CN102320632A - Method for preparing high-purity magnesium hydroxide and nanometer calcium carbonate as co-product from salt lake brine - Google Patents
Method for preparing high-purity magnesium hydroxide and nanometer calcium carbonate as co-product from salt lake brine Download PDFInfo
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- CN102320632A CN102320632A CN201110246618A CN201110246618A CN102320632A CN 102320632 A CN102320632 A CN 102320632A CN 201110246618 A CN201110246618 A CN 201110246618A CN 201110246618 A CN201110246618 A CN 201110246618A CN 102320632 A CN102320632 A CN 102320632A
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- mother liquor
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- calcium carbonate
- marinco
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 25
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 25
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 25
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 25
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000012267 brine Substances 0.000 title claims abstract description 12
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 14
- 235000011116 calcium hydroxide Nutrition 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 11
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910001626 barium chloride Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 8
- 239000011575 calcium Substances 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 230000008020 evaporation Effects 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims abstract description 4
- 239000012452 mother liquor Substances 0.000 claims description 49
- 241001131796 Botaurus stellaris Species 0.000 claims description 27
- 230000032683 aging Effects 0.000 claims description 20
- 238000009413 insulation Methods 0.000 claims description 18
- 235000017550 sodium carbonate Nutrition 0.000 claims description 10
- 229940045511 barium chloride Drugs 0.000 claims description 9
- 230000029087 digestion Effects 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 4
- 230000008030 elimination Effects 0.000 claims description 3
- 238000003379 elimination reaction Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000009987 spinning Methods 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005406 washing Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000010413 mother solution Substances 0.000 abstract 6
- 229910052791 calcium Inorganic materials 0.000 abstract 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 abstract 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000008267 milk Substances 0.000 abstract 1
- 210000004080 milk Anatomy 0.000 abstract 1
- 235000013336 milk Nutrition 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 20
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 8
- 239000012047 saturated solution Substances 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 229940056729 sodium sulfate anhydrous Drugs 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005008 domestic process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004572 hydraulic lime Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000010446 mirabilite Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229960003010 sodium sulfate Drugs 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for preparing high-purity magnesium hydroxide and nanometer calcium carbonate as a co-product from salt lake brine, and belongs to the technical field of comprehensive utilization of salt lake brine. The method comprises the following steps of 1) purifying raw materials; 2) adding barium chloride into refined brine and carrying out centrifugation separation to obtain a barium sulfate product and a mother solution I; 3) adding slaked lime milk into the mother solution I and carrying out solid-liquid separation to obtain magnesium hydroxide wet cakes and a mother solution II; 4) washing the magnesium hydroxide wet cakes at room temperature by deionized water to obtain high-purity magnesium hydroxide; 5) adding a sodium carbonate solution into the mother solution II and carrying out solid-liquid separation to obtain nanometer calcium carbonate and a mother solution III; and 6) carrying out beach field evaporation on the mother solution III to obtain sodium chloride solids. The method has the advantages that a completely comprehensive utilization of brine is realized; three-waste is not produced; no pollution on the environment is produced; a unique slaking edulcoration technology is adopted; low-calcium high-purity magnesium hydroxide is obtained; products have stable and high quality; mass production is realized easily; and obtained nanometer calcium carbonate has high whiteness and purity.
Description
Technical field
The invention belongs to salt lake brine comprehensive utilization technique field, relate to a kind of technology of utilizing salt lake brine to produce high purity magnesium hydroxide and coproduction nano-calcium carbonate, permanent white and sodium-chlor.
Background technology
Utilizing halogen (sea) water at present is that the method for raw material production Marinco H has following several kinds:
(1) caustic soda bittern method is a raw material with the bittern after magnesium chloride or the filtration, adds sodium hydroxide and carries out precipitin reaction, obtains Marinco H; Advantage is that speed of response is fast, and condition is easy to control, and product purity is high; Shortcoming is the sad filter of product, and raw materials cost is higher, equipment material is required high;
(2) ammoniacal liquor method; Bittern with after magnesium chloride or the filtration is raw material, is that precipitation agent reacts in reaction kettle with ammoniacal liquor, adds a certain amount of crystal seed before the reaction; Temperature of reaction is controlled at about 40 ℃; After having reacted, throw out is handled through operations such as filtration, washing, oven dry, pulverizing, makes magnesium hydroxide products; Advantage is that the Marinco H percent crystallinity that generates is higher, and sedimentation speed is fast, is easy to filter and washing, and product purity is high, and temperature of reaction is low, and condition is easy to control; Shortcoming is that raw materials cost is higher than the serum method, and operational condition is abominable;
(3) sodium hydrosulfide with salt lake brine or magnesium chloride and Sodium sulfhydrate reaction, obtains magnesium hydroxide products; Advantage is that speed of response is fast, and product purity is higher; Shortcoming is the sad filter of product, and raw materials cost is higher, equipment material is required high;
(4) lime bittern method is a raw material with the bittern after magnesium chloride or the filtration, with the milk of lime reaction after the digestion slagging-off, handles through operations such as filtration, washing, oven dry, pulverizing after the reaction again, makes magnesium hydroxide products; Advantage is that production cost is lower; Shortcoming is that foreign matter content is high.
