CN115180655A - Method for utilizing all components of steel slag and constructing nano functional material - Google Patents
Method for utilizing all components of steel slag and constructing nano functional material Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 37
- 239000002893 slag Substances 0.000 title claims abstract description 37
- 239000010959 steel Substances 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000003463 adsorbent Substances 0.000 claims abstract description 12
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 9
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 9
- 239000000378 calcium silicate Substances 0.000 claims abstract description 6
- 229910052918 calcium silicate Inorganic materials 0.000 claims abstract description 6
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 5
- 239000008204 material by function Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 38
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000000926 separation method Methods 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 13
- 238000004321 preservation Methods 0.000 claims description 13
- 238000003760 magnetic stirring Methods 0.000 claims description 11
- 235000006408 oxalic acid Nutrition 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- GAISRYMZAXLPHD-UHFFFAOYSA-N 2-hydroxybenzoic acid;methanol Chemical compound OC.OC(=O)C1=CC=CC=C1O GAISRYMZAXLPHD-UHFFFAOYSA-N 0.000 claims description 9
- 239000002131 composite material Substances 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- ASTWEMOBIXQPPV-UHFFFAOYSA-K trisodium;phosphate;dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[Na+].[O-]P([O-])([O-])=O ASTWEMOBIXQPPV-UHFFFAOYSA-K 0.000 claims description 9
- 239000004115 Sodium Silicate Substances 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 8
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 8
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 8
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- JLDKGEDPBONMDR-UHFFFAOYSA-N calcium;dioxido(oxo)silane;hydrate Chemical compound O.[Ca+2].[O-][Si]([O-])=O JLDKGEDPBONMDR-UHFFFAOYSA-N 0.000 claims description 5
- KAEAMHPPLLJBKF-UHFFFAOYSA-N iron(3+) sulfide Chemical compound [S-2].[S-2].[S-2].[Fe+3].[Fe+3] KAEAMHPPLLJBKF-UHFFFAOYSA-N 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 claims description 2
- AVVIDTZRJBSXML-UHFFFAOYSA-L calcium;2-carboxyphenolate;dihydrate Chemical compound O.O.[Ca+2].OC1=CC=CC=C1C([O-])=O.OC1=CC=CC=C1C([O-])=O AVVIDTZRJBSXML-UHFFFAOYSA-L 0.000 claims description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 229960004889 salicylic acid Drugs 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 abstract description 13
- 239000002699 waste material Substances 0.000 abstract description 5
- 239000002910 solid waste Substances 0.000 abstract description 4
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 abstract description 2
- 150000007524 organic acids Chemical class 0.000 abstract 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 238000005215 recombination Methods 0.000 abstract 1
- 230000006798 recombination Effects 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- 239000007790 solid phase Substances 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- 239000000843 powder Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 10
- 239000012153 distilled water Substances 0.000 description 9
- -1 polytetrafluoroethylene Polymers 0.000 description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 description 9
- 239000000725 suspension Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- PHIQPXBZDGYJOG-UHFFFAOYSA-N sodium silicate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-][Si]([O-])=O PHIQPXBZDGYJOG-UHFFFAOYSA-N 0.000 description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/24—Alkaline-earth metal silicates
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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Abstract
A method for utilizing all components of steel slag and constructing a nano functional material belongs to the field of solid waste recycling. The steel slag components are subjected to shunting and recombination based on the steel slag structure, and the nano functional material is prepared for sewage purification. By using acidsExtracting calcium-rich liquid-solid phase with weak organic acid to respectively prepare two adsorbents of hydrated calcium silicate and hydroxyapatite, and extracting with Mg-rich organic acid 2+ 、Al 3+ And Fe 3+ The layered double hydroxide loaded by iron sulfide is prepared from the filtrate of the metal ions, so that the full component utilization of the steel slag is realized, and the amount of the waste slag is reduced to the minimum. The work provides a simple, popular and environment-friendly strategy, fully avoids the disadvantage of complex components of the steel slag, and lays a foundation for widening the application of the steel slag in constructing novel nano functional materials.
Description
Technical Field
The invention relates to a method for constructing a nano functional material by utilizing all components of steel slag, belonging to the field of functional material application.
