CN110250201B - Leaf-burst-bud complex-leaf-shaped multilevel-structure nano magnesium hydroxide and preparation method and application thereof - Google Patents
Leaf-burst-bud complex-leaf-shaped multilevel-structure nano magnesium hydroxide and preparation method and application thereof Download PDFInfo
- Publication number
- CN110250201B CN110250201B CN201910540873.4A CN201910540873A CN110250201B CN 110250201 B CN110250201 B CN 110250201B CN 201910540873 A CN201910540873 A CN 201910540873A CN 110250201 B CN110250201 B CN 110250201B
- Authority
- CN
- China
- Prior art keywords
- leaf
- magnesium hydroxide
- bud
- burst
- nano magnesium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/06—Aluminium; Calcium; Magnesium; Compounds thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/10—Magnesium; Oxides or hydroxides thereof
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
-
- 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
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Dentistry (AREA)
- Environmental & Geological Engineering (AREA)
- Plant Pathology (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Mycology (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Biotechnology (AREA)
- Geology (AREA)
- Microbiology (AREA)
- Thermal Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Pest Control & Pesticides (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a method in the technical field of environmental protection, in particular to leaf-burst-bud complex-leaf-shaped multilevel-structure nano magnesium hydroxide and a preparation method and application thereof. Modifying with magnesium ion solution as raw material to obtain nanometer magnesium hydroxide material, modifying the surface with leaf explosion bud extract, and modifying with impregnation phase conversion under doping of lithium source to obtain leaf explosion bud multi-leaf multi-level structure nanometer magnesium hydroxide material. The prepared leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material can be applied to antibiosis, water pollution control or polluted environment restoration. The leaf-burst-bud multi-leaf-shaped multi-level-structure nano magnesium hydroxide material prepared by the invention has stable property, can remove various inorganic and organic compounds, has simple preparation process and cheap and easily-obtained raw materials, and belongs to a multipurpose environment-friendly material.
Description
Technical Field
The invention relates to a method in the technical field of environmental protection, in particular to leaf-burst-bud complex-leaf-shaped multilevel-structure nano magnesium hydroxide and a preparation method and application thereof.
Background
The nano magnesium hydroxide is used as an environment-friendly inorganic nano material, and has the properties of good thermal stability, strong adsorption capacity, large specific surface area, no toxicity, no smoke, no corrosion and the like, so that the nano magnesium hydroxide is called as a green safe neutralizer and the like. The nano magnesium hydroxide is widely applied to the fields of water treatment, medicine, chemical industry, environmental protection and the like due to the properties of the nano magnesium hydroxide, such as chemical adsorption of toxic gases and organic matters, heavy metal removal, neutralization of acid-containing wastewater, flame retardant and the like. At present, the research and development of the nano magnesium hydroxide are continuously developed, the application field is continuously expanded, and the nano magnesium hydroxide has wide application prospect in the future.
Firstly, the nano magnesium hydroxide is very easily influenced by the environment due to the higher reaction activity of the nano material, so that the nano material is inactivated; secondly, because of the strong polarity of the surfaces of the magnesium hydroxide particles, secondary agglomeration is easy to occur among the particles. Therefore, how to utilize the unique superiority of the nano magnesium hydroxide material and avoid the deficiency is very urgent and extremely important. Doping of the compound can modify the physical and chemical properties of the parent compound, such as increased defect concentration and increased catalytic activity. Incorporation of foreign elements into the crystal lattice of a compound can create lattice defects such as vacancies, interstitial atoms, substitutional atoms, and dislocations, which can often modify to some extent the physical and chemical properties of the parent compound, even mutations in the properties. Therefore, in order to improve the activity of nano magnesium hydroxide, a doping modification method is an effective method.
In recent years, with the improvement of the nano material preparation technology, the nano material with a multilevel structure has become a hot spot of the nano material. The nano material with the multilevel structure is modified, so that the agglomeration phenomenon among particles is effectively improved, the property is stable, and the catalytic activity is well enhanced. The leaf burst bud (also called as the root of the fallen land) is a common succulent plant, the plant grows to have compound leaves, small leaves grow on the big leaves, and the small leaves are long and round to oval. In addition, the leaf bud has certain antibacterial property, and is a common Chinese herbal medicine. So far, no report of the multilevel-structure nano magnesium hydroxide with the leaf burst bud complex leaf structure is found.
