CN111151217B - Preparation method of magnetic gangue geopolymer adsorbent - Google Patents

Preparation method of magnetic gangue geopolymer adsorbent Download PDF

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CN111151217B
CN111151217B CN202010063174.8A CN202010063174A CN111151217B CN 111151217 B CN111151217 B CN 111151217B CN 202010063174 A CN202010063174 A CN 202010063174A CN 111151217 B CN111151217 B CN 111151217B
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coal gangue
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geopolymer
powder
solution
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CN111151217A (en
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马建超
庞进
冯国瑞
王欣
马清亮
郭春丽
张晓朋
任凯文
郭精茂
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Taiyuan University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229—Compounds of Fe
    • 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
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009—Magnetic properties
    • 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

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Abstract

The invention discloses a preparation method of a magnetic coal gangue geopolymer adsorbent, which comprises the following steps: (1) and (3) putting the thermally activated coal gangue powder and an alkali activator into distilled water, uniformly mixing, curing and molding by a suspension curing method, washing by distilled water, drying, and grinding to obtain the coal gangue geopolymer powder. (2) Uniformly stirring the ferric salt solution and the coal gangue powder, preparing the magnetic coal gangue geopolymer by a coprecipitation method or a hydrothermal method, and after the reaction time is up, carrying out magnetic separation, washing and drying to obtain the magnetic coal gangue geopolymer adsorbent. The magnetic coal gangue geopolymer adsorbent prepared by the invention has typical geopolymer characteristics and unique magnetic recoverability, can greatly reduce the solid-liquid separation time after wastewater treatment, and has good industrial application prospect.

