CN111215430A - Alkaline residue utilization method for separating calcium and magnesium by phase transfer method - Google Patents
Alkaline residue utilization method for separating calcium and magnesium by phase transfer method Download PDFInfo
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- CN111215430A CN111215430A CN201911426687.4A CN201911426687A CN111215430A CN 111215430 A CN111215430 A CN 111215430A CN 201911426687 A CN201911426687 A CN 201911426687A CN 111215430 A CN111215430 A CN 111215430A
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- 238000000034 method Methods 0.000 title claims abstract description 49
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000011777 magnesium Substances 0.000 title claims abstract description 45
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 45
- 238000012546 transfer Methods 0.000 title claims abstract description 31
- 239000011575 calcium Substances 0.000 title claims abstract description 24
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 23
- 239000012071 phase Substances 0.000 claims abstract description 45
- 239000007790 solid phase Substances 0.000 claims abstract description 38
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 36
- 238000005406 washing Methods 0.000 claims abstract description 24
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 22
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 18
- 239000007791 liquid phase Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000000706 filtrate Substances 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 23
- 239000000047 product Substances 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000006276 transfer reaction Methods 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 9
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 8
- 239000001110 calcium chloride Substances 0.000 claims description 8
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 5
- 150000003839 salts Chemical class 0.000 abstract description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 3
- 238000009270 solid waste treatment Methods 0.000 abstract description 2
- 239000003518 caustics Substances 0.000 description 16
- 239000010802 sludge Substances 0.000 description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 239000003513 alkali Substances 0.000 description 6
- 239000004566 building material Substances 0.000 description 4
- 235000017550 sodium carbonate Nutrition 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 239000002893 slag Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000009621 Solvay process Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000192710 Microcystis aeruginosa Species 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 229940003871 calcium ion Drugs 0.000 description 1
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000009364 mariculture Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000003516 soil conditioner Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 that is Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for utilizing alkaline residue for separating calcium and magnesium by a phase transfer method, and belongs to the technical field of solid waste treatment. The method comprises the steps of using alkaline residue as a raw material, removing soluble salts by washing, converting carbonate and hydroxide phases into oxide phases by heat treatment, then separating calcium and magnesium well by a phase transfer method, wherein calcium ions enter a liquid phase, magnesium elements enter a solid phase, and finally preparing a calcium carbonate product from a calcium-containing solution after phase transfer, and meanwhile, enriching the magnesium elements in the solid phase, so that the calcium carbonate product can be used for producing a magnesium product.
Description
Technical Field
The invention belongs to the technical field of solid waste treatment, and particularly relates to a method for utilizing alkaline residue for separating calcium and magnesium by a phase transfer method.
Background
The caustic sludge, also called white mud, is waste residue produced in the process of preparing soda ash by an ammonia-soda process, and about 300 kg of caustic sludge is produced for every 1 ton of soda ash produced. For the treatment of the caustic sludge, a stacking mode is usually adopted, the stacking and discharging of the caustic sludge cause serious resource waste and environmental pollution, and a large amount of caustic sludge forms a 'white sea' after being deposited, so that the pollution of surrounding soil and underground water is caused.
The main components and content of the caustic sludge depend on the components of the raw materials for producing the alkali. At present, the alkali-making process of each alkali factory is largely the same and slightly different, so the components of the alkali residue are basically similar, mainly comprising CaCO3、CaCl2、Mg(OH)2NaCl and the like, together with a small amount of SiO2、Al2O3And other salts, water insoluble, and the like.
With the enhancement of environmental protection consciousness of the whole society and the improvement of the attention degree on the development and utilization of secondary resources, the comprehensive utilization of the caustic sludge is paid extensive attention. At present, the main utilization methods of the caustic sludge comprise:
1) engineering building materials: alkali slag cement, alkali slag soil, alkali slag brick, building mortar modifier and the like;
2) in the chemical industry aspect: flue gas desulfurization, rubber packing and the like;
3) agriculture and fishery: soil conditioner or calcium-magnesium compound fertilizer, mariculture pond bottom or water quality conditioner, etc.;
4) and (3) environmental protection: treating red tide and water bloom, and preparing sterilizing health products and the like.
In the field of engineering building materials, the caustic sludge is difficult to be doped into building materials on a large scale due to high alkalinity and high chlorine content, so that the use amount of the caustic sludge is limited, and meanwhile, the durability and stability of the building materials are seriously influenced due to the fact that the caustic sludge contains a large amount of soluble salts and chloride ions; in other fields, the consumption of caustic sludge is greatly limited due to the limitation of the film regulation of the market.
Disclosure of Invention
The invention aims to provide a method for utilizing alkaline residue for separating calcium and magnesium by a phase transfer method, which can realize the separation of calcium and magnesium from the alkaline residue, can absorb the alkaline residue on a large scale and simultaneously realize the utilization of the alkaline residue.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for utilizing alkaline residue for separating calcium and magnesium by a phase transfer method, which comprises the following steps:
mixing the alkaline residue with water, and sequentially and repeatedly washing and separating solid from liquid to obtain a solid phase and a liquid phase;
concentrating and crystallizing the liquid phase to obtain sodium chloride and calcium chloride;
carrying out heat treatment on the solid phase to obtain calcined powder;
mixing the calcined powder, a phase transfer agent and water, carrying out phase transfer reaction, and separating the obtained product to obtain filtrate containing calcium ions and a solid phase rich in magnesium;
and respectively preparing the filtrate containing calcium ions and the solid phase rich in magnesium into calcium carbonate and magnesium products.
Preferably, in the washing process, the solid-liquid ratio is 1: 2-5, the solid phase obtained by solid-liquid separation is washed for 2-5 times, the filtrate obtained by washing for each time is reused for 3-5 times until the solution density reaches more than 1.25g/mL, and the reuse is stopped for concentration and crystallization.
Preferably, the temperature of the heat treatment is 950 ℃ and the time is 1 h.
Preferably, the phase transfer agent is citric acid.
Preferably, the mass ratio of the calcium oxide to the phase transfer agent in the calcined powder is 1: 1-2.5.
Preferably, in the step of mixing the calcined powder, the phase transfer agent and water, the mass ratio of the calcined powder to the water is 1: 5-25.
Preferably, the reaction time of the phase transfer reaction is 10-100 min, and the reaction temperature is 20-60 ℃.
Preferably, the process for preparing calcium carbonate from the filtrate containing calcium ions comprises the following steps: introducing CO into the filtrate containing calcium ions2And aging, filtering, washing and drying the solution until the pH value of the solution is 7 to obtain the calcium carbonate.
Preferably, CO is introduced into the filtrate containing calcium ions under the condition of constant-temperature stirring2The temperature of the constant temperature was 50 ℃ until the solution pH was 7, and the stirring rate was 60 r/min.
Preferably, the aging time is 3h, and the drying temperature is 60 ℃.
The invention provides a method for utilizing alkaline residue for separating calcium and magnesium by a phase transfer method, which comprises the following steps: mixing the alkaline residue with water, and sequentially and repeatedly washing and separating solid from liquid to obtain a solid phase and a liquid phase; concentrating and crystallizing the liquid phase to obtain sodium chloride and calcium chloride; carrying out heat treatment on the solid phase to obtain calcined powder; mixing the calcined powder, a phase transfer agent and water, carrying out phase transfer reaction, and separating the obtained product to obtain filtrate containing calcium ions and a solid phase rich in magnesium; and respectively preparing the filtrate containing calcium ions and the solid phase rich in magnesium into calcium carbonate and magnesium products. The method comprises the steps of using alkaline residue as a raw material, removing soluble salts by washing, converting carbonate and hydroxide phases into oxide phases by heat treatment, then separating calcium and magnesium well by a phase transfer method, wherein calcium ions enter a liquid phase, magnesium elements enter a solid phase, and finally preparing a calcium carbonate product from a calcium-containing solution after phase transfer, and meanwhile, enriching the magnesium elements in the solid phase, so that the calcium carbonate product can be used for producing a magnesium product.
The method disclosed by the invention can realize the separation of calcium and magnesium in the alkaline residue, can be used for consuming the alkaline residue on a large scale, realizes the recycling of the medium, reduces the cost, is energy-saving and environment-friendly, and is suitable for industrial production.
Detailed Description
The invention provides a method for utilizing alkaline residue for separating calcium and magnesium by a phase transfer method, which comprises the following steps:
mixing the alkaline residue with water, and sequentially and repeatedly washing and separating solid from liquid to obtain a solid phase and a liquid phase;
concentrating and crystallizing the liquid phase to obtain sodium chloride and calcium chloride;
carrying out heat treatment on the solid phase to obtain calcined powder;
mixing the calcined powder, a phase transfer agent and water, carrying out phase transfer reaction, and separating the obtained product to obtain filtrate containing calcium ions and a solid phase rich in magnesium;
and respectively preparing the filtrate containing calcium ions and the solid phase rich in magnesium into calcium carbonate and magnesium products.
Mixing the caustic sludge with water, and sequentially and repeatedly washing and separating solid and liquid to obtain a solid phase and a liquid phase. In the invention, the alkaline residue is preferably waste residue generated in the process of preparing the soda ash by using an ammonia-soda process, and the alkaline residue used in the invention is sourced from a factory for producing the soda ash. In the embodiment of the present invention, the present invention preferably uses dry caustic sludge, that is, caustic sludge after drying, and the drying process is not particularly limited in the present invention. In the invention, the water is preferably tap water, the water washing is preferably carried out under stirring conditions, and the stirring time of each water washing is preferably 30 min; the rotation speed of the stirring is not particularly limited in the present invention, and a process well known in the art may be used. In the invention, in the water washing process, the solid-liquid ratio (namely the mass ratio of the alkaline residue to the water) is preferably 1: 2-5, more preferably 1: 3-4, the solid phase obtained by solid-liquid separation in each time is preferably repeatedly washed for 2-5 times (more preferably 3-4 times), the filtrate obtained by water washing in each time is preferably applied for 3-5 times until the solution density reaches more than 1.25g/mL, and the application is stopped, and subsequent concentration and crystallization are carried out. The solid-liquid separation method is not particularly limited in the present invention, and a solid-liquid separation method well known in the art may be selected, and for example, the solid-liquid separation method may specifically be filtration.
After a solid phase and a liquid phase are obtained, the liquid phase is concentrated and crystallized to obtain sodium chloride and calcium chloride; and carrying out heat treatment on the solid phase to obtain calcined powder. The process of the concentration and crystallization in the present invention is not particularly limited, and a process well known in the art may be selected. In the present invention, the temperature of the heat treatment is preferably 950 ℃ and the time is preferably 1 hour. The present invention converts carbonates and hydroxides in a solid phase into oxides by heat treatment, and the calcined powder mainly contains magnesium oxide and calcium oxide.
After calcined powder is obtained, the calcined powder, a phase transfer agent and water are mixed for phase transfer reaction, and after the obtained product is separated, filtrate containing calcium ions and a solid phase rich in magnesium are obtained. In the present invention, the phase transfer agent is preferably citric acid. The source of the citric acid is not particularly limited in the present invention, and commercially available products having a source well known in the art may be selected. In the invention, the mass ratio of the calcium oxide to the phase transfer agent in the calcined powder is preferably 1: 1-2.5, and more preferably 1: 1.5; the mass ratio of the calcined powder to water is preferably 1: 5-25, and more preferably 1: 10-15; the water is preferably distilled water. The mixing process is not particularly limited in the invention, and the raw materials can be uniformly mixed by selecting the process well known in the field.
In the invention, the reaction time of the phase transfer reaction is preferably 10-100 min, more preferably 30-80 min, and further preferably 50-60 min, and the reaction temperature is preferably 20-60 ℃, and more preferably 30-50 ℃. During the phase transfer reaction, calcium oxide is dissolved into the liquid phase and magnesium oxide remains in the solid phase.
In the present invention, the separation method is preferably solid-liquid separation, and the solid-liquid separation method is not particularly limited in the present invention, and may be any solid-liquid separation method known in the art, for example, filtration may be specifically used.
After the filtrate containing calcium ions and the solid phase rich in magnesium are obtained, the filtrate containing calcium ions and the solid phase rich in magnesium are respectively prepared into calcium carbonate and magnesium products. In the present invention, the process of preparing calcium carbonate from the filtrate containing calcium ions is preferably as follows: introducing CO into the filtrate containing calcium ions2And aging, filtering, washing and drying the solution until the pH value of the solution is 7 to obtain the calcium carbonate. The invention preferably introduces CO under the condition of constant temperature stirring2The constant temperature is preferably 50 ℃, and the stirring speed is preferably 60 r/min. In the present invention, the aging time is preferably 3 hours, and the aging temperature is preferably 50 ℃; the temperature of the drying is preferably 60 ℃. The present invention is not particularly limited to the other processes of filtering, washing and drying, and may be a process well known in the art. The process for preparing the magnesium product from the magnesium-rich solid phase is not particularly limited, and a process known in the art may be selected.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 2000mL of tap water into 1000g of dry caustic sludge, stirring for 30min, sequentially and repeatedly washing and filtering for 3 times, wherein the filtrate washed by each time is used as a solvent for next washing for 3 times, and after 3 times of repeated washing, the density of the filtrate reaches 1.28g/mL to obtain a solid phase and a liquid phase, and concentrating and crystallizing the liquid phase to obtain sodium chloride and calcium chloride, wherein 216g of sodium chloride and 197g of calcium chloride containing sodium chloride are obtained;
performing heat treatment on the solid phase at 950 ℃ for 1h to obtain calcined powder, mixing 100g of the calcined powder with citric acid (300g) and distilled water (1000g), wherein the mass ratio of calcium oxide to citric acid in the calcined powder is 1: 1.5, performing phase transfer reaction for 40min at 20 ℃ to obtain filtrate containing calcium ions and a solid phase rich in magnesium, wherein Ca is used for preparing the calcium-ion-containing solid phase2+And Mg2+The phase transfer rates of the calcium and the magnesium are respectively 96.36 percent and 2.43 percent, so that the separation of calcium and magnesium is realized;
introducing CO into the filtrate containing calcium ions at constant temperature of 50 deg.C under stirring (60r/min)2And aging the solution at 50 ℃ for 3h until the pH of the solution is 7, and sequentially filtering, washing and drying the obtained product at 60 ℃ to obtain the calcium carbonate.
According to the embodiment, the invention provides the method for utilizing the alkaline residue for separating calcium and magnesium by the phase transfer method, the alkaline residue is used as the raw material, soluble salt is removed by washing, carbonate and hydroxide phases are converted into oxide phases by heat treatment, then calcium and magnesium in the alkaline residue are well separated by the phase transfer method, the transfer rate is high, calcium ions enter a liquid phase, magnesium elements enter a solid phase, and finally calcium carbonate products are prepared from the calcium-containing solution after phase transfer, and meanwhile, the magnesium elements in the solid phase are enriched and can be used for producing magnesium products.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for utilizing alkaline residue for separating calcium and magnesium by a phase transfer method is characterized by comprising the following steps:
mixing the alkaline residue with water, and sequentially and repeatedly washing and separating solid from liquid to obtain a solid phase and a liquid phase;
concentrating and crystallizing the liquid phase to obtain sodium chloride and calcium chloride;
carrying out heat treatment on the solid phase to obtain calcined powder;
mixing the calcined powder, a phase transfer agent and water, carrying out phase transfer reaction, and separating the obtained product to obtain filtrate containing calcium ions and a solid phase rich in magnesium;
and respectively preparing the filtrate containing calcium ions and the solid phase rich in magnesium into calcium carbonate and magnesium products.
2. The method according to claim 1, wherein in the water washing process, the solid-liquid ratio is 1: 2-5, the solid phase obtained by solid-liquid separation is repeatedly washed with water for 2-5 times, the filtrate obtained by each water washing is reused for 3-5 times until the solution density reaches more than 1.25g/mL, and the reuse is stopped for concentration and crystallization.
3. The method according to claim 1, wherein the temperature of the heat treatment is 950 ℃ and the time is 1 hour.
4. The method of claim 1, wherein the phase transfer agent is citric acid.
5. The method as claimed in claim 4, wherein the calcined powder contains calcium oxide and a phase transfer agent at a mass ratio of 1: 1 to 2.5.
6. The method according to claim 1, wherein in the step of mixing the calcined powder, the phase transfer agent and water, the mass ratio of the calcined powder to the water is 1: 5 to 25.
7. The method according to any one of claims 4 to 6, wherein the reaction time of the phase transfer reaction is 10 to 100min, and the reaction temperature is 20 to 60 ℃.
8. The method according to claim 1, wherein the process of preparing calcium carbonate from the filtrate containing calcium ions comprises: introducing CO into the filtrate containing calcium ions2Until the pH value of the solution is 7, sequentially aging, filtering, washing and drying,calcium carbonate is obtained.
9. The method of claim 8, wherein the filtrate containing calcium ions is aerated with CO under constant temperature stirring2The temperature of the constant temperature was 50 ℃ until the solution pH was 7, and the stirring rate was 60 r/min.
10. The process according to claim 8, characterized in that the aging time is 3h and the drying temperature is 60 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113683102A (en) * | 2021-08-26 | 2021-11-23 | 四川大学 | High-purity basic magnesium carbonate and preparation method thereof |
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| JP4017456B2 (en) * | 2002-07-02 | 2007-12-05 | 太平洋セメント株式会社 | Method for recovering chloride from aqueous solution |
| CN102112637A (en) * | 2008-05-30 | 2011-06-29 | 阿尔托大学基金会 | Method of producing calcium carbonate from waste and byproducts |
| CN102092748A (en) * | 2010-04-30 | 2011-06-15 | 汪晋强 | Method for producing magnesium carbonate, calcium carbonate and ammonium sulfate by using soda ash waste residues |
| CN102161495A (en) * | 2011-02-28 | 2011-08-24 | 广东工业大学 | Method for recycling soda waste mud from soda plant |
| CN102744238A (en) * | 2012-07-14 | 2012-10-24 | 南京工业大学 | Comprehensive utilization method of plant ash for biomass power plant |
| CN103387254A (en) * | 2013-07-19 | 2013-11-13 | 合肥工业大学 | A preparation method for light calcium carbonate by using a phase transfer-carbonization method |
| CN104016393A (en) * | 2014-06-12 | 2014-09-03 | 合肥工业大学 | Method for preparing light calcium carbonate and magnesium oxide from dolomite |
| CN107555462A (en) * | 2017-08-21 | 2018-01-09 | 赵阳臣 | A kind of method of calcined soda waste residue comprehensive reutilization |
| CN109570186A (en) * | 2018-10-24 | 2019-04-05 | 湖北云应矿业技术开发有限公司 | A kind of reuse method of soda-manufacturing waste residue liquid and system using this method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113683102A (en) * | 2021-08-26 | 2021-11-23 | 四川大学 | High-purity basic magnesium carbonate and preparation method thereof |
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