Disclosure of Invention
The invention aims to provide leaf-burst-bud multi-leaf-shaped multilevel-structure nano magnesium hydroxide and a preparation method and application thereof, aiming at the defects of the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of leaf burst bud multi-leaf multilevel structure nano magnesium hydroxide comprises the steps of modifying a magnesium ion solution serving as a raw material to obtain a nano magnesium hydroxide material, modifying the surface of the nano magnesium hydroxide material serving as a parent compound through a leaf burst bud extract, and then obtaining the leaf burst bud multi-leaf multilevel structure nano magnesium hydroxide material through impregnation phase conversion modification under the doping of a lithium source.
The method specifically comprises the following steps:
(1) adding polyethylene glycol, acetate and sorbitol into the magnesium ion solution, mixing, reacting in a water bath at constant temperature of 50-80 ℃, adjusting the pH of the system to be more than or equal to 9, reacting for 2-3h, naturally cooling to room temperature, and collecting solid to obtain a nano magnesium hydroxide material;
(2) mixing the nano magnesium hydroxide material with the leaf bud extract solution, adding humate, and uniformly stirring to obtain a nano magnesium hydroxide suspension; wherein the adding amount of the nano magnesium hydroxide is 0.5-5% (mass ratio); the mass ratio of the leaf bud extract to the nano magnesium hydroxide in the mixed solution is controlled to be 0.1-10: 1;
(3) adding the obtained nano magnesium hydroxide suspension into a lithium ion solution, adding tartaric acid, stirring and uniformly mixing, adjusting the pH value of a system to be more than or equal to 12, distilling at the temperature of 60-80 ℃ to obtain paste, and washing to obtain the leaf burst bud compound leaf multi-stage structure nano magnesium hydroxide material; wherein the mass ratio of tartaric acid to the lithium ion compound in the lithium ion solution is controlled to be 0.5-1.5: 1; the volume ratio of the nano magnesium hydroxide suspension to the lithium ion solution is controlled to be 1-10: 1.
Washing the paste with distilled water and ethanol for several times, and drying at 80-100 ℃ to obtain the leaf burst bud multi-leaf multi-level structure nano magnesium hydroxide material.
In the step (1), the final concentration of polyethylene glycol in the system is 5.0-10.0wt%, the final concentration of acetate is 1.0-5.0wt%, and the final concentration of sorbitol is 0.1-0.5 wt%.
The magnesium ion solution in the step (1) is seawater, brine, bischofite or artificially prepared magnesium chloride solution containing 0.4-0.6mol/L magnesium ions; the acetate is one or more of sodium acetate, ammonium acetate and potassium acetate.
The leaf bud burst extract is prepared by crushing a leaf bud burst plant fresh sample, adding an extraction solvent to ensure that the weight ratio of the leaf bud burst plant fresh sample to the extraction solvent is 1:4-6, soaking for 1-3 days, performing reflux extraction, collecting a leaching solution, recovering the leaching solution under reduced pressure, and performing freeze drying to obtain the leaf bud burst extract; the extraction solvent is one or more of water, ethanol, methanol and ethyl acetate; the fresh sample of the leaf burst plant is the whole plant of the leaf burst plant or the fresh product of any part of the root, the stem and the leaf.
Adding the humate in the step (2) into the mixed solution to ensure that the final concentration of the humate in the mixed solution is 0.2-0.5 wt%; the humate is one or more of sodium humate, potassium humate and ammonium humate.
And (4) the lithium ion solution in the step (3) is a lithium chloride solution or a lithium nitrate solution.
And (3) adjusting the pH value of the system to be one or more of ammonia water, a sodium hydroxide solution or a potassium hydroxide solution.
The prepared nano magnesium hydroxide material has a leaf-exploded-bud compound-leaf-shaped multi-stage structure, a large number of small nano sheets are dotted at the edges of the large nano sheets, and the small nano sheets are approximately circular.