Description

Preparation method of magnetic gangue geopolymer adsorbent
Technical Field
The invention relates to a preparation method of a magnetic coal gangue geopolymer adsorbent, belonging to the technical field of environmental and material engineering.
Background
The coal gangue is solid waste generated in the coal mining process, and the output of the coal gangue breaks through hundreds of millions of tons at present in China, and the output is also increased sharply. The existing coal gangue utilization method comprises thermal power generation, fertilizer preparation filling material, water treatment material preparation and the like. However, these approaches do not achieve efficient utilization of coal gangue. Meanwhile, researchers are also promoted to develop a novel coal gangue utilization scheme.
In recent years, "three wastes" treatment has become a focus of attention of researchers, and the preparation of a wastewater treatment material by using a solid waste to prepare an inorganic polymer is favored. Among them, there have been many studies on the preparation of geopolymers from Fly ash, kaolin, red mud, etc., but they are mostly molded with a grinding tool (Jia Yi, et Al. a preparation method of a burning-free Fly ash-based geopolymer high-performance adsorbent material, china 201610870948.1 [ P ]; Guo Shi, et Al. a preparation method of a geopolymer adsorbent material and a preparation method thereof, china 201910300343.2 [ P ]; Yan S. et Al. Green synthesis of high-performance water control micro/geopolymer complex particle hydro-modification [ J ]. Journal of Cleaner Production, 2019, 227: 483 494), or ground into powder after molding (Al-Harahehh M.S. et Al. flash bed bonded geopolymer for gravity metal recovery: A. cement slurry J. (Journal of Chemical Engineering J.),1663, a pore and eco-friendly macromolecular geomonomer absorber for a heavymetals removal from an aqueous solution [ J ]. Journal of a purifier production, 2019, 215: 1233-. The two schemes have respective disadvantages, wherein a large amount of curing time is needed after the mould is formed, and the powdery geopolymer water treatment agent is not easy to recover after being used.
Disclosure of Invention
The invention aims to develop a magnetic geopolymer adsorbing material by utilizing solid waste, and provides a preparation method of the magnetic gangue geopolymer adsorbing material, which is simple in process and convenient to operate. The method takes coal gangue as a raw material, and obtains the magnetic coal gangue geopolymer adsorbent through two experimental steps.
In order to solve the two problems of long process time and difficult recovery, the invention provides a preparation method of a magnetic gangue geopolymer adsorbent without maintenance. The magnetic coal gangue geopolymer prepared by the method has the advantages of environmental protection, short process period, magnetic recovery of the water treatment agent after use and the like.
The invention provides a preparation method of a magnetic coal gangue geopolymer adsorbent, which comprises the following steps:
(1) the coal gangue geopolymer powder is prepared by the steps of thermally activating coal gangue powder at 400-1000 ℃ for 2-8 h, then uniformly mixing the coal gangue powder with an alkali activator in distilled water, curing and molding by a suspension curing method, washing by distilled water, drying and grinding.
(2) Uniformly stirring the ferric salt solution and the coal gangue powder, preparing the magnetic coal gangue geopolymer by a coprecipitation method or a hydrothermal method, and after the reaction time is up, carrying out magnetic separation, washing and drying to obtain the magnetic coal gangue geopolymer adsorbent.
In the preparation method, the reaction process of the coprecipitation method is as follows: fe with a concentration of 0.1-0.5 mol/L3+And Fe2+Solution (Fe)3+With Fe2+The molar ratio of 2: 1) and the coal gangue geopolymer powder are evenly stirred, and N is dropwise added under the nitrogen atmosphere2H4•H2O / NH4HCO3 / NaCO3 / NH3·H2O / CH3And (3) heating the COONa solution to 90 ℃ until the pH value reaches above 9, continuing heating and stirring for 1-3 hours, naturally cooling to room temperature, washing for a plurality of times by using 0.5% (v/v) acetic acid solution until the pH value of the solution is neutral, and thus preparing the magnetic coal gangue geopolymer powder.
In the preparation method, the hydrothermal reaction process comprises the following steps: FeCl is added3·6H2O and CH3And adding the COONa solution and the coal gangue geopolymer powder into 60mL of ethylene glycol, uniformly stirring, transferring to a high-pressure reaction kettle, and heating at 200 ℃ for 12 hours. And naturally cooling to room temperature, washing for several times by using 0.5% (v/v) acetic acid solution until the pH value of the solution is neutral, and thus preparing the magnetic coal gangue geopolymer powder.
In the preparation method, the magnetic separation process comprises the following steps: and placing the magnet at the bottom of a container containing the mixed liquid of the magnetic coal gangue geopolymer powder, and pouring or pumping out the liquid in the container when the magnetic coal gangue geopolymer powder is attracted by magnetic force to realize the quick solid-liquid separation.
The method for preparing the magnetic geopolymer adsorbing material,
preferably, in step (1), the alkali-activating agent is Na2SiO3、K2SiO3One of NaOH and KOH; n (SiO)2) (n (alkali activator) = 1.25-2); n (alkali activator)/n (Al)2O3)=0.6～1.5；n(H2O)/n (alkali activator) = 15-45; wherein n represents a number of moles.
Preferably, the reaction temperature in the hydrothermal method in the step (2) is 200-500 ℃; the mass ratio of the ferric salt solution to the coal gangue geopolymer powder is 20-200: 1.
preferably, the drying conditions in the (1) (2) step are: the temperature is 60-100 ℃, the time is 6-24 h, and the vacuum drying in the step (2) is carried out.
Further, the iron salt comprises FeCl3·6H2O or FeSO4·7H2O or FeCl2·4H2And O. Wherein the mass ratio of the iron salt to the coal gangue geopolymer powder is 0.2-5.
The invention has the beneficial effects that:
the magnetic coal gangue geopolymer adsorbent prepared by the invention has typical geopolymer characteristics and unique magnetic recoverability, can greatly reduce the solid-liquid separation time after wastewater treatment, and has good industrial application prospect.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
