mother liquor forms D in Fig. 3) repeats 100 DEG C of isothermal evaporations
Sodium chloride 0.97g is analysed, then cools to 25 DEG C of precipitation potassium chloride 0.66g.Obtaining 5.79g residue mother liquor again, (mother liquor forms in Fig. 3
D 100 DEG C of isothermal evaporations) are repeated and analyse sodium chloride 0.52g, then cool to 25 DEG C of precipitation potassium chloride 0.34g.It is recycled by four times, it can
So that sodium chloride amount of precipitation reaches stopping when 97.24%, potassium chloride amount of precipitation reaches 93.60%.
Embodiment 5: concrete operations are as follows:
One, prepared by basic carbonate magnesium crystal
Bittern raw material used in the present invention basic composition is: MgCl2: 165gL-1；NaCl:85gL-1；KCl:20g
L-1；MgSO4: 67.5gL-1。
(1) it takes bittern 250ml to be placed in 250ml three neck round bottom flask, and is placed in 60 DEG C of water-baths, company stirs
Device is mixed, 2.5molL is added to the inside-1Na2CO3And 3molL-1NaOH, guarantee Mg2+:CO3 2-:OH-Mol ratio
For 5:4.8:2, after being stirred to react 120s, 3.5h is stood, slurry is obtained.
(2) gained slurry in (1) step is filtered, obtains 533.4g filtrate and 52.9g solid, and with deionized water into
Row washing solid to neutrality, filtrate quality forms are as follows: Na+: 7.29%；K+: 0.49%；Cl-: 8.64%；SO4 2-: 2.53%；
CO3 2-: 0.99%；H2O:80.06%.
(3) dry: the solid product that (2) step obtains being dried into 10h at 100 DEG C, obtains basic carbonate magnesium crystal, product
SEM figure see Fig. 8, be spheric granules.
Two, NaCl and Na in basic carbonate magnesium crystal preparation post mother liquor2SO4·10H2O is extracted
(4) it is added in obtained filtrate into (2) step and CO in filtrate3 2-The 0.5molL of equivalent-1CaCl2It is molten
Liquid, by CO in mother liquor3 2-It completely removes, is filtered after reaction, obtain 704.8g mother liquor, quality group becomes: Na+:
5.52%；K+: 0.37%；Cl-: 7.43%；SO4 2-: 1.92%；H2O:84.76%.
(5) gained 704.8g filtrate isothermal evaporation under the conditions of 25 DEG C in step (4) after steaming 411.6g water, stops evaporation, mistake
Filter out NaCl；Filtrate is cooled to 0 DEG C, stops after moisture reduces 81.7g, filters out Na2SO4·10H2O；By residual filtrate
25 DEG C of isothermal evaporations are warming up to, after evaporating 24.3g water, stops evaporation, filters out NaCl；Remaining mother liquor is cooled to 0 DEG C, works as water
Divide after reducing 17.7g and stop, filtering out Na2SO4·10H2O；Filtrate 53.1g is obtained, quality group becomes: Na+: 6.97%；K+:
4.90%；Cl-: 13.99%；SO4 2-: 1.69%；H2O:72.45%.
Three, in remaining mother liquor KCl and NaCl separation and Extraction
(6) it is added into (5) step finally obtained filtrate and SO in filtrate4 2-The 0.3molL of equivalent-1BaCl2
Solution, by the SO in mother liquor4 2-It completely removes, is filtered after reaction, obtain filtrate 83.1g, quality group becomes: Na+:
4.45%；K+: 3.13%；Cl-: 9.75%；H2O:82.67%.
(7) 100 DEG C of isothermal evaporation 54.94g moisture of gained 83.1g filtrate (mother liquor forms m in Fig. 3) in step (6), are precipitated
After 5.8g solid, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, 2.49g is precipitated
After solid, KCl is filtered out.Again by 100 DEG C of isothermal evaporation 7.1g moisture of obtained 19.87g filtrate (mother liquor forms D in Fig. 3), analysis
Out after 1.9g solid, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, is precipitated
After 1.2g solid, KCl is filtered out.Obtained 9.67g residue mother liquor (mother liquor forms D in Fig. 3) repeats 100 DEG C of isothermal evaporation analysis chlorine
Change sodium 0.97g, then cools to 25 DEG C of precipitation potassium chloride 0.66g.4.74g residue mother liquor (mother liquor forms D in Fig. 3) weight is obtained again
Multiple 100 DEG C of isothermal evaporations analyse sodium chloride 0.52g, then cool to 25 DEG C of precipitation potassium chloride 0.34g.It is recycled, be may make by four times
Sodium chloride amount of precipitation reaches stopping when 97.66%, potassium chloride amount of precipitation reaches 94.37%.