The application of the nano magnesium hydroxide material with the leaf burst bud compound leaf-shaped multi-level structure is in antibiosis, water pollution control or polluted environment restoration.
The invention has the advantages that:
the leaf-burst-bud multi-leaf-shaped multilevel-structure nano magnesium hydroxide material has stable property, can remove various inorganic and organic compounds, has simple preparation process and cheap and easily-obtained raw materials, and belongs to a multipurpose environment-friendly material; the method specifically comprises the following steps:
1) the material of the invention breaks the limitation that the treatment effect is not ideal because of the agglomeration of the nano magnesium hydroxide material in the past, has stable property, can remove various inorganic and organic compounds, and belongs to a multipurpose environment-friendly material.
2) In the preparation process of the leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material, nano magnesium hydroxide is immersed in a lithium ion solution to promote the formation of lattice defect active sites, and the catalytic activity is well enhanced.
3) The leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material has a simple preparation process, and the raw materials are cheap and easy to obtain. The magnesium ion solution used in the preparation process of the material is selected from magnesium salt water solution or bittern rich in magnesium ions or seawater. A large amount of magnesium in nature is dissolved in seawater or brine in the form of chloride, and the material has wide magnesium ion sources for preparation and higher comprehensive development and utilization values.
Drawings
FIG. 1 is a scanning electron micrograph of a prepared material according to an embodiment of the present invention; the prepared nano magnesium hydroxide has a leaf-burst-bud multi-leaf multi-stage structure, a large number of small nano sheets are dotted on the edge of the large nano sheet, and the small nano sheets are approximately round.
Detailed Description
The present invention is further illustrated by the following examples, which, however, are not intended to limit the scope of the invention.
Example 1
Preparing a leaf-burst-bud complex leaf-shaped multilevel-structure nano magnesium hydroxide material:
(1) adding polyethylene glycol with the final concentration of 5%, sodium acetate with the final concentration of 2.0% and sorbitol with the final concentration of 0.5% into 0.4mol/L brine, keeping the temperature of a water bath at 50 ℃, dropwise adding ammonia water while stirring, adjusting the pH of the system to be 9, reacting for 2h, naturally cooling to room temperature, washing the product for several times by using distilled water and ethanol to obtain a nano magnesium hydroxide material, and drying at 60 ℃ for later use.
The bittern is rich in magnesium from salt lake, and is prepared into solution containing magnesium ion at concentration of 0.4mol/L
(2) Pulverizing the whole plant of the leaf bud-bursting plant, adding ethanol with the weight of 4 times of the plant, soaking for 1 day, reflux extracting, collecting the extract, recovering the extract under reduced pressure, and freeze-drying to obtain the leaf bud-bursting extract.
(3) Adding the nano magnesium hydroxide material obtained in the step (1) into the leaf explosion bud extract solution according to the mass ratio of 2%, controlling the mass ratio of the leaf explosion bud extract to the nano magnesium hydroxide in the solution to be 1:1, adding sodium humate with the final concentration of 0.3%, and stirring and mixing for 1h to obtain a nano magnesium hydroxide suspension.
(4) Adding the obtained nano magnesium hydroxide suspension into a lithium chloride solution, adding tartaric acid, controlling the mass ratio of tartaric acid to lithium chloride in the mixed solution to be 0.5:1, controlling the volume ratio of the nano magnesium hydroxide suspension to the lithium chloride solution to be 1:1, mixing and stirring for 30min, dropwise adding ammonia water while stirring, adjusting the pH of a system to be 12, gradually evaporating excessive solvent from the mixture at 60 ℃ to form paste, collecting the paste, washing the paste for a plurality of times by using distilled water and ethanol, drying the paste at 80 ℃ to obtain the leaf-burst-bud complex-leaf-shaped multi-stage-structure nano magnesium hydroxide material (see figure 1), drying and sealing for later use.