Example 1:
in a 100mL beaker was added 12g of technical grade Na2SiO3·9H2O and 12mL of aqueous solution are stirred uniformly; putting 10g of coal gangue powder into a muffle furnace, and heating for 5h at 800 ℃; taking out the cooled activated coal gangue powder, and placing the activated coal gangue powder into a 100mL single-neck round-bottom flask; adding the water glass solution into a round-bottom flask filled with activated coal gangue, and stirring for 30 min; and (3) dripping the slurry after alkali excitation into dimethyl silicone oil at the temperature of 80 ℃ by using a 5mL syringe, separating and washing the solidified geopolymer small particles after 30min, drying for 12h at the temperature of 80 ℃ to obtain geopolymer particles, and grinding the geopolymer particles into powder for later use.
5g of geopolymer powder, 2.16 g of FeCl were weighed3• 6H2O and 5g CH3COONa is dissolved in 60mL of ethylene glycol, after the mixture is fully stirred, the mixed solution is put into a high-pressure reaction kettle with a polytetrafluoroethylene inner liner, the mixture is heated for 12 hours at the temperature of 200 ℃, after the mixture is naturally cooled to the room temperature, the mixture is washed for a plurality of times by 0.5% (v/v) acetic acid solution until the pH value of the solution is neutral, the magnetic separation is carried out, and the mixture is dried for 6 hours at the temperature of 60 ℃ in a vacuum drying oven, so that the magnetic coal gangue geopolymer is obtained. Applying it to Pb2+Adsorption to obtain the data in Table 1.
Example two
Adding 5.5g of NaOH and 27mL of aqueous solution into a 100mL beaker, and uniformly stirring; putting 20g of coal gangue powder into a muffle furnace, and heating for 5 hours at 800 ℃; taking out the cooled activated coal gangue powder, and placing the activated coal gangue powder into a 100mL single-neck round-bottom flask; adding NaOH solution into a round-bottom flask filled with activated coal gangue, and stirring for 30 min; and (3) dripping the slurry into silicone oil at 80 ℃ by using a 5mL injector, separating and washing the solidified geopolymer small particles after 30min, drying at 80 ℃ for 12h to obtain geopolymer particles, and grinding into powder for later use.
3.76 g of FeCl3·6H2O、1.97 g FeSO4·7H2Dissolving O in 50 mL of distilled water, adding 4g of coal gangue geopolymer powder, uniformly stirring, and then dropwise adding NaCO3And (4) solution until the pH of the mixed solution reaches 10. Heating to 90 ℃ while mechanically stirring for 1 h, wherein the reaction process is N2In a protective atmosphere. And after the reaction is finished, cooling to room temperature, carrying out magnetic separation on the precipitate, washing for a plurality of times by using 0.5% (v/v) acetic acid solution respectively until the pH of the solution is neutral, collecting the product by applying a magnetic field for magnetic separation, and drying for 6 hours in a vacuum drying oven at 60 ℃ to obtain the magnetic coal gangue geopolymer. Applying it to Pb2+Adsorption to obtain the data in Table 1.
EXAMPLE III
6.5g of technical grade K are added to a 100mL beaker2SiO3And 12mL of aqueous solution, and uniformly stirring; putting 10g of coal gangue powder into a muffle furnace, and heating for 5h at 800 ℃; taking out the cooled activated coal gangue powder, and placing the activated coal gangue powder into a 100mL single-neck round-bottom flask; will K2SiO3Adding the solution into a round-bottom flask containing activated coal gangue, and stirring for 30 min; and (3) dripping the slurry into polyethylene glycol (with the molecular weight of 600) at the temperature of 80 ℃ by using a 5mL syringe, separating and washing the solidified geopolymer small particles after 30min, drying for 12h at the temperature of 80 ℃ to obtain geopolymer particles, and grinding the geopolymer particles into powder for later use.
3.76 g of FeCl3·6H2O、1.97 g FeSO4·7H2Dissolving O in 50 mL of distilled water, adding 4g of coal gangue geopolymer powder, stirring uniformly, and then dropwise adding NH4HCO3And N2H4•H2O mix the solution until the mixed solution pH reaches 10. Heating to 90 ℃ while mechanically stirring for 1 h, wherein the reaction process is N2In a protective atmosphere. And after the reaction is finished, cooling to room temperature, carrying out magnetic separation on the precipitate, washing for a plurality of times by using 0.5% (v/v) acetic acid solution respectively until the pH of the solution is neutral, collecting the product by applying a magnetic field for magnetic separation, and drying for 6 hours in a vacuum drying oven at 60 ℃ to obtain the magnetic coal gangue geopolymer. Applying it to Cu2+Adsorption to obtain the data in Table 1.
Example four
Adding 7.7g of KOH and 27mL of aqueous solution into a 100mL beaker, and uniformly stirring; putting 20g of coal gangue powder into a muffle furnace, and heating for 5 hours at 800 ℃; taking out the cooled activated coal gangue powder, and placing the activated coal gangue powder into a 100mL single-neck round-bottom flask; adding KOH solution into a round-bottom flask filled with activated coal gangue, and stirring for 30 min; and (3) dripping the slurry into silicone oil at 80 ℃ by using a 5mL injector, separating and washing the solidified geopolymer small particles after 30min, drying at 80 ℃ for 12h to obtain geopolymer particles, and grinding into powder for later use.
7.52 g FeCl3·6H2O、3.94 g FeSO4·7H2Dissolving O in 100mL of distilled water, adding 7g of coal gangue geopolymer powder, stirring uniformly, and then dropwise adding NH4HCO3And (4) solution until the pH of the mixed solution reaches 10. Heating to 90 ℃ while mechanically stirring for 1 h, wherein the reaction process is N2In a protective atmosphere. And after the reaction is finished, cooling to room temperature, carrying out magnetic separation on the precipitate, washing the precipitate for several times by using 0.5% (v/v) acetic acid solution respectively until the pH value of the solution is neutral, carrying out magnetic separation, and drying the precipitate for 6 hours in a vacuum drying oven at 60 ℃ to obtain the magnetic coal gangue geopolymer. Applying it to Cu2+Adsorption to obtain the data in Table 1.
TABLE 1 magnetic gangue geopolymer adsorption data
Figure DEST_PATH_IMAGE002
。

Claims (5)

1. A preparation method of a magnetic coal gangue geopolymer adsorbent is characterized by comprising the following steps:
(1) performing thermal activation on coal gangue powder at 400-1000 ℃ for 2-8 h, then uniformly mixing the coal gangue powder with an alkali activator in distilled water, performing curing molding by a suspension curing method, washing with distilled water, drying, and grinding to obtain coal gangue geopolymer powder;
(2) uniformly stirring an iron salt solution and coal gangue powder, preparing a magnetic coal gangue geopolymer by a coprecipitation method or a hydrothermal method, and after the reaction time is up, carrying out magnetic separation, washing and drying to obtain a magnetic coal gangue geopolymer adsorbent; wherein the mass ratio of the ferric salt to the coal gangue geopolymer powder is 0.2-5;
the reaction process of the coprecipitation method is as follows: fe with a concentration of 0.1-0.5 mol/L3+And Fe2+The solution is evenly stirred with coal gangue geopolymer powder, wherein Fe3+With Fe2+The molar ratio is 2: 1; dropwise adding N under nitrogen atmosphere2H4•H2O、 NH4HCO3 、 Na2CO3、NH3·H2O、CH3One of COONa solutions is added until the pH value reaches more than 9, the temperature is raised to 90 ℃, the heating and stirring are continued for 1 to 3 hours, the solution is naturally cooled to the room temperature, and then the solution is washed for a plurality of times by using acetic acid solution with the volume ratio of 0.5 percent until the pH value of the solution is neutral, and then the magnetic gangue geopolymer powder can be prepared; said Fe3+And Fe2+The source of iron in the solution is FeCl3·6H2O or FeSO4·7H2O or FeCl2·4H2O；
The hydrothermal reaction process comprises: FeCl is added3·6H2O and CH3Adding the COONa solution and the coal gangue geopolymer powder into 60mL of ethylene glycol, mixing uniformly, transferring to a high-pressure reaction kettle, and heating at 200 ℃ for 12 hours; and naturally cooling to room temperature, washing for several times by using an acetic acid solution with the volume ratio of 0.5% until the pH value of the solution is neutral, and thus preparing the magnetic coal gangue geopolymer powder.
2. The preparation method of the magnetic coal gangue geopolymer adsorbent as claimed in claim 1, wherein: the magnetic separation process comprises the following steps: and placing the magnet at the bottom of the container for containing the mixed liquid of the magnetic coal gangue geopolymer powder, and pouring or pumping out the liquid in the container when the magnetic coal gangue geopolymer powder is attracted by magnetic force, so as to realize the quick solid-liquid separation.
3. The preparation method of the magnetic coal gangue geopolymer adsorbent according to claim 1, wherein the preparation method comprises the following steps: in the step (1), the alkali activator is Na2SiO3、K2SiO3One of NaOH and KOH; n (SiO)2) (n (alkali activator) = 1.25-2); n (alkali activator)/n (Al)2O3)=0.6～1.5；n(H2O)/n (alkali activator) = 15-45; and n represents a mole number.
4. The preparation method of the magnetic coal gangue geopolymer adsorbent as claimed in claim 1, wherein: the drying conditions in the steps (1) and (2) are as follows: the temperature is 60-100 ℃, and the time is 6-24 h.
5. The preparation method of the magnetic coal gangue geopolymer adsorbent as claimed in claim 1, wherein: the drying in the step (2) is vacuum drying.
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CN115282971B (en) * 2022-08-19 2024-01-19 太原理工大学 High-performance denitrification non-noble metal catalyst and preparation method and application thereof
CN115477948A (en) * 2022-09-22 2022-12-16 昆明理工大学 Method for preparing FeOOH modified coal gangue by utilizing red mud
CN115970636A (en) * 2023-01-17 2023-04-18 中煤科工西安研究院(集团)有限公司 Coal gangue-based C-A-S-H gel, preparation method and application
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