Embodiment 6: concrete operations are as follows:
One, prepared by basic carbonate magnesium crystal
Bittern raw material used in the present invention basic composition is: MgCl2: 165gL-1；NaCl:85gL-1；KCl:20g
L-1；MgSO4: 67.5gL-1。
(1) it takes bittern 250ml to be placed in 250ml three neck round bottom flask, and is placed in 60 DEG C of water-baths, company stirs
Device is mixed, 2.5molL is added to the inside-1Na2CO3And 3molL-1NaOH, guarantee Mg2+:CO3 2-:OH-Mol ratio
For 5:4.8:2, after being stirred to react 120s, 4h is stood, slurry is obtained.
(2) gained slurry in (1) step is filtered, obtains 533.8g filtrate and 52.5g solid, and with deionized water into
Row washing solid to neutrality, filtrate quality forms are as follows: Na+: 7.29%；K+: 0.49%；Cl-: 8.64%；SO4 2-: 2.53%；
CO3 2-: 0.99%；H2O:80.06%.
(3) dry: the solid product that (2) step obtains being dried into 9h at 105 DEG C, obtains basic carbonate magnesium crystal, product
SEM figure see Fig. 9, be spheric granules.
Two, NaCl and Na in basic carbonate magnesium crystal preparation post mother liquor2SO4·10H2O is extracted
(4) it is added in obtained filtrate into (2) step and CO in filtrate3 2-The 0.5molL of equivalent-1CaCl2It is molten
Liquid, by CO in mother liquor3 2-It completely removes, is filtered after reaction, obtain 705.1g mother liquor, quality group becomes: Na+:
5.52%；K+: 0.37%；Cl-: 7.43%；SO4 2-: 1.92%；H2O:84.76%.
(5) gained 704.9g filtrate isothermal evaporation under the conditions of 25 DEG C in step (4) after steaming 411.2g water, stops evaporation, mistake
Filter out NaCl；Filtrate is cooled to 0 DEG C, stops after moisture reduces 81.7g, filters out Na2SO4·10H2O；By residual filtrate
25 DEG C of isothermal evaporations are warming up to, after evaporating 24.3g water, stops evaporation, filters out NaCl；Remaining mother liquor is cooled to 0 DEG C, works as water
Divide after reducing 17.7g and stop, filtering out Na2SO4·10H2O；Filtrate 53.6g is obtained, quality group becomes: Na+: 6.90%；K+:
4.85%；Cl-: 13.86%；SO4 2-: 1.68%；H2O:72.71%.
Three, in remaining mother liquor KCl and NaCl separation and Extraction
(6) it is added into (5) step finally obtained filtrate and SO in filtrate4 2-The 0.3molL of equivalent-1BaCl2
Solution, by the SO in mother liquor4 2-It completely removes, is filtered after reaction, obtain filtrate 83.6g, quality group becomes: Na+:
4.43%；K+: 3.11%；Cl-: 9.69%；H2O:82.77%.
(7) 100 DEG C of isothermal evaporation 54.77g moisture of gained 83.6g filtrate (mother liquor forms m in Fig. 3) in step (6), are precipitated
After 5.75g solid, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, is precipitated
After 2.48g solid, KCl is filtered out.Again by 100 DEG C of isothermal evaporation 7.1g water of obtained 20.6g filtrate (mother liquor forms D in Fig. 3)
Point, after 1.9g solid is precipitated, stops evaporation, filter out NaCl；Remaining mother liquor (satisfy composition E altogether in Fig. 3) is cooled to 25 DEG C, analysis
Out after 1.2g solid, KCl is filtered out.Obtained 10.4g residue mother liquor (mother liquor forms D in Fig. 3) repeats 100 DEG C of isothermal evaporation analysis
Sodium chloride 0.97g, then cool to 25 DEG C of precipitation potassium chloride 0.66g.Obtaining 0.567g residue mother liquor again, (mother liquor forms in Fig. 3
D 100 DEG C of isothermal evaporations) are repeated and analyse sodium chloride 0.52g, then cool to 25 DEG C of precipitation potassium chloride 0.34g.It is recycled by four times, it can
So that sodium chloride amount of precipitation reaches stopping when 97.13%, potassium chloride amount of precipitation reaches 94.16%.
