CN113797884A - Steel slag/fly ash composite waste slag porous adsorption material, preparation method and application - Google Patents
Steel slag/fly ash composite waste slag porous adsorption material, preparation method and application Download PDFInfo
- Publication number
- CN113797884A CN113797884A CN202111160743.1A CN202111160743A CN113797884A CN 113797884 A CN113797884 A CN 113797884A CN 202111160743 A CN202111160743 A CN 202111160743A CN 113797884 A CN113797884 A CN 113797884A
- Authority
- CN
- China
- Prior art keywords
- slag
- fly ash
- steel slag
- porous
- preparation
- 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.)
- Pending
Links
- 239000002893 slag Substances 0.000 title claims abstract description 151
- 239000000463 material Substances 0.000 title claims abstract description 98
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 90
- 239000010959 steel Substances 0.000 title claims abstract description 90
- 239000010881 fly ash Substances 0.000 title claims abstract description 87
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 61
- 239000010786 composite waste Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000011148 porous material Substances 0.000 claims abstract description 41
- 239000002699 waste material Substances 0.000 claims abstract description 37
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 230000000694 effects Effects 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 230000005284 excitation Effects 0.000 claims description 14
- 239000002002 slurry Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 12
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 8
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000010812 mixed waste Substances 0.000 claims description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 3
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000002910 solid waste Substances 0.000 abstract description 10
- 239000003463 adsorbent Substances 0.000 abstract description 5
- 239000002351 wastewater Substances 0.000 abstract description 4
- 239000010883 coal ash Substances 0.000 abstract description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 2
- 229910052708 sodium Inorganic materials 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 13
- 230000001276 controlling effect Effects 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 230000001360 synchronised effect Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000010310 metallurgical process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Images
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
- 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
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4893—Residues derived from used synthetic products, e.g. rubber from used tyres
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
A steel slag/fly ash composite waste residue porous adsorption material, a preparation method and application belong to the technical field of green preparation of solid waste adsorption materials. The adsorbing material is of an amorphous structure, and the surface of the adsorbing material is provided with a micro-nano pore structure. The preparation method comprises the steps of crushing and mixing the metallurgical waste residue, preparing a potassium hydroxide/sodium excited sol solution, and forming, granulating and dealkalizing the steel slag/fly ash composite waste residue porous material. According to the invention, the coal ash, the slag and the steel slag are used as reaction raw materials in a mode of directly controlling the reaction process of material preparation by controlling the activity and the proportion of the raw materials, and the composite porous adsorption material for metallurgical waste residues is prepared at low temperature and room temperature, so that the problem of functional utilization of three solid wastes of the steel slag, the slag and the coal ash and the problem of low-temperature preparation of a porous adsorbent are solved, the porous adsorption material with low cost and high adsorption property is obtained, the adsorption performance is improved, and the utilization of the metallurgical solid wastes and the treatment of wastewater are realized.
Description
Technical Field
The invention relates to a steel slag/fly ash composite waste residue porous adsorption material and a preparation method thereof, in particular to a method for preparing a composite metallurgical waste residue porous adsorption material by taking three metallurgical waste residues of fly ash, slag and steel slag as reaction raw materials in a mode of directly controlling the reaction process of material preparation by controlling the activity and the proportion of the raw materials at low temperature and room temperature, and belongs to the technical field of green preparation of solid waste adsorption materials.
Background
A large amount of solid waste residues such as steel slag, fly ash and the like are generated in the metallurgical process, land occupation and environment pollution are caused, and the material mainly contains elements such as silicon, aluminum, oxygen and the like, and has important significance for environmental protection if the material can be utilized. In addition, a large amount of wastewater is generated in the metallurgical process, and the adsorption method is low in cost, efficient and recyclable in wastewater treatment, and is widely applied. At present, the material system used as the adsorbent material mainly comprises active carbon, natural adsorbent, synthetic adsorbent and the like, but the price is generally higher and the process is complex. The solid waste material powder has the adsorption characteristic, thereby providing a way for sewage treatment. Although the conventional solid waste powder has the adsorption characteristic, the particle size is too small, and the powder is not easy to remove after adsorption, so that the powder has certain limitation in practical application.