Technical Field
In recent years, people actively encourage the utilization of raw materials with low cost, easy acquisition and large storage capacity, especially industrial solid waste materials with huge application potential, to develop and construct novel functional nano materials. The steel slag is a byproduct generated in the steel-making process, and is heterogeneous waste with Fe, mg, al and Ca elements as main components, so that the steel slag has great application potential to prepare the nano functional composite material with excellent performance. Although the utilization advantage of the steel slag is obvious, the complete utilization of all the components of the steel slag is very difficult to minimize the resource waste due to the complex component characteristics, so the high-efficiency utilization of the steel slag is greatly limited, and huge resource waste is caused. These have inspired us to develop a novel strategy and a nano-functional material using steel slag as a raw material, and improve the potential utilization value of steel slag. The invention researches the structure and component evolution of the steel slag, provides a strategy for converting the steel slag into an adsorbent and a catalyst with excellent performance, and realizes the high-efficiency utilization of the steel slag.
Disclosure of Invention
The invention aims to provide a method for constructing a nano functional material by utilizing all components of steel slag, which can greatly reduce the waste of steel slag resources, promote the development of industrial solid waste utilization and is expected to be applied in actual industry.
The purpose of the invention is realized by the following technical scheme:
the raw material used in the invention is the tailings of the steel plant, and the tailings can be used after being screened (0.45 mu m).
The invention provides a method for utilizing all components of steel slag and constructing a nano functional material, which is characterized by comprising the following steps of:
(1) Putting the steel slag into a salicylic acid-methanol solution, performing ultrasonic dispersion uniformly, performing magnetic stirring under a water bath condition, and performing solid-liquid separation, wherein the liquid is a calcium salicylate solution, and the solid is filter residue with the surface rich in Fe, mg and Al elements; wherein the concentration of the salicylic acid in the salicylic acid-methanol solution is preferably 80-120g/L, and each 15g of steel slag corresponds to 120-180mL of the salicylic acid-methanol solution; the temperature of the water bath is 25-35 ℃, and the heat preservation time is 12-24h;
(2) Adding the liquid obtained after solid-liquid separation in the step (1) into a mixed solution of sodium silicate and sodium hydroxide, and synthesizing an amorphous Calcium Silicate Hydrate (CSH) adsorbent by adopting a hydrothermal or water bath method; wherein the concentration of sodium silicate in the mixed solution of sodium silicate and sodium hydroxide is 3-4mol/L, the concentration of sodium hydroxide is 0.2-0.6mol/L, every 6mL of the liquid obtained after solid-liquid separation in the step (1) corresponds to 4-8mL of the mixed solution of sodium silicate and sodium hydroxide, the temperature of a hydrothermal or water bath method is 60-80 ℃, and the heat preservation time is 16-24 hours;
(3) Dispersing the solid obtained after solid-liquid separation in the step (1) into an oxalic acid solution, dissolving soluble metal ions in the oxalic acid solution in a water bath, and then carrying out solid-liquid separation, wherein the liquid is rich in soluble metal ions Mg 2+ 、Al 3+ And Fe 3+ The solid is calcium oxalate precipitation; wherein the concentration of the oxalic acid solution is 0.19-0.21mol/L, every 2.5g of the filter residue obtained in the step (1) corresponds to 180-220mL of the oxalic acid solution, the water bath temperature is 80-90 ℃, and the heat preservation time is 2-6h;
(4) Adding the solid obtained after solid-liquid separation in the step (3) into a trisodium phosphate dodecahydrate solution, and synthesizing a hydroxyapatite (Hap) adsorbent by adopting a hydrothermal method; wherein the concentration of the trisodium phosphate dodecahydrate solution is 1.9-4.5mol/L, and each 0.2g of the solid obtained after the solid-liquid separation in the step (3) corresponds to 20-40mL of the trisodium phosphate dodecahydrate solution; the temperature of the hydrothermal method is 140-180 ℃, and the heat preservation time is 2-6h;
(5) Dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate into the liquid obtained after solid-liquid separation in the step (3), adding sodium hydroxide to keep the pH value at 10-12, and then sequentially dropwise adding sodium carbonate and thioacetamide solutions, wherein each 30-50mL of the liquid obtained after solid-liquid separation in the step (3) corresponds to 3-4g of magnesium nitrate hexahydrate and 2-3g of aluminum nitrate nonahydrate5-10mL of hydrated aluminum nitrate, 5-10mL of sodium carbonate with the concentration of 0.2-0.4mol/L and 10-15mL of thioacetamide with the concentration of 0.134-0.67mol/L, and synthesizing the layered double hydroxide (FeS-LDH-CO) loaded with the ferric sulfide by adopting a hydrothermal method 3 ) The temperature of the composite material by a hydrothermal method is 180-200 ℃, and the heat preservation time is 12-24h; finally, a green layered double hydroxide is obtained, wherein green is the color of iron sulfide.
The beneficial effects of the invention are: the nano functional material obtained by the invention has better removal performance on heavy metal ions in the environment, and the product obtained by the preparation method has good repeatability, simple operation and low cost. Has better application prospect in the fields of full utilization of solid waste steel slag and environmental pollution treatment.