Above example is all the technique by set of system, realizes recycling for bittern, realizes sodium in mother liquor, potassium etc.
Element is kept completely separate.Mg in experimentation2+Conversion ratio reach approximately 100%, be substantially free of Mg in remaining mother liquor2+、
HCO3 -, subsequent phasor is facilitated to separate.And the reaction time is reduced to 2.5h, reaction temperature is 60 DEG C, and energy saving, economic benefit is aobvious
It writes.The present invention devises the technique of set of system, realizes recycling for bittern, realizes the elements such as sodium in mother liquor, potassium
It is kept completely separate.
Unaccomplished matter of the present invention is well-known technique.
Claims (2)
1. a kind of bittern mixes the separation method that alkaline process prepares basic magnesium carbonate and its natrium potassium salt, it is characterized in that this method includes following
Step:
(1) prepared by basic carbonate magnesium crystal
(1) bittern is added in reactor, Na is then added2CO3Solution and NaOH solution, obtain mixed liquor, at 60~80 DEG C
After being stirred to react 100~150s, then 2.5~4.5h is stood, obtains slurry；
Wherein, the Na2CO3The concentration of solution is 1.0~2.5molL-1；The concentration of NaOH solution is 1~3molL-1；
Molar ratio Mg in mixed liquor2+:CO3 2-:OH-=5:4.8:1.9~2.1；
(2) gained slurry in (1) step is filtered, obtains filtrate and solid；And solid is washed with deionized to neutrality；
(3) dry: the solid after the washing of (2) step being dried into 8~10h at 100~110 DEG C, obtains basic carbonate magnesium crystal；
(2) NaCl and Na in basic carbonate magnesium crystal preparation post mother liquor2SO4·10H2O is extracted
(4) 0.3~0.5molL is added in obtained filtrate into (2) step-1CaCl2Solution is filtered after reaction,
Obtain filtrate；Wherein, CO in filtrate3 2-With CaCl2Ca in solution+Equivalent；
(5) to filtrate isothermal evaporation under the conditions of 25 DEG C is obtained in step (4), every 1000g filtrate evaporates 571.4~588.8g water,
NaCl is precipitated in crystallization, stops evaporation, filters out NaCl；Filtrate is cooled to 0 DEG C again, and is stopped after reducing moisture 114.0-119.0g
Only, Na is filtered out2SO4·10H2O；Continue for residual filtrate to be warming up to 25 DEG C of isothermal evaporations, after evaporating 33.9-35.4g moisture,
Stop evaporation, filters out NaCl；Remaining mother liquor is finally cooled to 0 DEG C, stops when moisture reduces 24.70-25.78g, filters out
Na2SO4·10H2O；
(3) in remaining mother liquor KCl and NaCl separation and Extraction
(6) 0.3~0.5molL is added into (5) step finally obtained filtrate-1BaCl2Solution carried out after reaction
Filter；(5) the last SO in obtained filtrate of step4 2-With BaCl2The Ba of solution+Equivalent；
(7) NaCl is precipitated in 100 DEG C of isothermal evaporations of gained filtrate in step (6), and every 1000g filtrate evaporates 649.9-661.1g water, knot
Partial crystallization goes out NaCl, stops evaporation, filters out the NaCl of 56.96-70.89g；Remaining mother liquor is cooled to 25 DEG C again, solid is precipitated
Afterwards, the KCl of 29.23-29.96g is filtered out；NaCl, evaporation water 83.72- is precipitated in 100 DEG C of isothermal evaporations in obtained filtrate
85.23g stops evaporation, filters out the NaCl of 22.41-22.86g；Remaining mother liquor is cooled to 25 DEG C again, after solid is precipitated, mistake
Filter out the KCl of 14.15-14.44g；Obtained remaining mother liquor repeats 1~3 time, and " 100 DEG C of isothermal evaporations analyse sodium chloride, then cool to
The process of 25 DEG C of analysis potassium chloride ", so that stopping when sodium chloride, potassium chloride amount of precipitation respectively reach 97% and 93% or more.
2. the bittern as belonging to claim 1 mixes the separation method that alkaline process prepares basic magnesium carbonate and its natrium potassium salt, it is characterized in that
The bittern composition in the step (one) includes: MgCl2: 150~180gL-1；NaCl:60~110gL-1；
KCl:18~22gL-1；MgSO4: 60~75gL-1。
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