The present domestic method for preparing nano-calcium carbonate mainly contains: intermittent type carborization, overweight force method, multi-stage spray carborization, non-refrigeration method and film disperse micro-structured reactor method etc.
Utilizing halogen (sea) water to present China is the deficiency of raw material production Marinco H technology, remain to be researched and developed a kind ofly can efficiently utilize bittern, and the method for the Marinco H that can be mass-produced.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing salt lake brine to prepare high purity magnesium hydroxide and coproduction nano-calcium carbonate, utilize mineral salt lake bittern water and milk of lime, produce high-purity Marinco H, and coproduction nano-calcium carbonate, permanent white and sodium-chlor.
The present invention realizes through following technical scheme:
Utilize salt lake brine to prepare the method for high purity magnesium hydroxide and coproduction nano-calcium carbonate, may further comprise the steps:
(1) purification of raw material: bittern is heated to 50-90 ℃, filters, must make with extra care bittern behind the elimination impurity with zeyssatite;
(2) removal of sulfate radical: slowly add bariumchloride in the refining bittern, wherein add-on is by SO in the refining bittern
4 2-With Ba in the bariumchloride
2+Equivalence ratio be that 1:1 calculates, controlled temperature react 0.5-2 hour at 30-60 ℃, was incubated ageing, 0.5-1.5 hour, spinning got barium sulfate product and mother liquor I;
(3) preparation of Marinco H: the milk of lime good digestion slowly joins in the mother liquor I, and wherein add-on is pressed Ca in the milk of lime
2+With the Mg in the mother liquor I
2+Equivalence ratio be that 1.05-1.50:1 calculates, controlled temperature is at 50-90 ℃, reinforced time 1-3 hour, react 2-4 hour, solid-liquid separation is carried out in insulation ageing 2-3 hour then, Marinco H wet cake and mother liquor II;
(4) preparation of high purity magnesium hydroxide: use quality to wash at normal temperatures the wet cake of Marinco H, dry down at 100-120 ℃ then and promptly get high purity magnesium hydroxide as Marinco H quality 20-50 deionized water doubly;
(5) preparation of nano-calcium carbonate: in the mother liquor II, slowly add sodium carbonate solution, wherein add-on is pressed Ca in the mother liquor II
2+With CO in the yellow soda ash
3 2-Equivalence ratio is that 1-1.2:1 calculates, and controlled temperature fed in raw material time 1-8 hour at 30-100 ℃, reacts 2-6 hour, and solid-liquid separation is carried out in insulation ageing 2-5 hour then, obtains nano-calcium carbonate and the mother liquor III of particle diameter 0.01um-10um;
(6) preparation of sodium-chlor: the mother liquor III is carried out the evaporation of field, beach, promptly get solid sodium chloride.
The salt lake, Yuncheng belongs to landlocked sulfate type salt lake, and bittern belongs to Na
+, Mg
2+//SO
4 2-, Cl
--H
2The O mutual system of quadruplex for many years, follows always and supports halogen summer; Analyse nitre winter, is the technology of raw material production Sodium sulfate anhydrous.min(99) with the mirabilite hydrate, because single extraction sodium sulfate; Making the magnesium salts enrichment not only influences the quality product of Sodium sulfate anhydrous.min(99), and causes wasting of magnesium resource.For making full use of salt lake resources, produce high value added product, utilize the inventive method to produce high purity magnesium hydroxide, may further comprise the steps:
(1) bittern is heated to 50-65 ℃, filters, must make with extra care bittern behind the elimination impurity, record SO in the bittern with zeyssatite
4 2-Content is 40g/L;
(2) slowly adding bariumchloride in the refining bittern, is that 1:1 prepares burden by the equivalence ratio of sulfate radical and barium ion,, temperature is controlled at 30-45 ℃, and in 2 hours reaction times, spinning gets barium sulfate product and mother liquor I;
(3) slowly join the good milk of lime of digestion in the mother liquor I, wherein add-on is pressed Ca in the milk of lime
2+With the Mg in the mother liquor I
2+Equivalence ratio be that 1.05:1 calculates, controlled temperature is at 70-90 ℃, the reinforced 1 hour time, react 2 hours, solid-liquid separation is carried out in insulation ageing 2 hours then, Marinco H wet cake and mother liquor II;
(4) uses quality to wash at normal temperatures the wet cake of Marinco H, dry down at 100-110 ℃ then that promptly to get purity be 98.2% Marinco H as the deionized water of 35 times of Marinco H quality;
(5) in the mother liquor II, slowly add sodium carbonate solution, wherein add-on is pressed Ca in the mother liquor II
2+With CO in the yellow soda ash
3 2-Equivalence ratio is that 1.2:1 calculates, and controlled temperature feeds in raw material 5 hours time at 30-50 ℃, reacts 2 hours, and solid-liquid separation is carried out in insulation ageing 3 hours then, obtains nano-calcium carbonate and the mother liquor III of particle diameter 0.01um-10um;
(6) preparation of sodium-chlor: the mother liquor III is carried out the evaporation of field, beach, promptly get solid sodium chloride.