Drawings
FIG. 1: iron sulfide-loaded layered double hydroxide (FeS-LDH-CO) obtained in example 1 3 ) An X-ray diffraction pattern of the composite powder;
FIG. 2: iron sulfide-loaded layered double hydroxide (FeS-LDH-CO) obtained in example 1 3 ) Transmission electron microscopy of the composite powder;
FIG. 3: iron sulfide-loaded layered double hydroxide (FeS-LDH-CO) obtained in example 2 3 ) An X-ray diffraction pattern of the composite powder;
FIG. 4 is a schematic view of: iron sulfide Supported layered double hydroxide (FeS-LDH-CO) obtained in example 3 3 ) X-ray diffraction pattern of the composite powder.
FIG. 5: iron sulfide-loaded layered double hydroxide (FeS-LDH-CO) obtained in example 3 3 ) Raman spectrum of the composite material powder.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
1. Dispersing 15g of steel slag into 150mL,100g/L salicylic acid-methanol solution, ultrasonically dispersing, transferring the suspension into a water bath at 30 ℃, preserving the temperature for 18h under magnetic stirring (300 rpm), and then carrying out solid-liquid separation to respectively obtain filter residue and filtrate for later use.
2. In the polytetrafluoroethylene lining, 0.9g of sodium silicate nonahydrate is firstly dissolved in 6mL of sodium hydroxide solution with the concentration of 6.4 mol/L, magnetic stirring is carried out for 20min, then 6mL of filtrate obtained in the step (1) is dropwise added, stirring is carried out for 20min again, the temperature is increased to 80 ℃ along with the furnace, and the temperature is kept for 16.5h. The powder is synthesized, washed by distilled water and ethanol, and placed in an oven to be dried at 60 ℃ overnight, and then the amorphous Calcium Silicate Hydrate (CSH) adsorbent is obtained.
3. And (2.5) dispersing the filter residue obtained in the step (1) into 200mL of 125g/L oxalic acid solution, ultrasonically dispersing, transferring the suspension into a water bath at 90 ℃, keeping the temperature for 2 hours under magnetic stirring (300 rpm), and then carrying out solid-liquid separation to obtain the filter residue and filtrate for later use.
4. And (4) dissolving 0.6g of sodium phosphate dodecahydrate in 30mL of aqueous solution in the polytetrafluoroethylene lining, continuously stirring for 20min, then adding 0.2g of filter residue collected in the step (3), uniformly dispersing by ultrasonic, stirring for 20min again, heating to 160 ℃ along with a furnace, and preserving heat for 6h. The powder is cleaned by distilled water and ethanol after being synthesized, and is placed in an oven to be dried overnight at 60 ℃, and then the Hydroxyapatite (Hydroxyapatite) adsorbent is obtained.
5. 40mL of the filtrate obtained in step (3) was added to the polytetrafluoroethylene liner, followed by 3.7g of Mg (NO) each 3 ) 2 And 2.4gAl (NO) 3 ) 3 The resulting mixture was dissolved in NaOH (5 g) to maintain the pH of the mixture at 10. Then sequentially dropwise adding 5ml of 0.2mol/L NaCO 3 Mixing the solution with 10mL of thioacetamide solution with the concentration of 0.67mol/L, magnetically stirring the mixed solution for 20min, heating to 180 ℃ along with a furnace, and preserving the temperature for 12h. The powder is cleaned by distilled water and ethanol after being synthesized and is placed in an oven to be dried at 60 ℃ overnight, and then the layered double hydroxide (FeS-LDH-CO) loaded with ferric sulfide is obtained 3 )。
Example 2
1. Dispersing 15g of steel slag into 150mL,100g/L salicylic acid-methanol solution, ultrasonically dispersing, transferring the suspension into a water bath at 30 ℃, preserving the temperature for 18h under magnetic stirring (300 rpm), and then carrying out solid-liquid separation to respectively obtain filter residue and filtrate for later use.
2. In the polytetrafluoroethylene lining, 0.9g of sodium silicate nonahydrate is firstly dissolved in 6mL of 0.4mol/L sodium hydroxide solution, magnetic stirring is carried out for 20min, then 8mL of filtrate obtained in the step (1) is dropwise added, stirring is carried out for 20min again, and heat preservation is carried out in a water bath at 80 ℃ for 16.5h. The powder is synthesized, washed by distilled water and ethanol, and placed in an oven to be dried at 60 ℃ overnight, and then the amorphous Calcium Silicate Hydrate (CSH) adsorbent is obtained.