The steel slag and the slag are typical solid wastes in metallurgical industry, are associated products in steel making and blast furnace iron making processes respectively, and mainly comprise silicon-rich aluminum components such as silicon dioxide and aluminum oxide. Fly ash is a tiny soot particle that is discharged during the combustion of coal. If the three can be utilized, the waste can be changed into valuable. The conventional utilization is that the three materials are used as raw materials of cement, and the building structural material with certain mechanical property is obtained by matching with the cement. The three materials have adsorption characteristics, and if the adsorption performance of the three materials can be utilized to obtain the high-efficiency adsorbent material, the high-value utilization of waste residues and the treatment of wastewater can be realized, and the waste residues can be functionally utilized. By taking the preparation idea of cement as a reference, the three can be activated and combined through alkali excitation, a novel green environment-friendly material which can be prepared at low temperature is obtained, and a new idea can be provided for the development of a novel porous adsorption material. The obtained composite waste residue porous material has controllable components, a special three-dimensional network gel structure in the composite waste residue porous material, and micro/nano-level pores are distributed in the composite waste residue porous material. At present, previous researches show that the single introduction of the steel slag, the slag and the fly ash can not obtain short-time low-temperature preparation and effective regulation and control of pores, the distribution of the pores directly influences the adsorption performance of the adsorption material, the three can effectively react with the alkali activator by premixing, controlling the particle size and regulating and controlling the component proportion of the excitation solution, the adsorption efficiency of the obtained adsorption material is effectively improved, and in addition, reports about the synchronous introduction of the three into the adsorption material are relatively few. The low-temperature and short-time preparation of the steel slag/fly ash composite waste residue porous adsorption material and the effective removal of color and heavy metal ion pollutants in wastewater can be realized by premixing and component control. The method not only efficiently utilizes the waste residues, but also removes pollutants in the industrial wastewater at low cost, the prepared porous adsorption material has strong recoverability, the cost of raw materials is low, the preparation process is simple, the process can be realized at room temperature and low temperature, and the method is suitable for large-scale production and application.
Disclosure of Invention
The invention provides a novel process for synthesizing a steel slag/fly ash composite waste residue porous adsorption material by directly controlling the reaction process by controlling the activity and the proportion of raw materials aiming at the problems of high-value utilization of the steel slag, the slag and the fly ash waste residue and reaction preparation of the porous adsorption material. The preparation method of the steel slag/fly ash composite waste residue porous adsorption material solves the problems by utilizing the adsorption characteristics of the steel slag, the slag and the fly ash and realizing the synchronous reaction of the steel slag, the slag and the fly ash with an alkali-activated solution in a short time through proper premixing and dispersion, overcomes the preparation problem of the adsorption material taking the steel slag, the slag and the fly ash as raw materials simultaneously. The invention adopts the following technical scheme:
the invention obtains the steel slag/fly ash composite waste residue porous adsorption material by a method of directly controlling the reaction process by controlling the activity and the proportion of raw materials. The method comprises the steps of taking steel slag/fly ash micron-sized powder with specific composition and an alkaline excitation solution mainly containing silica sol as raw materials, preparing and mixing the steel slag/fly ash powder in advance, preparing a potassium hydroxide/sodium excitation sol solution, preparing a waste residue alkali activation slurry, and forming, granulating and alkaline removing a steel slag/fly ash composite waste residue porous material to obtain the steel slag/fly ash composite waste residue porous adsorption material. The obtained adsorbing material mainly comprises an amorphous phase, and micro-nano-scale pores are distributed on the surface of the adsorbing material.
