CN113262753B - Preparation method and application of millimeter-sized monodisperse magnesium oxide pellets - Google Patents

Preparation method and application of millimeter-sized monodisperse magnesium oxide pellets Download PDF

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CN113262753B
CN113262753B CN202110415122.7A CN202110415122A CN113262753B CN 113262753 B CN113262753 B CN 113262753B CN 202110415122 A CN202110415122 A CN 202110415122A CN 113262753 B CN113262753 B CN 113262753B
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magnesium oxide
oxide pellets
millimeter
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application
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CN113262753A (en
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孔祥贵
毛方琪
郝培培
林彦军
段雪
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Beijing University of Chemical Technology
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Beijing University of Chemical 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
    • B01J20/04—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
    • B01J20/041—Oxides or hydroxides
    • 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
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • 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
    • B01J20/28014—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 form
    • B01J20/28016—Particle form
    • B01J20/28019—Spherical, ellipsoidal or cylindrical
    • 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
    • B01J20/28054—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 surface properties or porosity
    • 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
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a preparation method and application of millimeter-sized monodisperse magnesium oxide pellets. The invention dissolves magnesium salt and precipitant in common solvent, obtains precursor under mild condition, and then directly obtains high-dispersion millimeter-sized magnesium oxide pellets through roasting without steps of extrusion, granulation and the like. The preparation method of the invention has the advantages of simple equipment, mild synthesis condition, simple operation, abundant raw material sources, low price and great application prospect. The magnesium oxide pellets prepared by the method have higher specific surface area and rich pore structure, are favorable for adsorbing heavy metal lead, and show excellent performance in the aspect of removing the heavy metal lead. More importantly, the magnesium oxide pellets prepared by the method have larger size, do not need operations such as filtration, centrifugation and the like, can be subjected to automatic solid-liquid separation, are convenient for industrial application, not only reduce the cost, but also improve the efficiency, and solve the problem that powder materials are difficult to separate.

Description

Preparation method and application of millimeter-sized monodisperse magnesium oxide pellets
Technical Field
The invention belongs to the technical field of inorganic material synthesis and heavy metal ion removal, and particularly relates to a preparation method of millimeter-sized monodisperse magnesium oxide pellets and application of the millimeter-sized monodisperse magnesium oxide pellets in heavy metal lead removal.
Background
Water is the most important and fundamental natural resource, not only the root for human survival, but also the key to the sustainable development of society and economy. The serious pollution hazard of the current water body is mainly pollution to the water body caused by pollutants generated by human activities due to the rapid development of human activities and global economy, and heavy metal pollutants are one of the pollutants.
Lead (Pb) is a toxic heavy metal element, is difficult to degrade in the environment, can be enriched and absorbed by aquatic animals and plants, and can harm human and animal safety when entering a human food chain. In addition, the Pb-containing water can enter human body by direct drinking or skin contact, which causes harm to human health. Pb poisoning can cause insomnia, hallucination, headache, anxiety, myasthenia and other symptoms in human body, and can damage central nervous system of human body, and has serious harm to kidney, liver, reproductive system and brain. Therefore, an efficient and environment-friendly method for treating Pb-containing wastewater is sought, so that the Pb-containing wastewater is discharged up to the standard, and the environmental pollution is reduced, thus being an environmental problem which is urgently needed to be researched and solved. The adsorption method is one of the main methods for treating the heavy metal wastewater at present, and has the advantages of high efficiency, simplicity, convenience, good selectivity and the like.
The magnesium oxide has the characteristics of high activity, excellent adsorption capacity, high buffering capacity, basically no corrosiveness, environmental friendliness and the like, is an environment-friendly, safe and environment-friendly water treatment agent, and on the other hand, salt lake brine, seawater and magnesium-containing minerals contain a large amount of magnesium salts, so that the magnesium oxide has wide sources and low preparation cost, and has wide application prospects in the environment-friendly field. Such as removal of dyes, heavy metal ions, phosphorous and ammonia compounds, etc. from the wastewater.
However, the magnesium oxide adsorbents prepared at present are all basically ultrafine powder, and have good adsorption performance, but solid-liquid separation after adsorption is extremely difficult, and industrial application is difficult, so that development of a magnesium oxide adsorbent with excellent adsorption performance and easy solid-liquid separation is extremely necessary.
Disclosure of Invention
The invention provides a preparation method of millimeter-sized monodisperse magnesium oxide pellets and application of the millimeter-sized monodisperse magnesium oxide pellets in heavy metal lead removal.
The preparation method of the millimeter-sized monodisperse magnesium oxide pellets comprises the following steps: uniformly mixing the magnesium salt, the structure inducer, the precipitator and the solvent, then pouring the mixed solution into a high-pressure reaction kettle, reacting for 1-6 hours at 85-180 ℃, cooling to room temperature, centrifugally washing, drying, and roasting the product at 300-850 ℃ for 1-5 hours to obtain the millimeter-sized monodisperse magnesium oxide pellets.
The magnesium salt is one or more selected from magnesium nitrate, magnesium sulfate and magnesium chloride.
The mass concentration of the magnesium ion substance in the mixed solution is 0.05-3mol/L.
The structure inducer is one or more selected from sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and polyvinylpyrrolidone.
The amount of the substance of the structure inducer is 0.05-2 times of the amount of the substance of magnesium ions.
The precipitant is one or more selected from urea, triethylamine, hexamethylenetetramine and sodium hydroxide.
The amount of the substance of the precipitant is 1.5-5 times of the amount of the substance of magnesium ions.
The solvent is a mixed solvent consisting of deionized water and dimethyl sulfoxide.
The volume ratio of deionized water to dimethyl sulfoxide in the mixed solvent is 1-20:1.
The millimeter-sized monodisperse magnesium oxide pellets prepared above are applied to removal of heavy metal lead in water.
The invention dissolves magnesium salt and precipitant in common solvent, obtains precursor under mild condition, and then directly obtains high-dispersion millimeter-sized magnesium oxide pellets through roasting without steps of extrusion, granulation and the like. The preparation method of the invention has the advantages of simple equipment, mild synthesis condition, simple operation, abundant raw material sources, low price and great application prospect. The magnesium oxide pellets prepared by the method have higher specific surface area and rich pore structure, are favorable for adsorbing heavy metal lead, and show excellent performance in the aspect of removing the heavy metal lead. More importantly, the magnesium oxide pellets prepared by the method have larger size, do not need operations such as filtration, centrifugation and the like, can be subjected to automatic solid-liquid separation, are convenient for industrial application, not only reduce the cost, but also improve the efficiency, and solve the problem that powder materials are difficult to separate.
Drawings
Fig. 1 is an XRD pattern of the magnesium oxide precursor prepared in example 1.
FIG. 2 is a photograph showing the magnesium oxide pellets prepared in example 1.
FIG. 3 is a photograph showing the magnesium oxide pellets prepared in example 2.
Fig. 4 is an XRD pattern of the magnesium oxide pellets prepared in example 2.
FIG. 5 is a graph showing the removal rate of lead ions from an aqueous solution by using the magnesium oxide pellets of example 1.
Detailed Description
The invention will be further illustrated by the following examples in order to provide a better understanding of the manner in which the invention operates, but the scope of the invention is not limited thereto.
Example 1
Weighing 6.3g of magnesium chloride, placing 7.2g of urea in a 150mL beaker, adding 60mL of deionized water, 10mL of dimethyl sulfoxide and 2g of sodium dodecyl sulfate, magnetically stirring at room temperature for 20 minutes, pouring the solution into a reaction kettle, crystallizing at 110 ℃ for 6 hours, centrifugally washing with deionized water, placing the precipitate in a 40 ℃ oven, drying for 12 hours to obtain a magnesium oxide precursor, and then placing in a muffle furnace, roasting at 600 ℃ for 3 hours to obtain millimeter-level high-dispersion magnesium oxide pellets. Fig. 1 is an XRD pattern of the precipitate obtained after the hydrothermal reaction, from which it can be seen that the magnesium oxide precursor is basic magnesium carbonate. FIG. 2 is a photograph showing the magnesium oxide pellets obtained after calcination, and it can be seen from the photograph that the magnesium oxide pellets obtained are spherical and have good dispersibility and a particle size of about 0.5 mm.
Example 2
5.0g of magnesium sulfate heptahydrate is weighed, 8.4g of hexamethylenetetramine is placed in a 150mL beaker, 60mL of deionized water, 9mL of dimethyl sulfoxide and 1g of sodium dodecyl sulfate are added, after magnetic stirring is carried out for 20 minutes at room temperature, the solution is poured into a reaction kettle, after crystallization for 8 hours at 140 ℃, the deionized water is centrifugally washed, the precipitate is placed in a baking oven at 40 ℃ for drying for 12 hours, and then the precipitate is placed in a muffle furnace for roasting for 3 hours at 600 ℃ to obtain millimeter-level high-dispersion magnesium oxide pellets. FIG. 3 is a photograph showing the magnesium oxide pellets obtained after calcination, and it can be seen from the figure that the magnesium oxide pellets obtained are spherical and have good dispersibility and a particle size of about 1 mm. Fig. 4 is an XRD pattern of the obtained magnesium oxide, and it can be seen from the pattern that diffraction peaks of the material obtained after calcination show characteristic diffraction peaks of standard magnesium oxide, indicating that the method can prepare pure-phase magnesium oxide.
Application example 1
0.1g of the magnesium oxide prepared in example 1 was weighed into a 1L beaker, and 500ml of Pb-containing powder was added 2+ Wherein Pb 2+ After magnetically stirring at room temperature for 20 min, the upper layer solution was filtered through a 0.22 μm filter membrane and Pb was measured by ICP-MS 2+ Is a concentration of (3). The result shows that the removal rate of the prepared magnesium oxide pellets to lead reaches more than 90%, and the magnesium oxide pellets show extremely high removal amount and removal efficiency. The results of the different time period removal rates are shown in fig. 5.