3. And (2.5) dispersing the filter residue obtained in the step (1) into 200mL of 125g/L oxalic acid solution, ultrasonically dispersing, transferring the suspension into a water bath at 90 ℃, keeping the temperature for 4 hours under magnetic stirring (300 rpm), and then carrying out solid-liquid separation to respectively obtain the filter residue and filtrate for later use.
4. Dissolving 1.0g of sodium phosphate dodecahydrate in 30mL of aqueous solution in a polytetrafluoroethylene lining, continuously stirring for 20min, then adding 0.2g of filter residue collected in the step (3), ultrasonically dispersing uniformly, stirring for 20min again, heating to 160 ℃ along with a furnace, and preserving heat for 2h. The powder is cleaned by distilled water and ethanol after being synthesized, and is placed in an oven to be dried overnight at 60 ℃, and then the Hydroxyapatite (Hydroxyapatite) adsorbent is obtained.
5. 40mL of the filtrate obtained in step (3) was added to a polytetrafluoroethylene liner, and then 3.7g of Mg (NO) was added thereto 3 ) 2 And 2.4gAl (NO) 3 ) 3 The resulting mixed solution was dissolved in NaOH (5 g) to maintain the pH of the mixed solution at 10. Then sequentially dropwise adding 5ml of 0.2mol/L NaCO 3 The solution and 10mL of 0.67mol/L thioacetamide solution, then the mixed solution is magnetically stirred for 20min, the temperature is raised to 180 ℃ along with a furnace, and the temperature is kept for 24h. The powder is cleaned by distilled water and ethanol after being synthesized and is placed in an oven to be dried at 60 ℃ overnight, and then the layered double hydroxide (FeS-LDH-CO) loaded with ferric sulfide is obtained 3 )。
Example 3
1. Dispersing 15g of steel slag into 150mL of 100g/L salicylic acid-methanol solution, ultrasonically dispersing, transferring the suspension into a water bath at 30 ℃, preserving heat for 18 hours under magnetic stirring (300 rpm), and then carrying out solid-liquid separation to obtain filter residue and filtrate respectively for later use.
2. In the polytetrafluoroethylene lining, 0.9g of sodium silicate nonahydrate is firstly dissolved in 6mL of 0.4mol/L sodium hydroxide solution, magnetic stirring is carried out for 20min, then 8mL of filtrate obtained in the step (1) is dropwise added, stirring is carried out for 20min again, and heat preservation is carried out in a water bath at 80 ℃ for 16.5h. The powder is synthesized, washed by distilled water and ethanol, and dried in an oven at 60 ℃ overnight to obtain the amorphous Calcium Silicate Hydrate (CSH) adsorbent.
3. And (2.5) dispersing the filter residue obtained in the step (1) into 200mL (130g/L) oxalic acid solution, performing ultrasonic dispersion, transferring the suspension into a water bath at 90 ℃, performing heat preservation for 2 hours under magnetic stirring (300 rpm), and performing solid-liquid separation to obtain the filter residue and filtrate for later use.
4. Dissolving 1.4g of sodium phosphate dodecahydrate in 30mL of aqueous solution in a polytetrafluoroethylene lining, continuously stirring for 20min, then adding 0.2g of filter residue collected in the step (3), ultrasonically dispersing uniformly, stirring for 20min again, heating to 160 ℃ along with a furnace, and preserving heat for 6h. The powder is cleaned by distilled water and ethanol after being synthesized, and is placed in an oven to be dried overnight at 60 ℃, and then the Hydroxyapatite (Hydroxyapatite) adsorbent is obtained.
