CN115180655B - 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
- Publication number
- CN115180655B CN115180655B CN202210834760.7A CN202210834760A CN115180655B CN 115180655 B CN115180655 B CN 115180655B CN 202210834760 A CN202210834760 A CN 202210834760A CN 115180655 B CN115180655 B CN 115180655B
- Authority
- CN
- China
- Prior art keywords
- solid
- steel slag
- solution
- liquid
- liquid separation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 36
- 239000002893 slag Substances 0.000 title claims abstract description 36
- 239000010959 steel Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 title claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 13
- 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 8
- 239000008204 material by function Substances 0.000 claims abstract description 8
- 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
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 6
- 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 6
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 42
- 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 31
- 238000000926 separation method Methods 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 12
- 235000006408 oxalic acid Nutrition 0.000 claims description 11
- 238000003756 stirring Methods 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
- 238000004321 preservation Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 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
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 claims description 5
- 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
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAAHAAMILDNBPS-UHFFFAOYSA-L calcium hydrogenphosphate dihydrate Chemical compound O.O.[Ca+2].OP([O-])([O-])=O XAAHAAMILDNBPS-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
- 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 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
- 239000002244 precipitate Substances 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
- 239000007790 solid phase Substances 0.000 abstract 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract 1
- 150000007524 organic acids Chemical class 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
- 239000000843 powder Substances 0.000 description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- 239000012153 distilled water Substances 0.000 description 9
- 238000003760 magnetic stirring Methods 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
- 238000002441 X-ray diffraction Methods 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
- 238000002360 preparation method Methods 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 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000001000 micrograph 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
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A method for utilizing and constructing nano functional materials by using all components of steel slag belongs to the field of solid waste recycling. The steel slag components are subjected to 'diversion' and 'recombination' based on the steel slag structure, and the nano functional material is prepared for purifying sewage. Preparing two adsorbents of hydrated calcium silicate and hydroxyapatite respectively by extracting a liquid-solid phase rich in calcium by using an organic acid with weaker acidity, and then using a liquid-solid phase rich in Mg 2+ 、Al 3+ And Fe (Fe) 3+ The layered double hydroxide loaded by iron sulfide is prepared from the filtrate of metal ions, so that the full-component utilization of steel slag is realized, and the amount of waste slag is reduced to the minimum. The work provides a simple, popular and environment-friendly strategy, fully avoids the disadvantage of complex steel slag components, 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, development and construction of novel functional nanomaterials using raw materials, particularly industrial solid waste materials, which have a great application potential, at low cost, easy availability and large reserves have been actively encouraged. The steel slag is a byproduct generated in the steelmaking process, is a heterogeneous waste taking Fe, mg, al and Ca as main components, and has great application potential to prepare the nano-functional composite material with excellent performance. Although the utilization advantage of the steel slag is obvious, it is very difficult to fully utilize all the components of the steel slag to reduce the resource waste as much as possible due to the complex component characteristics, so that the high-efficiency utilization of the steel slag is greatly limited, and huge resource waste is caused. These all inspire us to develop novel strategies and nano-functional materials with steel slag as raw materials, and improve the potential utilization value of the steel slag. The invention researches the structure and component evolution of steel slag, and provides a strategy for converting the steel slag into an adsorbent and a catalyst with excellent performance, so that the high-efficiency utilization of the steel slag is realized.
Disclosure of Invention
The invention aims to provide a method for constructing nano functional materials by utilizing full components of steel slag, which can greatly reduce waste of steel slag resources and promote development of industrial solid waste utilization, and is expected to be applied to practical industry.
The aim of the invention is realized by the following technical scheme:
the raw material used in the invention is steel mill tailings, and the tailings can be used after sieving (0.45 mu m) treatment.
The invention provides a method for utilizing and constructing a nano functional material by using all components of steel slag, which is characterized by comprising the following steps:
(1) Placing the steel slag into salicylic acid-methanol solution for ultrasonic dispersion uniformly, magnetically stirring under the water bath condition, and then carrying out solid-liquid separation, wherein the liquid is calcium salicylate solution, and the solid is filter residue with the surface rich in Fe, mg and Al elements; wherein, the concentration of salicylic acid in salicylic acid-methanol solution is preferably 80-120g/L, and each 15g of steel slag corresponds to 120-180mL of salicylic acid-methanol solution; the temperature of the water bath is 25-35 ℃, and the heat preservation time is 12-24 hours;
(2) Adding the liquid 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, each 6mL of liquid 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 after solid-liquid separation in the step (1) into oxalic acid solution, dissolving soluble metal ions in the oxalic acid solution in water bath, and then carrying out solid-liquid separation, wherein the liquid is rich in soluble metal ions Mg 2+ 、Al 3+ And Fe (Fe) 3+ The solid is a brushite precipitate; wherein the concentration of the oxalic acid solution is 0.19-0.21mol/L, each 2.5g of filter residue obtained in the step (1) corresponds to 180-220mL of oxalic acid solution, the water bath temperature is 80-90 ℃, and the heat preservation time is 2-6h;
(4) Adding the solid after solid-liquid separation in the step (3) into 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 after solid-liquid separation in the step (3) corresponds to 20-40mL of 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 after solid-liquid separation in the step (3), adding sodium hydroxide to keep the pH value at 10-12, then sequentially and dropwise adding sodium carbonate and thioacetamide solution, wherein each 30-50mL of the liquid after solid-liquid separation in the step (3) corresponds to 3-4g of magnesium nitrate hexahydrate, 2-3g of aluminum nitrate nonahydrate, the concentration of 0.2-0.4mol/L sodium carbonate is 5-10mL, the concentration of 0.134-0.67mol/L thioacetamide is 10-15mL, and synthesizing the layered double hydroxide (FeS-LDH-CO) loaded with iron sulfide by adopting a hydrothermal method 3 ) The temperature of the composite material in the hydrothermal method is 180-200 ℃, and the heat preservation time is 12-24 hours; finally, the green layered double hydroxide is obtained, wherein the green color is the color of the ferric sulfide.
The beneficial effects of the invention are as follows: the nano functional material obtained by the preparation method has good 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 field of solid waste steel slag full utilization and environmental pollution treatment.
Drawings
Fig. 1: iron sulfide Loading obtained in example 1Layered double hydroxides (FeS-LDH-CO) 3 ) An X-ray diffraction pattern of the composite powder;
fig. 2: iron sulfide-supported layered double hydroxide (FeS-LDH-CO) obtained in example 1 3 ) A transmission electron microscope image of the composite material powder;
fig. 3: iron sulfide-supported layered double hydroxide (FeS-LDH-CO) obtained in example 2 3 ) An X-ray diffraction pattern of the composite powder;
fig. 4: iron sulfide-supported layered double hydroxide (FeS-LDH-CO) obtained in example 3 3 ) X-ray diffraction pattern of composite powder.
Fig. 5: iron sulfide-supported layered double hydroxide (FeS-LDH-CO) obtained in example 3 3 ) Raman spectrum of the composite powder.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
1. 15g of steel slag is dispersed into 150mL of 100g/L salicylic acid-methanol solution, after ultrasonic dispersion, the suspension is transferred into a water bath at 30 ℃, the temperature is kept for 18 hours under magnetic stirring (300 rpm), and then the filter residue and filtrate are respectively obtained through solid-liquid separation for standby.
2. In a polytetrafluoroethylene lining, firstly, 0.9g of sodium silicate nonahydrate is dissolved in 6mL of 0.4mol/L sodium hydroxide solution, magnetic stirring is carried out for 20min, then 6mL of filtrate obtained in the step (1) is added dropwise, stirring is carried out for 20min again, the temperature is raised to 80 ℃ along with the furnace, and the temperature is kept for 16.5h. After the powder is synthesized, the powder is washed by distilled water and ethanol, and is dried in an oven at 60 ℃ for overnight, thus obtaining the amorphous Calcium Silicate Hydrate (CSH) adsorbent.