As can be seen from fig. 1, from the appearance, a large number of small nanosheets are dotted on the edge of the large nanosheet, the small nanosheets are approximately circular, and the multilevel structure is similar to a leaf bursting bud complex leaf structure (small leaves are grown on the large leaves, and the small leaves are oval to elliptical). The material is named as leaf burst bud complex leaf-shaped multilevel-structure nano magnesium hydroxide.
The prepared leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material is used for bacteriostasis, escherichia coli is used as a model strain, the minimum bacteriostasis concentration and the 24-hour sterilization rate of the prepared material are tested, and the sterilization rate is over 99 percent. Mixing and dissolving bacteriostatic agents with different concentrations in a nutrient broth culture medium by adopting a nutrient broth dilution method, then inoculating bacteria, and determining the minimum concentration of the bacteriostatic agents for inhibiting the growth of tested bacteria according to the growth or non-growth of the bacteria, namely the minimum bacteriostatic concentration.
The 24h sterilization rate is calculated according to the following formula:
K＝(A-B)/B×100％
in the formula:
k-24h kill rate/%;
a-the number of colonies for viable counting of bacteria in the positive control group;
b-the number of colonies counted by the living body of bacteria after the action of the antibacterial powder.
Example 2
Preparing a leaf-burst-bud complex leaf-shaped multilevel-structure nano magnesium hydroxide material:
(1) adding polyethylene glycol with the final concentration of 8%, ammonium acetate with the final concentration of 1.0% and sorbitol with the final concentration of 0.1% into 0.5mol/L seawater, keeping the temperature of 60 ℃ in a water bath, dropwise adding sodium hydroxide while stirring, adjusting the pH of the system to be 10, reacting for 2.5h, naturally cooling to room temperature, washing the product for several times by using distilled water and ethanol to obtain the nano magnesium hydroxide material, and drying at 60 ℃ for later use. The seawater is rich in magnesium, and is prepared into solution containing magnesium ions with concentration of 0.5 mol/L.
(2) Pulverizing root of leaf bud plant, adding ethyl acetate 5 times of the weight of the plant, soaking for 2 days, reflux extracting, collecting extractive solution, recovering the extractive solution under reduced pressure, and freeze drying to obtain leaf bud extract.
(3) Adding the nano magnesium hydroxide material obtained in the step (1) into the leaf explosion bud extract solution according to the mass ratio of 0.5%, controlling the mass ratio of the leaf explosion bud extract to the nano magnesium hydroxide to be 0.1:1, adding potassium humate with the final concentration of 0.2%, stirring and mixing for 2h to obtain a nano magnesium hydroxide suspension.
(4) Adding the obtained nano magnesium hydroxide suspension into a lithium nitrate solution, adding tartaric acid, controlling the mass ratio of tartaric acid to lithium nitrate in the mixed solution to be 1:1, controlling the volume ratio of the nano magnesium hydroxide suspension to the lithium nitrate solution to be 5:1, mixing and stirring for 10min, dropwise adding sodium hydroxide while stirring, adjusting the pH of a system to be 12.5, gradually evaporating excessive solvent from the mixture at 70 ℃ to form paste, collecting the paste, washing the paste for a plurality of times by distilled water and ethanol, drying the paste at 90 ℃ to obtain the leaf-burst-bud complex leaf-shaped multi-stage-structure nano magnesium hydroxide material, drying and sealing for later use.
The prepared leaf-bursting-bud multi-level-structure nano magnesium hydroxide material is used in a catalytic ozonation reaction system to research the removal effect of ofloxacin in a water body. Taking an ofloxacin solution with the initial concentration of 50mg/L as a research object, wherein the flow rate of ozone is 0.1L/min, and the addition amount of the leaf bud complex leaf-shaped multi-stage structure nano magnesium hydroxide material is 0.3g/L, compared with single ozone oxidation, after the leaf bud complex leaf-shaped multi-stage structure nano magnesium hydroxide material is added, the removal rate of ofloxacin is improved by 40.5%.