The invention discloses a preparation method of a steel slag/fly ash composite waste residue porous adsorption material, which takes three metallurgical waste residues of fly ash/slag/steel slag as reaction raw materials under room temperature conditions by controlling the activity of the raw materials and the reaction progress of components, and the preparation process is carried out according to the following steps:
step one, crushing and mixing treatment of metallurgical waste residues: crushing and grinding the bulk raw materials of the steel slag and the slag in a mechanical way, grinding the fly ash in a mechanical way, sieving the crushed steel slag, the crushed slag and the crushed fly ash through a 100-mesh and 200-mesh sieve for standby use, and sieving the steel slag, the crushed slag and the fly ash according to the mass ratio of (10-25)%: (10-25)%: (50-80)% is mixed uniformly by mechanical stirring.
Step two, preparing an alkaline excitation sol solution: pouring potassium hydroxide or sodium hydroxide into silica sol with the mass fraction of 25-45%, stirring and mixing by adopting magnetic force, and uniformly stirring to obtain alkaline excitation sol solution; the mass ratio of the potassium hydroxide or the sodium hydroxide to the silica sol with the mass fraction of 25-45% is (20-30): (55-65).
Step three, preparing the waste residue alkali activation slurry: slowly adding the mixed steel slag, fly ash and slag powder in the step one into the alkali-activated sol solution in the step two, uniformly stirring by using a mechanical stirrer, and adding distilled water to adjust the viscosity of the slurryThe slurry is subjected to a shear rate of 50 to 60S-1The viscosity is 500-800 mPas, and alkali-activated slurry containing waste residue is obtained; the mass ratio of the mixed waste residue to the exciting solution is (60-85): 85.
step four, forming the steel slag/fly ash composite waste slag porous material: and pouring the alkali-activated slurry obtained in the third step into a mold, and curing for 1-5h at 25-60 ℃ for molding to obtain the massive alkali-activated waste residue porous material.
Step five, granulating the steel slag/fly ash composite waste slag porous material: and (3) crushing the blocky alkali-activated waste residue porous material in the fourth step by adopting a mechanical mode, crushing the blocky alkali-activated waste residue porous material into particles with the particle size of 150-450 mu m, sieving the particles, and selecting the particles with the particle size of 40-100 meshes to obtain the granular porous material.
Step six, preparing the porous steel slag/fly ash composite waste residue adsorption material: and (4) putting the granular porous material obtained in the fifth step into deionized water, adding a low-concentration hydrochloric acid solution to neutralize redundant alkalinity, soaking for 1-3 days, then washing for 1-3 days by adopting an oscillation box in a shaking way, taking out, washing with absolute ethyl alcohol, and then drying for 1-3 days at 25-60 ℃ to obtain the steel slag/fly ash composite waste residue porous adsorption material.
Further, in the first step, the particle size of the crushed steel slag and slag is 1-10 μm, and the particle size of the ground fly ash is 1-8 μm.
Further, in the first step, the steel slag, the slag and the fly ash are mixed for 1 to 10 minutes in a mechanical stirring manner.
Furthermore, the mass ratio of the steel slag, the slag and the fly ash is preferably (10-20)%: (10-20)%: (60-80)%.
Further, in the second step, the stirring speed is 1000-1200rpm, and the stirring time is 0.5-2 h.
Further, in the third step, the stirring time of the mechanical stirrer is 15-25 minutes.
Further, in the third step, the mass ratio of the mixed waste residue to the exciting solution is 75: 85.
further, in the sixth step, the number of times of washing with absolute ethyl alcohol is 1 to 3.
The steel slag/fly ash composite slag porous adsorption material comprises the following components in percentage by mass: (10-25)%: (10-25)%: (50-80)%, mainly amorphous structure.
The application of the steel slag/fly ash composite waste slag porous adsorption material can be used for adsorbing methylene blue and cadmium ions.