3. 2.5g of the filter residue obtained in the step (1) is dispersed into 200mL of 125g/L oxalic acid solution, after ultrasonic dispersion, the suspension is transferred into a water bath with the temperature of 90 ℃, the temperature is kept for 2 hours under magnetic stirring (300 rpm), and then the filter residue and filtrate are respectively obtained through solid-liquid separation for standby.
4. Dissolving 0.6g of sodium phosphate dodecahydrate in 30mL of aqueous solution in a polytetrafluoroethylene lining, continuously stirring for 20min, 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. After the powder is synthesized, the powder is washed by distilled water and ethanol, and is dried overnight in an oven at 60 ℃ to obtain the Hydroxyapatite (hydroxypatite) adsorbent.
5. 40mL of the filtrate obtained in the step (3) was first added to a polytetrafluoroethylene liner, followed by 3.7g of Mg (NO) 3 ) 2 And 2.4g Al (NO) 3 ) 3 In this, 5g of NaOH was added to the resulting mixed solution to maintain the pH of the mixed solution at 10. Then 5ml of NaCO 0.2mol/L are added dropwise in sequence 3 The solution and 10mL of 0.67mol/L thioacetamide solution are stirred magnetically for 20min, and the temperature is raised to 180 ℃ along with the furnace, and the temperature is kept for 12h. After the powder is synthesized, the powder is washed by distilled water and ethanol, and is dried in an oven at 60 ℃ for overnight, and then the layered double hydroxide (FeS-LDH-CO) loaded by iron sulfide is obtained 3 )。
Example 2
1. 15g of steel slag is dispersed into 150mL of 100g/L salicylic acid-methanol solution, after ultrasonic dispersion, the suspension is transferred into a water bath at 30 ℃, the temperature is kept for 18 hours under magnetic stirring (300 rpm), and then the filter residue and filtrate are respectively obtained through solid-liquid separation for standby.
2. In a polytetrafluoroethylene lining, firstly, 0.9g of sodium silicate nonahydrate is dissolved in 6mL of 0.4mol/L sodium hydroxide solution, magnetic stirring is carried out for 20min, then 8mL of the filtrate obtained in the step (1) is added dropwise, stirring is carried out for 20min again, and the temperature is kept in a water bath at 80 ℃ for 16.5h. After the powder is synthesized, the powder is washed by distilled water and ethanol, and is dried in an oven at 60 ℃ for overnight, thus obtaining the amorphous Calcium Silicate Hydrate (CSH) adsorbent.
3. 2.5g of the filter residue obtained in the step (1) is dispersed into 200mL of 125g/L oxalic acid solution, after ultrasonic dispersion, the suspension is transferred into a water bath with the temperature of 90 ℃, the temperature is kept for 4 hours under magnetic stirring (300 rpm), and then the filter residue and filtrate are respectively obtained through solid-liquid separation for standby.
4. In the polytetrafluoroethylene lining, firstly, 1.0g of sodium phosphate dodecahydrate is dissolved in 30mL of water solution, the stirring is continued for 20min, then 0.2g of filter residue collected in the step (3) is added, the ultrasonic dispersion is uniform, the stirring is continued for 20min, the temperature is raised to 160 ℃ along with the furnace, and the heat is preserved for 2h. After the powder is synthesized, the powder is washed by distilled water and ethanol, and is dried overnight in an oven at 60 ℃ to obtain the Hydroxyapatite (hydroxypatite) adsorbent.