Example 3
Preparing a leaf-burst-bud complex leaf-shaped multilevel-structure nano magnesium hydroxide material:
(1) adding polyethylene glycol with the final concentration of 10%, potassium acetate with the final concentration of 5.0% and sorbitol with the final concentration of 0.3% into a bischofite solution with the concentration of 0.6mol/L, keeping the temperature of a water bath at 80 ℃, dropwise adding potassium hydroxide while stirring, adjusting the pH of a system to be 10.5, reacting for 3 hours, naturally cooling to the room temperature, washing a product for several times by distilled water and ethanol to obtain a nano magnesium hydroxide material, and drying at the temperature of 60 ℃ for later use. The bischofite is natural bischofite taken from salt lake, and is prepared into solution containing magnesium ions with concentration of 0.6mol/L when in use.
(2) Crushing leaves of the leaf bud-bursting plant, adding methanol with the weight 6 times of the leaves of the leaf bud-bursting plant, soaking for 3 days, performing reflux extraction, collecting a leaching solution, recovering the leaching solution under reduced pressure, and performing freeze drying to obtain the leaf bud-bursting extract.
(3) Adding the nano magnesium hydroxide material obtained in the step (1) into the leaf explosion bud extract solution according to the mass ratio of 5%, controlling the mass ratio of the leaf explosion bud extract to the nano magnesium hydroxide to be 10:1, adding ammonium humate with the final concentration of 0.5%, and stirring and mixing for 1.5h to obtain a nano magnesium hydroxide suspension.
(4) Adding the obtained nano magnesium hydroxide suspension into a lithium chloride solution, adding tartaric acid, controlling the mass ratio of tartaric acid to lithium chloride in the mixed solution to be 1.5:1, controlling the volume ratio of the nano magnesium hydroxide suspension to the lithium chloride solution to be 10:1, mixing and stirring for 50min, dropwise adding potassium hydroxide while stirring, adjusting the pH of a system to be 13, gradually evaporating excessive solvent from the mixture at 80 ℃ to form paste, collecting the paste, washing the paste for a plurality of times by using distilled water and ethanol, drying the paste at 100 ℃ to obtain the leaf-burst-bud complex leaf-shaped multi-stage structure nano magnesium hydroxide material, and drying and sealing the nano magnesium hydroxide material for later use.
The prepared leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material is used for removing heavy metal-containing wastewater, and the effect of removing heavy metals in water is researched. Adding 2 percent (mass ratio) of the leaf-exploded-bud multi-leaf multi-stage-structure nano magnesium hydroxide material into wastewater containing heavy metals (5 mg/L of copper, 3mg/L of zinc and 2mg/L of lead), wherein the removal rate of the heavy metals exceeds 90 percent.
Claims (7)
1. A preparation method of leaf burst bud compound leaf-shaped multilevel-structure nano magnesium hydroxide is characterized by comprising the following steps:
(1) adding polyethylene glycol, acetate and sorbitol into the magnesium ion solution, mixing, reacting in a water bath at constant temperature of 50-80 ℃, adjusting the pH of the system to be more than or equal to 9, reacting for 2-3h, naturally cooling to room temperature, and collecting solid to obtain a nano magnesium hydroxide material;
(2) mixing the nano magnesium hydroxide material with the leaf bud extract solution, adding humate, and uniformly stirring to obtain a nano magnesium hydroxide suspension; wherein the mass ratio of the adding amount of the nano magnesium hydroxide is 0.5-5%; the mass ratio of the leaf bud extract to the nano magnesium hydroxide in the mixed solution is controlled to be 0.1-10: 1;
(3) adding the obtained nano magnesium hydroxide suspension into a lithium ion solution, adding tartaric acid, stirring and uniformly mixing, adjusting the pH value of a system to be more than or equal to 12, distilling at the temperature of 60-80 ℃ to obtain paste, and washing to obtain the leaf burst bud compound leaf multi-stage structure nano magnesium hydroxide material; wherein the mass ratio of tartaric acid to the lithium ion compound in the lithium ion solution is controlled to be 0.5-1.5: 1; the volume ratio of the nano magnesium hydroxide suspension to the lithium ion solution is controlled to be 1-10: 1;
washing the paste with distilled water and ethanol for several times, and drying at 80-100 ℃ to obtain the leaf burst bud multi-leaf multi-level structure nano magnesium hydroxide material;
the leaf bud burst extract is prepared by crushing a leaf bud burst plant fresh sample, adding an extraction solvent to ensure that the weight ratio of the leaf bud burst plant fresh sample to the extraction solvent is 1:4-6, soaking for 1-3 days, performing reflux extraction, collecting a leaching solution, recovering the leaching solution under reduced pressure, and performing freeze drying to obtain the leaf bud burst extract; the extraction solvent is one or more of water, ethanol, methanol and ethyl acetate; the fresh sample of the leaf burst plant is the whole plant of the leaf burst plant or the fresh product of any part of the root, the stem and the leaf.
2. The leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material obtained by the preparation method according to claim 1 is characterized in that: in the step (1), the final concentration of polyethylene glycol in the system is 5.0-10.0wt%, the final concentration of acetate is 1.0-5.0wt%, and the final concentration of sorbitol is 0.1-0.5 wt%.
3. The leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material obtained by the preparation method according to claim 1 is characterized in that: the magnesium ion solution in the step (1) is seawater, brine, bischofite or artificially prepared magnesium chloride solution containing 0.4-0.6mol/L magnesium ions; the acetate is one or more of sodium acetate, ammonium acetate and potassium acetate.
4. The leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material obtained by the preparation method according to claim 1 is characterized in that: adding the humate in the step (2) into the mixed solution to ensure that the final concentration of the humate in the mixed solution is 0.2-0.5 wt%; the humate is one or more of sodium humate, potassium humate and ammonium humate.
5. The leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material obtained by the preparation method according to claim 1 is characterized in that: and (4) the lithium ion solution in the step (3) is a lithium chloride solution or a lithium nitrate solution.
6. The leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material prepared by the method of claim 1 is characterized in that: the nano magnesium hydroxide material has a leaf burst bud complex leaf-shaped multi-stage structure, a large number of small nano sheets are dotted on the edge of the large nano sheet, and the small nano sheets are approximately circular.
7. The application of the leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material as claimed in claim 6 is characterized in that: the leaf-burst-bud multi-leaf multi-level-structure nano magnesium hydroxide material is applied to antibiosis, water pollution control or polluted environment restoration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910540873.4A CN110250201B (en) | 2019-06-21 | 2019-06-21 | Leaf-burst-bud complex-leaf-shaped multilevel-structure nano magnesium hydroxide and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910540873.4A CN110250201B (en) | 2019-06-21 | 2019-06-21 | Leaf-burst-bud complex-leaf-shaped multilevel-structure nano magnesium hydroxide and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110250201A CN110250201A (en) | 2019-09-20 |
| CN110250201B true CN110250201B (en) | 2022-03-22 |
Family
ID=67920167
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910540873.4A Active CN110250201B (en) | 2019-06-21 | 2019-06-21 | Leaf-burst-bud complex-leaf-shaped multilevel-structure nano magnesium hydroxide and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110250201B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177289A (en) * | 2007-11-05 | 2008-05-14 | 昆明理工大学 | Method for preparing fibrous nano magnesium hydrate |
| CN101376511B (en) * | 2007-11-23 | 2010-08-11 | 清华大学深圳研究生院 | Preparation of nano magnesium hydrate |
| WO2011136521A9 (en) * | 2010-04-28 | 2012-06-14 | 한국생명공학연구원 | Water-soluble fluorescent fullerene derivative, and preparation method thereof |
| CN102969492A (en) * | 2012-12-04 | 2013-03-13 | 广州有色金属研究院 | Carbon-coated doping modified lithium titanate and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724734B (en) * | 2013-12-18 | 2017-08-25 | 中国科学院福建物质结构研究所 | A kind of manufacture lightweight, high-specific surface area, the method for bouquet type nano-sized magnesium hydroxide |
-
2019
- 2019-06-21 CN CN201910540873.4A patent/CN110250201B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177289A (en) * | 2007-11-05 | 2008-05-14 | 昆明理工大学 | Method for preparing fibrous nano magnesium hydrate |
| CN101376511B (en) * | 2007-11-23 | 2010-08-11 | 清华大学深圳研究生院 | Preparation of nano magnesium hydrate |
| WO2011136521A9 (en) * | 2010-04-28 | 2012-06-14 | 한국생명공학연구원 | Water-soluble fluorescent fullerene derivative, and preparation method thereof |
| CN102969492A (en) * | 2012-12-04 | 2013-03-13 | 广州有色金属研究院 | Carbon-coated doping modified lithium titanate and preparation method thereof |
Non-Patent Citations (5)
| Title |
|---|
| Catalytic Ozonation of Sulfonamide, Fluoroquinolone,and Tetracycline Antibiotics Using Nano-Magnesium Hydroxide from Natural Bischofite;Qi Sun et,al;《Water Air Soil Pollut》;20190212;第230卷(第3期);第2-3页第2.2节、图1，第8页第3.1节 * |
| Effect of LiOH Addition on Dehydration Reaction of Mg(OH)(2);Kurosawa, R et,al;《JOURNAL OF CHEMICAL ENGINEERING OF JAPAN》;20190131;第52卷(第1期);第152-158页 * |
| 氢氧化镁对水质、底质改良的研究与应用;黄永强等;《渔业研究》;20171231;第39卷(第2期);第144页第3节 * |
| 纳米氢氧化镁/氧化镁的制备及其抗菌性能研究;郑军;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20150215;第20-21页第2.2.2.1节 * |
| 纳米氧化镁及其掺杂粉体的制备与吸附、抗菌性能;王维;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20091215;第48页第4.1节，第75-76页第6.2.2节，第99页第7.4.3节，第103页第7.5节 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110250201A (en) | 2019-09-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109095751B (en) | Method for treating activated sludge through lower-temperature thermokalite decomposition | |
| WO2016115964A1 (en) | Ecological nitrogen fertilizer and preparation method | |
| CN110813237A (en) | Application of Mg/Fe oxide modified biochar nanocomposite in removal of antibiotics | |
| CN102260163B (en) | Method for recovering lactic acid from marigold fermentation wastewater | |
| CN106268259A (en) | SO in a kind of flue gas2method with the removing of Hg biochemical synchronization | |
| CN105502566A (en) | Environment-friendly wastewater treating agent and preparing method thereof | |
| WO2021057556A1 (en) | System and method for remediation of river/lake water body by means of floating water purification facility | |
| CN104707560A (en) | Preparation method of modified mesopore TiO2 capable of effectively removing phosphorus in wastewater | |
| CN108623414A (en) | A kind of improvement salt-soda soil type biological organic complex fertilizer and preparation method thereof | |
| CN110250201B (en) | Leaf-burst-bud complex-leaf-shaped multilevel-structure nano magnesium hydroxide and preparation method and application thereof | |
| CN107381836A (en) | A kind of water conditioner | |
| CN108866105B (en) | Method for producing nano cadmium sulfide by using enterobacter LY6 | |
| CN107416863B (en) | Method for preparing industrial-grade ammonium salt from wastewater generated in iron phosphate production | |
| CN104609573A (en) | Method for treating acid waste water containing arsenic | |
| CN115478182B (en) | Preparation method of ionic rare earth leaching agent | |
| CN111226528A (en) | Method for delaying soil salt crystallization by utilizing bacillus subtilis | |
| CN108083450B (en) | Complexing agent for rare earth wastewater | |
| CN105777221B (en) | Method for preparing organic carbon fertilizer from high-concentration lysine fermentation waste liquid | |
| CN112852886B (en) | Method for preparing struvite by recovering nitrogen and phosphorus from chromium-containing sewage | |
| CN110078101B (en) | Preparation and application of tea fungus disease resistant nano magnesium hydroxide | |
| CN104445827A (en) | Method for synthesizing jarosite to process pickling waste water employing biological method | |
| EP2319820A1 (en) | A plant nutrient obtained from the rice husk and a process of preparation thereof | |
| CN109704838A (en) | A kind of municipal sludge trough type fermentation technique | |
| JP6148485B2 (en) | How to grow rice | |
| CN104707571B (en) | Method for preparing magnesium-aluminum salt material with slow-release phosphorus removal function by biological template method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |