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 PDF

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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
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王金淑
孙领民
吴俊书
杜玉成
李永利
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Beijing University of Technology
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    • 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
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    • 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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    • C01B25/00—Phosphorus; Compounds thereof
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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

Method for utilizing all components of steel slag and constructing nano functional material
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.
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