Compared with the prior art, the invention has the advantages that: according to the porous steel slag/fly ash composite waste residue adsorption material prepared by the invention, the steel slag, the slag and the fly ash are compounded according to different activities and proportions, and a polymerization reaction can be generated in a short time under the excitation action of potassium hydroxide/sodium hydroxide under an alkaline condition, so that raw materials with different activities fully participate in a synchronous reaction and utilization, and further, the porous waste residue adsorption material with a micro-nano pore structure can be obtained under a low-temperature condition, and the porous waste residue adsorption material is used for efficiently adsorbing heavy metals and colored solutions. The raw materials are from three metallurgical solid wastes of steel slag, slag and fly ash with specific dimensions and component proportions, the three metallurgical solid wastes are crushed and mixed in advance to be in full contact with a subsequent alkali-activated solution and react with the subsequent alkali-activated solution, the reaction process is controllable, in addition, the three waste residues are crushed into micron-sized powder with different activities and close components, mainly silicon, aluminum, oxygen and iron elements, the three crushed into the powder level have good compatibility, and the three crushed into the powder level can react with an alkaline excitation liquid synchronously and approximately synchronously in a short time to form a porous material in a short time.
The mass ratio of the mixed waste residue raw material of the composite waste residue adsorbing material to the alkaline exciting solution is controllable, the components of the obtained adsorbing material can be directly regulated and controlled by controlling the proportion of the mixed waste residue raw material to the alkaline exciting solution, and the process is simple.
The porous steel slag/fly ash composite waste residue adsorbing material can be obtained by low-temperature molding, crushing and alkali-removing neutralization processes of the composite waste residue adsorbing material, the particle size of the adsorbing material is controllable, the particle size is between 150 and 450 mu m, and the specific surface area can be 15-100m2The water-soluble polymer can adsorb various pollutants and has the adsorption component for high-concentration 100mg/L methylene blue and cadmium ionsRespectively reach 5-120mg/g and 10-94mg/g, has high adsorption effect compared with the original steel slag, slag and fly ash materials, and is easy to recover and separate after adsorption. The porous steel slag/fly ash composite waste residue adsorbing material prepared by the invention controls the reaction process by controlling the raw material composition, the size of the adsorbing material is in the micron level, the pore structure of the adsorbing material is mainly micro-nano, the pores are adjustable, the application problem of the steel slag, slag and fly ash waste residue in the aspect of adsorbing materials is solved, the preparation process is simple, the porous adsorbing material can be realized at low temperature, the operation and the popularization are easy, the obtained porous adsorbing material has good adsorbing effect, and the porous adsorbing material can be used for solid waste treatment and green development of environment-friendly materials.
Drawings
FIG. 1 is an XRD pattern of the porous steel slag/fly ash composite slag adsorption material obtained in example 1 of the present invention.
FIG. 2 is an SEM image of the porous steel slag/fly ash composite slag adsorbing material obtained in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
The invention uses three metallurgical waste residues of fly ash/slag/steel slag as reaction raw materials under room temperature condition by controlling the activity of the raw materials and the reaction of the components, and the preparation process is carried out according to the following steps:
step one, crushing and mixing treatment of metallurgical waste residues: crushing and grinding bulk raw materials of steel slag and slag by adopting a mechanical crushing and grinding mode, wherein the median particle size after crushing is about 5 mu m, grinding large-particle fly ash into 5 mu m, sieving the pulverized coal ash by a 100-mesh sieve for standby use, and mixing the steel slag, the slag and the fly ash according to the mass ratio: 20% to 60% by mass, and mechanically stirring and mixing for 10 minutes in advance.
Step two, preparation of potassium hydroxide excited sol solution: pouring potassium hydroxide into silica sol with the mass fraction of 40%, magnetically stirring and mixing, and stirring at 1200rpm for 2h to obtain an alkaline excitation solution;
step three, activating the slurry by waste residue alkaliConfiguration: mixing the composite waste residue powder with the excitation solution obtained in the step two, wherein the mass ratio of the mixed waste residue to the excitation solution is 75: 85. slowly adding the waste residue into the prepared alkali-activated sol solution obtained in the second step, stirring for 25 minutes by using a mechanical stirrer, adding distilled water to adjust the viscosity of the slurry, and enabling the shear rate to be 50-60S-1The viscosity is 500-800 mPas, and alkali-activated slurry containing three waste residues is obtained;
step four, forming the alkali-activated steel slag/fly ash composite waste slag porous material: and pouring the slurry obtained in the third step into a cylindrical mold, and curing for 3 hours at the temperature of 60 ℃ for molding to obtain the massive alkali-activated waste residue porous material.