5. 40mL of the filtrate obtained in the step (3) was first added to a polytetrafluoroethylene liner, followed by 3.7g of Mg (NO) 3 ) 2 And 2.4g Al (NO) 3 ) 3 In this, 5g of NaOH was added to the resulting mixed solution to maintain the pH of the mixed solution at 10. Then 5ml of NaCO 0.2mol/L are added dropwise in sequence 3 The solution and 10mL of 0.67mol/L thioacetamide solution are stirred magnetically for 20min, and the temperature is raised to 180 ℃ along with the furnace, and the temperature is kept for 24h. After the powder is synthesized, the powder is washed by distilled water and ethanol, and is dried in an oven at 60 ℃ for overnight, and then the layered double hydroxide (FeS-LDH-CO) loaded by iron sulfide is obtained 3 )。
Example 3
1. 15g of steel slag is dispersed into 150mL of 100g/L salicylic acid-methanol solution, after ultrasonic dispersion, the suspension is transferred into a water bath at 30 ℃, the temperature is kept for 18 hours under magnetic stirring (300 rpm), and then the filter residue and filtrate are respectively obtained through solid-liquid separation for standby.
2. In a polytetrafluoroethylene lining, firstly, 0.9g of sodium silicate nonahydrate is dissolved in 6mL of 0.4mol/L sodium hydroxide solution, magnetic stirring is carried out for 20min, then 8mL of the filtrate obtained in the step (1) is added dropwise, stirring is carried out for 20min again, and the temperature is kept in a water bath at 80 ℃ for 16.5h. After the powder is synthesized, the powder is washed by distilled water and ethanol, and is dried in an oven at 60 ℃ for overnight, thus obtaining the amorphous Calcium Silicate Hydrate (CSH) adsorbent.
3. 2.5g of the filter residue obtained in the step (1) is dispersed into 200mL of 130g/L oxalic acid solution, after ultrasonic dispersion, the suspension is transferred into a water bath with the temperature of 90 ℃, the temperature is kept for 2 hours under magnetic stirring (300 rpm), and then the filter residue and filtrate are respectively obtained through solid-liquid separation for standby.
4. In the polytetrafluoroethylene lining, firstly, 1.4g of sodium phosphate dodecahydrate is dissolved in 30mL of water solution, the stirring is continued for 20min, then 0.2g of filter residue collected in the step (3) is added, the ultrasonic dispersion is uniform, the stirring is continued for 20min, the temperature is raised to 160 ℃ along with the furnace, and the heat is preserved for 6h. After the powder is synthesized, the powder is washed by distilled water and ethanol, and is dried overnight in an oven at 60 ℃ to obtain the Hydroxyapatite (hydroxypatite) adsorbent.
5. 40mL of the filtrate obtained in the step (3) was first added to a polytetrafluoroethylene liner, followed by 3.7g of Mg (NO) 3 ) 2 And 2.4g Al (NO) 3 ) 3 To the resulting mixed solution was dissolved 5g of NaOH, and the pH of the mixed solution was kept at 12. Then 5ml of NaCO 0.2mol/L are added dropwise in sequence 3 The solution and 10mL of 0.67mol/L thioacetamide solution are stirred magnetically for 20min, and the temperature is raised to 180 ℃ along with the furnace, and the temperature is kept for 24h. After the powder is synthesized, the powder is washed by distilled water and ethanol, and is dried in an oven at 60 ℃ for overnight, and then the layered double hydroxide (FeS-LDH-CO) loaded by iron sulfide is obtained 3 )。
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and all such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (6)
1. The method for utilizing and constructing the nano functional material by using the whole components of the steel slag is characterized by comprising the following steps of:
(1) Placing the steel slag into salicylic acid-methanol solution for ultrasonic dispersion uniformly, magnetically stirring under the water bath condition, and then carrying out solid-liquid separation, wherein the liquid is calcium salicylate solution, and the solid is filter residue with the surface rich in Fe, mg and Al elements;
(2) Adding the liquid 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 after solid-liquid separation in the step (1) into oxalic acid solution, dissolving soluble metal ions in the oxalic acid solution in water bath, and then carrying out solid-liquid separation, wherein the liquid is rich in soluble metal ions Mg 2+ 、Al 3+ And Fe (Fe) 3+ The solid is a brushite precipitate;
(4) Adding the solid after solid-liquid separation in the step (3) into trisodium phosphate dodecahydrate solution, and synthesizing a hydroxyapatite (Hap) adsorbent by adopting a hydrothermal method;
(5) Dissolving magnesium nitrate hexahydrate and aluminum nitrate nonahydrate in the liquid obtained after solid-liquid separation in the step (3), adding sodium hydroxide, keeping the pH value to be 10-12, then sequentially and dropwise adding sodium carbonate and thioacetamide solution, and synthesizing the iron sulfide supported layered double hydroxide (FeS-LDH-CO) by adopting a hydrothermal method 3 ) A composite material.