5. 40mL of the filtrate obtained in step (3) was added to a polytetrafluoroethylene liner, and then 3.7g of Mg (NO) was added thereto, respectively 3 ) 2 And 2.4gAl (NO) 3 ) 3 The resulting mixed solution was dissolved in NaOH (5 g) to maintain the pH of the mixed solution at 12. Then sequentially dropwise adding 5ml of 0.2mol/L NaCO 3 The solution and 10mL of 0.67mol/L thioacetamide solution, then the mixed solution is magnetically stirred for 20min, the temperature is raised to 180 ℃ along with a furnace, and the temperature is kept for 24h. The powder is cleaned by distilled water and ethanol after being synthesized, and is placed in a drying oven to be dried at 60 ℃ overnight, and then the layered double hydroxide (FeS-LDH-CO) loaded by ferric sulfide is obtained 3 )。
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A method for utilizing all components of steel slag and constructing a nano functional material is characterized by comprising the following steps:
(1) Putting the steel slag into a salicylic acid-methanol solution, performing ultrasonic dispersion uniformly, performing magnetic stirring under a water bath condition, and performing solid-liquid separation, wherein the liquid is a calcium salicylate solution, and the solid is filter residue with the surface rich in Fe, mg and Al elements;
(2) Adding the liquid obtained after solid-liquid separation in the step (1) into a mixed solution of sodium silicate and sodium hydroxide, and synthesizing an amorphous Calcium Silicate Hydrate (CSH) adsorbent by adopting a hydrothermal or water bath method;
(3) Dispersing the solid obtained after solid-liquid separation in the step (1) into an oxalic acid solution, dissolving soluble metal ions in the oxalic acid solution in a water bath, and then carrying out solid-liquid separation, wherein the liquid is rich in soluble metal ions Mg 2+ 、Al 3+ And Fe 3+ The solid is calcium oxalate precipitation;
(4) And (4) adding the solid obtained after solid-liquid separation in the step (3) into a trisodium phosphate dodecahydrate solution, and synthesizing a hydroxyapatite (Hap) adsorbent by adopting a hydrothermal method.
(5) Dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate into the liquid obtained after solid-liquid separation in the step (3), adding sodium hydroxide, keeping the pH value at 10-12, then sequentially adding sodium carbonate and thioacetamide solution dropwise, and synthesizing the layered double hydroxide (FeS-LDH-CO) loaded with ferric sulfide by adopting a hydrothermal method 3 ) A composite material.
2. The method for utilizing and constructing the nano functional material by the full components of the steel slag according to the claim 1, wherein the concentration of the salicylic acid in the salicylic acid-methanol solution in the step (1) is 80-120g/L, and each 15g of the steel slag corresponds to 120-180mL of the salicylic acid-methanol solution; the temperature of the water bath is 25-35 ℃, and the heat preservation time is 12-24h.
3. The method for utilizing and constructing the nano functional material by the whole components of the steel slag according to claim 1, wherein the concentration of the sodium silicate in the mixed solution of the sodium silicate and the sodium hydroxide in the step (2) is 3-4mol/L, the concentration of the sodium hydroxide is 0.2-0.6mol/L, each 6mL of the liquid obtained after the solid-liquid separation in the step (1) corresponds to 4-8mL of the mixed solution of the sodium silicate and the sodium hydroxide, the temperature of the hydrothermal or water bath method is 60-80 ℃, and the heat preservation time is 16-24h.
4. The method for utilizing and constructing the nano functional material by the whole components of the steel slag according to claim 1, wherein the concentration of the oxalic acid solution in the step (3) is 0.19-0.21mol/L, each 2.5g of the filter residue obtained in the step (1) corresponds to 180-220mL of the oxalic acid solution, the water bath temperature is 80-90 ℃, and the heat preservation time is 2-6h.
5. The method for utilizing and constructing nano-functional materials based on the full components of steel slag as claimed in claim 1, wherein the concentration of the trisodium phosphate dodecahydrate solution in step (4) is 1.9-4.5mol/L, and each 0.2g of the solid after solid-liquid separation in step (3) corresponds to 20-40mL of the trisodium phosphate dodecahydrate solution; the temperature of the hydrothermal method is 140-180 ℃, and the heat preservation time is 2-6h.
6. The method for utilizing and constructing a nano-functional material from all components of steel slag according to claim 1, wherein in the step (5), magnesium nitrate hexahydrate and aluminum nitrate nonahydrate are dissolved in the liquid obtained after the solid-liquid separation in the step (3), sodium hydroxide is added to maintain the pH value at 10-12, then sodium carbonate and thioacetamide solution are sequentially added dropwise, wherein each 30-50mL of the liquid obtained after the solid-liquid separation in the step (3) corresponds to 3-4g of magnesium nitrate hexahydrate, 2-3g of aluminum nitrate nonahydrate, 5-10mL of sodium carbonate with the concentration of 0.2-0.4mol/L and 10-15mL of thioacetamide with the concentration of 0.134-0.67mol/L, and iron sulfide-loaded layered double hydroxide (FeS-LDH-CO) is synthesized by a hydrothermal method 3 ) The temperature of the composite material by a hydrothermal method is 180-200 ℃, and the heat preservation time is 12-24h; finally, a green layered double hydroxide is obtained, wherein green is the color of iron sulfide.
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| CN103539242A (en) * | 2013-10-15 | 2014-01-29 | 包头稀土研究院 | Method used for reducing calcium content of rare earth industrial wastewater |
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| CN103539242A (en) * | 2013-10-15 | 2014-01-29 | 包头稀土研究院 | Method used for reducing calcium content of rare earth industrial wastewater |
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