Compared with prior art, the present invention has following advantage:
(1) bittern has been realized comprehensive utilization completely, has not had any three wastes and produce that environment is not had any pollution;
(2) be the raw material production high purity magnesium hydroxide with bittern and milk of lime, adopt exclusive digestion impurity removing technology, obtain the low high purity magnesium hydroxide of calcic, the products obtained therefrom quality is high and stable, easy realization of large-scale production;
(3) produced mother liquor and nano-calcium carbonate, the sodium-chlor coproduction of Marinco H, the lime carbonate whiteness that this method is produced is good, and purity is high;
(4) find a good in economic efficiency approach for the bittern comprehensive utilization.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Embodiment 1
Get SO
4 2-Content is the bittern 1L of 48g/L and the saturated solution reaction that contains the 104g bariumchloride, reacts 30 minutes down at 35 ℃, and the insulation ageing was carried out solid-liquid separation after 1 hour, got 115g permanent white and mother liquor I 1.35L; Is 1.7 liters of good solid contents of digestion that 15% milk of lime adds in the mother liquor I slowly, and control reaction temperature is at 80 ℃, the reinforced 1.5 hours time; Reacted 2 hours; Solid-liquid separation is carried out in insulation ageing 2 hours then, gets wet cake 360g of Marinco H and mother liquor II 2.86L; After the wet cake of Marinco H washs with the deionized water of 7200g at normal temperatures, dry by the fire down at 110 ℃ that to prepare main content in 3 hours be 98.02% high purity magnesium hydroxide product 174g; The saturated solution that in the mother liquor II, slowly adds 290 g yellow soda ash reacts; Temperature of reaction is controlled at 50-70 ℃, the reinforced 5 hours time, reacts 5 hours; Insulation ageing 5 hours; Carry out solid-liquid separation then, obtain nano-calcium carbonate 275g and mother liquor III 3.25L, evaporate the mother liquor III and obtain solid sodium chloride 85g.
Embodiment 2
Get SO
4 2-Content is the bittern 1L of 55g/L and the saturated solution reaction that contains the 119g bariumchloride, reacts 50 minutes down at 50 ℃, and the insulation ageing was carried out solid-liquid separation after 1.5 hours, got 130g permanent white and mother liquor I 1.55L; Is 1.95 liters of good solid contents of digestion that 15% milk of lime adds in the mother liquor I slowly, and control reaction temperature is at 75 ℃, the reinforced 3 hours time; Reacted 4 hours; Solid-liquid separation is carried out in insulation ageing 2 hours then, gets wet cake 415g of Marinco H and mother liquor II 3.28L; After the wet cake of Marinco H washs with the deionized water of 16600g at normal temperatures, dry by the fire down at 100 ℃ that to prepare main content in 2.5 hours be 98.11% high purity magnesium hydroxide product 200g; The saturated solution that in the mother liquor II, slowly adds 335g yellow soda ash reacts; Temperature of reaction is controlled at 90-100 ℃, the reinforced 1 hour time, reacts 2 hours; Insulation ageing 2 hours; Carry out solid-liquid separation then, obtain nano-calcium carbonate 315g and mother liquor III 3.70L, evaporate the mother liquor III and obtain solid sodium chloride 96g.