Step five, granulating the steel slag/fly ash composite waste slag porous material: and (3) crushing the waste residue porous material block in the fourth step by adopting a mechanical mode, and crushing the waste residue porous material block into particles of 150-450 mu m to obtain the granular porous material.
Step six, preparing the porous steel slag/fly ash composite waste residue adsorption material: and (4) putting the granular material obtained in the fifth step into deionized water, adding a low-concentration hydrochloric acid solution to neutralize redundant alkalinity, soaking for 3 days, then washing for 1 day by adopting an oscillation box in a shaking way, taking out, washing for 3 times by using absolute ethyl alcohol, and then drying for 1 day at 60 ℃ to obtain the steel slag/fly ash composite waste residue adsorbing material for adsorption.
From the porous steel slag/fly ash composite waste residue adsorbing material obtained in the sixth step of the example 1, it can be seen that the porous adsorbing material is in a polygonal granular shape, the gray black color of the original waste residue is retained, and the size of the adsorbing material is in a micron level.
FIG. 1 is an XRD spectrum of the porous steel slag/fly ash composite slag adsorption material obtained in example 1. As can be seen from the figure, the porous material is basically in an amorphous structure, contains a small amount of impurities which are stable mineral phase structures introduced by mullite and slag and steel slag introduced by the fly ash, and the impurities do not participate in the reaction and are remained due to the chemical stability.
FIG. 2 is an SEM image of the porous steel slag/fly ash composite slag adsorbing material obtained in example 1; as can be seen from the figure, micro-nano level pores are distributed on the surface of the porous material particles, and the pores are uniformly distributed.
The porous steel slag/fly ash composite waste residue adsorbing material obtained in the embodiment has good adsorption performance and controllable pores, when the using amount of the adsorbing material is 6mg/L, the adsorbing amount of the adsorbing material on a 100mg/L methylene blue solution reaches 16.5mg/g, and the removal rate reaches-99%. When the dosage of the adsorbing material is 10mg/L, the adsorbing amount of the adsorbing material to the methylene blue solution of 100mg/L reaches 10.0mg/g, and the removal rate reaches 100 percent.
When the dosage of the adsorbing material is 10mg/L, the adsorbing capacity of the adsorbing material to the cadmium ion solution of 100mg/L reaches 9.9mg/g, and the removal rate reaches 99%.
Example 2
The difference from the embodiment 1 is that the steel slag, the slag and the fly ash in the first step are as follows according to the mass ratio: 10 percent to 80 percent.
The surface of the porous steel slag/fly ash composite waste residue adsorbing material obtained in the embodiment has a micro-nano pore structure, when the using amount of the adsorbing material is 10mg/L, the adsorbing amount of the adsorbing material to a methylene blue solution of 100mg/L respectively reaches 9.9mg/g, and the removal rate reaches 99%.
Example 3
The difference from the embodiment 1 is that the steel slag, the slag and the fly ash in the first step are as follows according to the mass ratio: 25 percent, 25 percent and 50 percent.
The surface of the porous steel slag/fly ash composite waste residue adsorbing material obtained in the embodiment has a micro-nano pore structure, when the using amount of the adsorbing material is 10mg/L, the adsorbing amount of the adsorbing material on a 100mg/L methylene blue solution reaches 8.4mg/g, and the removal rate reaches 84%.
Example 4
The steel slag-fly ash slag-slag composite material is different from the steel slag-slag composite material in the embodiment 1 in that the steel slag, the slag and the fly ash are as follows according to the mass ratio: 15 percent to 70 percent. When the dosage of the adsorbing material is 10mg/L, the adsorbing amount of the adsorbing material to the methylene blue solution of 100mg/L reaches 8.5mg/g, and the removal rate reaches 85 percent.
The analysis of the data is integrated, which shows that the method can successfully prepare the porous steel slag/fly ash composite waste residue adsorbing material.
Claims (10)
1. The invention discloses a preparation method of a steel slag/fly ash composite waste residue porous adsorption material, which is characterized in that three metallurgical waste residues of fly ash/slag/steel slag are used as reaction raw materials under the room temperature condition by controlling the activity of the raw materials and the reaction process of components, and the preparation process is carried out according to the following steps:
step one, crushing and mixing treatment of metallurgical waste residues: crushing and grinding the bulk raw materials of the steel slag and the slag in a mechanical way, grinding the fly ash in a mechanical way, sieving the crushed steel slag, the crushed slag and the crushed fly ash through a 100-mesh and 200-mesh sieve for standby use, and sieving the steel slag, the crushed slag and the fly ash according to the mass ratio of (10-25)%: (10-25)%: (50-80)% is mixed uniformly in a mechanical stirring mode in advance;
step two, preparing an alkaline excitation sol solution: pouring potassium hydroxide or sodium hydroxide into silica sol with the mass fraction of 25-45%, stirring and mixing by adopting magnetic force, and uniformly stirring to obtain alkaline excitation sol solution; the mass ratio of the potassium hydroxide or the sodium hydroxide to the silica sol with the mass fraction of 25-45% is (20-30): (55-65);
step three, preparing the waste residue alkali activation slurry: slowly adding the mixed steel slag, fly ash and slag powder in the step one into the alkali-activated sol solution in the step two, uniformly stirring by using a mechanical stirrer, adding distilled water to adjust the viscosity of the slurry, and enabling the shear rate of the slurry to be 50-60S-1The viscosity is 500-800 mPas, and alkali-activated slurry containing waste residue is obtained; the mass ratio of the mixed waste residue to the exciting solution is (60-85): 85 parts by weight;
step four, forming the steel slag/fly ash composite waste slag porous material: pouring the alkali-activated slurry obtained in the third step into a mold, and curing for 1-5h at 25-60 ℃ for molding to obtain a blocky alkali-activated waste residue porous material;
step five, granulating the steel slag/fly ash composite waste slag porous material: crushing the blocky alkali-activated waste residue porous material in the fourth step by adopting a mechanical mode, crushing the blocky alkali-activated waste residue porous material into particles of 150-450 mu m, sieving the particles, and selecting particles with the particle size of 40-100 meshes to obtain a granular porous material;
step six, preparing the porous steel slag/fly ash composite waste residue adsorption material: and (4) putting the granular porous material obtained in the fifth step into deionized water, adding a low-concentration hydrochloric acid solution to neutralize redundant alkalinity, soaking for 1-3 days, then washing for 1-3 days by adopting an oscillation box in a shaking way, taking out, washing with absolute ethyl alcohol, and then drying for 1-3 days at 25-60 ℃ to obtain the steel slag/fly ash composite waste residue porous adsorption material.
2. The preparation method of the steel slag/fly ash composite slag porous adsorption material according to claim 1, wherein in the first step, the particle size of the crushed steel slag and crushed slag is 1-10 μm, and the particle size of the ground fly ash is 1-8 μm.
3. The preparation method of the steel slag/fly ash composite slag porous adsorption material according to claim 1, wherein in the first step, the steel slag, the slag and the fly ash are mixed for 1-10 minutes by a mechanical stirring manner.
4. The preparation method of the steel slag/fly ash composite slag porous adsorption material according to claim 1, wherein the mass ratio of the steel slag, the slag and the fly ash is preferably (10-20)%: (10-20)%: (60-80)%.
5. The preparation method of the steel slag/fly ash composite slag porous adsorption material as claimed in claim 1, wherein in the second step, the stirring speed is 1000-1200rpm, and the stirring time is 0.5-2 h.
6. The preparation method of the steel slag/fly ash composite slag porous adsorption material according to claim 1, wherein in the third step, the stirring time of a mechanical stirrer is 15-25 minutes.
7. The preparation method of the steel slag/fly ash composite slag porous adsorption material according to claim 1, wherein in the third step, the mass ratio of the mixed slag to the excitation solution is 75: 85.
8. the preparation method of the steel slag/fly ash composite slag porous adsorption material according to claim 1, wherein in the sixth step, the absolute ethyl alcohol is washed for 1-3 times.
9. The steel slag/fly ash composite slag porous adsorption material prepared by the preparation method of any one of claims 1 to 8.
10. The application of the steel slag/fly ash composite slag porous adsorption material prepared by the preparation method of any one of claims 1 to 8, wherein the steel slag/fly ash composite slag porous adsorption material is used for adsorbing methylene blue and cadmium ions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111160743.1A CN113797884A (en) | 2021-09-30 | 2021-09-30 | Steel slag/fly ash composite waste slag porous adsorption material, preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111160743.1A CN113797884A (en) | 2021-09-30 | 2021-09-30 | Steel slag/fly ash composite waste slag porous adsorption material, preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113797884A true CN113797884A (en) | 2021-12-17 |
Family
ID=78897240
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111160743.1A Pending CN113797884A (en) | 2021-09-30 | 2021-09-30 | Steel slag/fly ash composite waste slag porous adsorption material, preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113797884A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114835509A (en) * | 2022-06-08 | 2022-08-02 | 浙江工业大学 | Preparation method of sintering-free alkali-activated inorganic sponge heat-insulation fireproof plate |
| CN115254038A (en) * | 2022-06-21 | 2022-11-01 | 陕西汇康职业卫生技术服务有限公司 | Heavy metal industrial wastewater treatment material, preparation method thereof and wastewater treatment device |
| CN116986829A (en) * | 2023-06-13 | 2023-11-03 | 中国地质大学（武汉） | Semi-dry desulfurization ash-fly ash-slag composite cementing material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007035101A2 (en) * | 2005-09-26 | 2007-03-29 | Stichting Energieonderzoek Centrum Nederland | Composition comprising active charcoal, steel slag and contaminated material and use thereof |
| US20160122207A1 (en) * | 2014-10-31 | 2016-05-05 | The Board Of Regents For Oklahoma State University | Method for surface treatment of sieved steel slag for increasing phosphorus removal capacity |
| CN105817196A (en) * | 2016-04-20 | 2016-08-03 | 菏泽学院 | High-aluminum fly ash heavy metal ion adsorbent and preparation method thereof |
| CN110255932A (en) * | 2019-07-03 | 2019-09-20 | 安徽工业大学 | A kind of alkali-activated carbonatite solid waste type high temperature resistant, high shear force inorganic glue and preparation method thereof |
| CN111377665A (en) * | 2020-03-18 | 2020-07-07 | 山东大学 | Solid waste based porous sewage treatment agent and preparation method and application thereof |
| CN113060954A (en) * | 2021-04-22 | 2021-07-02 | 山东交通学院 | Method for preparing tobermorite-based inorganic cementing material by using alkali-activated solid waste micro powder at normal temperature and product thereof |
-
2021
- 2021-09-30 CN CN202111160743.1A patent/CN113797884A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007035101A2 (en) * | 2005-09-26 | 2007-03-29 | Stichting Energieonderzoek Centrum Nederland | Composition comprising active charcoal, steel slag and contaminated material and use thereof |
| US20160122207A1 (en) * | 2014-10-31 | 2016-05-05 | The Board Of Regents For Oklahoma State University | Method for surface treatment of sieved steel slag for increasing phosphorus removal capacity |
| CN105817196A (en) * | 2016-04-20 | 2016-08-03 | 菏泽学院 | High-aluminum fly ash heavy metal ion adsorbent and preparation method thereof |
| CN110255932A (en) * | 2019-07-03 | 2019-09-20 | 安徽工业大学 | A kind of alkali-activated carbonatite solid waste type high temperature resistant, high shear force inorganic glue and preparation method thereof |
| CN111377665A (en) * | 2020-03-18 | 2020-07-07 | 山东大学 | Solid waste based porous sewage treatment agent and preparation method and application thereof |
| CN113060954A (en) * | 2021-04-22 | 2021-07-02 | 山东交通学院 | Method for preparing tobermorite-based inorganic cementing material by using alkali-activated solid waste micro powder at normal temperature and product thereof |
Non-Patent Citations (4)
| Title |
|---|
| 冷发光等: "混凝土标准规范及工程应用", 《中国建材工业出版社》, 30 October 2005 (2005-10-30), pages 444 - 445 * |
| 张文清: "分离分析化学", 《华东理工大学出版社》, 30 September 2016 (2016-09-30), pages 97 - 98 * |
| 贾德昌: "无机聚合物及其复合材料", 《哈尔滨工业大学出版社》, 31 March 2014 (2014-03-31), pages 100 - 102 * |
| 赵亚娟等: "粉煤灰吸附剂的研究进展", 《材料导报》, vol. 21, no. 11, 15 November 2007 (2007-11-15) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114835509A (en) * | 2022-06-08 | 2022-08-02 | 浙江工业大学 | Preparation method of sintering-free alkali-activated inorganic sponge heat-insulation fireproof plate |
| CN115254038A (en) * | 2022-06-21 | 2022-11-01 | 陕西汇康职业卫生技术服务有限公司 | Heavy metal industrial wastewater treatment material, preparation method thereof and wastewater treatment device |
| CN116986829A (en) * | 2023-06-13 | 2023-11-03 | 中国地质大学（武汉） | Semi-dry desulfurization ash-fly ash-slag composite cementing material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113797884A (en) | Steel slag/fly ash composite waste slag porous adsorption material, preparation method and application | |
| CN103588404B (en) | Method for processing recycled aggregate and method for preparing high performance concrete using same | |
| CN112608043B (en) | High-strength nickel slag-based solid waste cementing material and preparation method thereof | |
| CN110606721B (en) | Cementing material based on various solid wastes and preparation method thereof | |
| CN110228973A (en) | A kind of burning city domestic garbage bottom ash regeneration method for preparing mortar | |
| CN111892325B (en) | Preparation method of wet-milling dechlorination nano-alkali residue inorganic salt early strength agent | |
| CN113185194B (en) | Porous permeable geopolymer material and preparation method and application thereof | |
| CN115893879B (en) | Preparation method of solid waste-based superfine special composite cementing material and cementing material | |
| CN114538839A (en) | Nano-alumina-based municipal solid waste incineration fly ash heavy metal curing material and preparation method thereof | |
| CN112608088B (en) | Geopolymer grouting material based on incineration fly ash and preparation method thereof | |
| CN114163174A (en) | Solid waste base modified cementing material and application thereof | |
| CN112805260B (en) | Method for producing synthetic light ceramic sand and application thereof | |
| CN107522276B (en) | Preparation method of water defluorinating agent | |
| CN113121142B (en) | Activation recovery powder, preparation method thereof and asphalt mixture containing activation recovery powder | |
| CN111170673B (en) | Composite nano material for anti-seepage partition wall and preparation method thereof | |
| CN113831082A (en) | Tungsten-iron-tailing-based photocatalytic water permeable brick and preparation method thereof | |
| CN112174279A (en) | Polymeric aluminosilicate inorganic flocculant and preparation method and application thereof | |
| CN111960697A (en) | Energy-saving environment-friendly cement for buildings and production process thereof | |
| CN112521068A (en) | Resource treatment method for environment-friendly concrete and waste CRT glass | |
| CN113877532B (en) | Graphene oxide reinforced solid waste inorganic spherical adsorbent, preparation method and application thereof | |
| CN108499522B (en) | Coal gangue cenosphere/aluminosilicate polymer composite adsorbent and preparation method thereof | |
| CN109574059A (en) | A kind of preparation method of calcium carbonate fine powder | |
| CN111559901B (en) | Alkali-activated recycled nickel slag cement concrete | |
| CN110105050A (en) | A method of cadmium in trade waste is stabilized using kaolin | |
| CN116396018B (en) | Method for preparing nano-micron crystal nucleus additive by utilizing commercial mixing station waste slurry and wastewater integrated carbon fixation |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211217 |