Claims (2)

1. A preparation method of millimeter-sized monodisperse magnesium oxide pellets is characterized by weighing 5.0g of magnesium sulfate heptahydrate, placing 8.4g of hexamethylenetetramine in a 150mL beaker, adding 60mL of deionized water, 9mL of dimethyl sulfoxide and 1g of sodium dodecyl sulfate, magnetically stirring at room temperature for 20 minutes, pouring the solution into a reaction kettle, crystallizing at 140 ℃ for 8 hours, centrifuging the deionized water, washing, drying the precipitate in a baking oven at 40 ℃ for 12 hours, and roasting in a muffle furnace at 600 ℃ for 3 hours to obtain millimeter-sized monodisperse magnesium oxide pellets.
2. The application of the millimeter-sized monodisperse magnesium oxide pellets prepared by the method in removing heavy metal lead in water.
CN202110415122.7A 2021-04-17 2021-04-17 Preparation method and application of millimeter-sized monodisperse magnesium oxide pellets Active CN113262753B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101209847A (en) * 2006-12-27 2008-07-02 中国科学院大连化学物理研究所 Method for preparing monodisperse magnesium oxide microsphere
CN106082287A (en) * 2016-06-14 2016-11-09 中山大学 A kind of preparation method of magnesium oxide
CN108569712A (en) * 2018-04-04 2018-09-25 内江师范学院 Preparation method of tetragonal body shape magnesium oxide material and products thereof and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101209847A (en) * 2006-12-27 2008-07-02 中国科学院大连化学物理研究所 Method for preparing monodisperse magnesium oxide microsphere
CN106082287A (en) * 2016-06-14 2016-11-09 中山大学 A kind of preparation method of magnesium oxide
CN108569712A (en) * 2018-04-04 2018-09-25 内江师范学院 Preparation method of tetragonal body shape magnesium oxide material and products thereof and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"聚乙二醇辅助合成氧化镁及其处理含铅溶液的性能";程文婷，等;《中国科学: 化学》;第1490-1496页 *

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