Embodiment 3
Get SO
4 2-Content is the bittern 1L of 60g/L and the saturated solution reaction that contains the 130g bariumchloride, reacts 120 minutes down at 30 ℃, and the insulation ageing was carried out solid-liquid separation after 0.5 hour, got 145g permanent white and mother liquor I 1.80L; Is 2.1 liters of good solid contents of digestion that 14% milk of lime adds in the mother liquor I slowly, and control reaction temperature is at 85 ℃, the reinforced 2 hours time; Reacted 3 hours; Solid-liquid separation is carried out in insulation ageing 1 hour then, gets wet cake 445g of Marinco H and mother liquor II 3.75L; After the wet cake of Marinco H washs with the deionized water of 22250g at normal temperatures, dry by the fire down at 120 ℃ that to prepare main content in 2 hours be 98.30% high purity magnesium hydroxide product 220g; The saturated solution that in the mother liquor II, slowly adds 360g yellow soda ash reacts; Temperature of reaction is controlled at 30-50 ℃, the reinforced 8 hours time, reacts 6 hours; Insulation ageing 3.5 hours; Carry out solid-liquid separation then, obtain nano-calcium carbonate 355g and mother liquor III 4.2L, evaporate the mother liquor III and obtain solid sodium chloride 105g.
Embodiment 4
Get SO
4 2-Content is the bittern 1L of 40g/L and the saturated solution reaction that contains the 130g bariumchloride, reacts 90 minutes down at 60 ℃, and the insulation ageing was carried out solid-liquid separation after 0.5 hour, got 145g permanent white and mother liquor I 1.80L; Is 2.1 liters of good solid contents of digestion that 14% milk of lime adds in the mother liquor I slowly, and control reaction temperature is at 90 ℃, the reinforced 1 hour time; Reacted 2 hours; Solid-liquid separation is carried out in insulation ageing 3 hours then, gets wet cake 445g of Marinco H and mother liquor II 3.75L; After the wet cake of Marinco H washs with the deionized water of 13350g at normal temperatures, dry by the fire down at 110 ℃ that to prepare main content in 3 hours be 98.23% high purity magnesium hydroxide product 220g; The saturated solution that in the mother liquor II, slowly adds 385g yellow soda ash reacts; Temperature of reaction is controlled at 70-90 ℃, the reinforced 3 hours time, reacts 4 hours; Insulation ageing 3.5 hours; Carry out solid-liquid separation then, obtain nano-calcium carbonate 360g and mother liquor III 4.3L, evaporate the mother liquor III and obtain solid sodium chloride 110g.
Claims (1)
1. method of utilizing salt lake brine to prepare high purity magnesium hydroxide and coproduction nano-calcium carbonate is characterized in that may further comprise the steps:
(1) purification of raw material: bittern is heated to 50-90 ℃, filters, must make with extra care bittern behind the elimination impurity with zeyssatite;
(2) removal of sulfate radical: slowly add bariumchloride in the refining bittern, wherein add-on is by SO in making with extra care in the bittern
4 2-With Ba in the bariumchloride
2+Equivalence ratio be that 1:1 calculates, controlled temperature react 0.5-2 hour at 30-60 ℃, was incubated ageing, 0.5-1.5 hour, spinning got barium sulfate product and mother liquor I;
(3) preparation of Marinco H: the milk of lime good digestion slowly joins in the mother liquor I, and wherein add-on is pressed Ca in the milk of lime
2+With the Mg in the mother liquor I
2+Equivalence ratio be that 1.05-1.50:1 calculates, controlled temperature is at 50-90 ℃, reinforced time 1-3 hour, react 2-4 hour, solid-liquid separation is carried out in insulation ageing 2-3 hour then, Marinco H wet cake and mother liquor II;
(4) preparation of high purity magnesium hydroxide: use quality to wash at normal temperatures the wet cake of Marinco H, dry down at 100-120 ℃ then and promptly get high purity magnesium hydroxide as Marinco H quality 20-50 deionized water doubly;
(5) preparation of nano-calcium carbonate: in the mother liquor II, slowly add sodium carbonate solution, wherein add-on is pressed Ca in the mother liquor II
2+With CO in the yellow soda ash
3 2-Equivalence ratio is that 1-1.2:1 calculates, and controlled temperature fed in raw material time 1-8 hour at 30-100 ℃, reacts 2-6 hour, and solid-liquid separation is carried out in insulation ageing 2-5 hour then, obtains nano-calcium carbonate and the mother liquor III of particle diameter 0.01um-10um;
(6) preparation of sodium-chlor: the mother liquor III is carried out the evaporation of field, beach, promptly get solid sodium chloride.
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| CN106946275A (en) * | 2017-03-06 | 2017-07-14 | 青海锂业有限公司 | The method for directly producing battery-stage monohydrate lithium hydroxide using the rich lithium bittern in salt lake |
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| CN105540624A (en) * | 2015-12-07 | 2016-05-04 | 上海实业振泰化工有限公司 | Preparation method of high purity acicular magnesium hydroxide |
| CN106946275A (en) * | 2017-03-06 | 2017-07-14 | 青海锂业有限公司 | The method for directly producing battery-stage monohydrate lithium hydroxide using the rich lithium bittern in salt lake |
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Application publication date: 20120118 |