2. The method for utilizing and constructing nano functional materials from steel slag according to claim 1, wherein the concentration of salicylic acid in the salicylic acid-methanol solution in the step (1) is 80-120g/L, and each 15g of steel slag corresponds to 120-180mL of 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 using the steel slag full components according to claim 1, wherein the concentration of sodium silicate in the mixed solution of sodium silicate and sodium hydroxide in the step (2) is 3-4mol/L, the concentration of sodium hydroxide is 0.2-0.6mol/L, each 6mL of the liquid 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 16-24h.
4. The method for utilizing and constructing nano functional materials from 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 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 from full components of steel slag according to claim 1, wherein the concentration of trisodium phosphate dodecahydrate solution in the step (4) is 1.9-4.5mol/L, and each 0.2g of solid after solid-liquid separation in the step (3) corresponds to 20-40mL of 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 nano functional materials according to the whole components of steel slag as claimed in claim 1, wherein the step (5) is to dissolve magnesium nitrate hexahydrate and aluminum nitrate nonahydrate into the liquid after solid-liquid separation in the step (3), add sodium hydroxide to maintain pH10-12, then sequentially add sodium carbonate and thioacetamide solution dropwise, wherein each 30-50mL of the liquid after solid-liquid separation in the step (3) corresponds to 3-4g of magnesium nitrate hexahydrate, 2-3g of aluminum nitrate nonahydrate, the concentration is 0.2-0.4mol/L sodium carbonate 5-10mL, the concentration is 0.134-0.67mol/L thioacetamide 10-15mL, and the layered double hydroxide (FeS-LDH-CO) loaded with iron sulfide is synthesized by a hydrothermal method 3 ) The temperature of the composite material in the hydrothermal method is 180-200 ℃, and the heat preservation time is 12-24 hours; finally, the green layered double hydroxide is obtained, wherein the green color is the color of the ferric sulfide.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210834760.7A CN115180655B (en) | 2022-07-14 | 2022-07-14 | Method for utilizing all components of steel slag and constructing nano functional material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210834760.7A CN115180655B (en) | 2022-07-14 | 2022-07-14 | Method for utilizing all components of steel slag and constructing nano functional material |
Publications (2)
Publication Number | Publication Date |
---|---|
CN115180655A CN115180655A (en) | 2022-10-14 |
CN115180655B true CN115180655B (en) | 2023-09-12 |
Family
ID=83519651
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210834760.7A Active CN115180655B (en) | 2022-07-14 | 2022-07-14 | Method for utilizing all components of steel slag and constructing nano functional material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115180655B (en) |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN104860325A (en) * | 2015-05-07 | 2015-08-26 | 石家庄学院 | Pectolite nano fiber and preparation method thereof |
CN106268572A (en) * | 2016-07-16 | 2017-01-04 | 沈阳理工大学 | A kind of method preparing layered hydroxide for raw material with solid waste |
CN108584969A (en) * | 2018-04-04 | 2018-09-28 | 南方科技大学 | Preparation method of hydrated calcium silicate nanosheet |
CN109205582A (en) * | 2018-10-22 | 2019-01-15 | 南昌航空大学 | A kind of method that presoma conversion prepares nano-pore hydroxyapatite |
-
2022
- 2022-07-14 CN CN202210834760.7A patent/CN115180655B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN104860325A (en) * | 2015-05-07 | 2015-08-26 | 石家庄学院 | Pectolite nano fiber and preparation method thereof |
CN106268572A (en) * | 2016-07-16 | 2017-01-04 | 沈阳理工大学 | A kind of method preparing layered hydroxide for raw material with solid waste |
CN108584969A (en) * | 2018-04-04 | 2018-09-28 | 南方科技大学 | Preparation method of hydrated calcium silicate nanosheet |
CN109205582A (en) * | 2018-10-22 | 2019-01-15 | 南昌航空大学 | A kind of method that presoma conversion prepares nano-pore hydroxyapatite |
Non-Patent Citations (1)
Title |
---|
In-situ constructing nanostructured magnesium ferrite on steel slag for Cr(VI) photoreduction;Lingmin Sun等;《Journal of Hazardous Materials》;第126951页 * |
Also Published As
Publication number | Publication date |
---|---|
CN115180655A (en) | 2022-10-14 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108837803A (en) | A kind of layered double-hydroxide loads the preparation method of biological carbon composite | |
CN102516607B (en) | Preparation method of magnetic rectorite/chitosan nano-grade composite material | |
CN103877927B (en) | Magnetic Nano Fe 3o 4living things catalysis prepares method and the application in uranium-containing waste water process thereof | |
CN103119763B (en) | Method of preparing olivine cathod material for lithium secondary battery | |
CN113044823B (en) | Iron phosphate material and preparation method and application thereof | |
CN106946382B (en) | A kind of environment-friendly treatment method of heavy metal chromium ion waste water | |
CN114700097B (en) | Fe 2 O 3 -MXenes composite catalyst and preparation method and application thereof | |
Ji et al. | A review of metallurgical slag for efficient wastewater treatment: Pretreatment, performance and mechanism | |
CN101343152A (en) | Strontium calcium aluminium sulphate cement | |
CN115180655B (en) | Method for utilizing all components of steel slag and constructing nano functional material | |
CN101289474B (en) | Process for preparing humic acid from residue after extraction of coal humic acid | |
CN110639535B (en) | Modification method of industrial waste red mud and high-value environment-friendly application | |
CN110394154B (en) | Preparation method and application of moso bamboo charcoal/FeMn-LDH composite material | |
CN100431722C (en) | Electroplating sludge hydrothermal ferritizing treating method | |
CN110302746A (en) | It is a kind of for hexavalent chromium polluted water or the composite material and preparation method of soil remediation | |
CN102153061B (en) | Method for synthesizing ferric phosphate material | |
CN103803662A (en) | Method for preparing solid polymeric aluminum ferric sulfate by use of bauxite oxide | |
CN102583495B (en) | Preparation method of rare earth metal ion doping cerium oxide nanometer material | |
Amarray et al. | Reduction of cadmium content in 29% and 54% P2O5 phosphoric acid by manganese oxide material birnessite-type Na-MnO2 | |
CN102001710B (en) | Method for preparing hollow urchin-shaped alpha-basic iron oxide | |
CN110194463B (en) | Halloysite-ferrite composite material and preparation method thereof | |
CN103420387B (en) | Tubular clay mineral-magnetic metal nano composite and preparation method thereof | |
CN113413873A (en) | Preparation method of load type sludge-based biomass charcoal adsorbent | |
CN103073043A (en) | Method for increasing growth of titanium dioxide gypsum particle crystals | |
CN103447054B (en) | Manganese magnetic solid acid catalyst preparation method and manganese magnetic solid acid catalyst |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |