CN110078101B - Preparation and application of tea fungus disease resistant nano magnesium hydroxide - Google Patents
Preparation and application of tea fungus disease resistant nano magnesium hydroxide Download PDFInfo
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- CN110078101B CN110078101B CN201910462167.2A CN201910462167A CN110078101B CN 110078101 B CN110078101 B CN 110078101B CN 201910462167 A CN201910462167 A CN 201910462167A CN 110078101 B CN110078101 B CN 110078101B
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- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to preparation and application of tea fungus disease resistant nano magnesium hydroxide. The preparation method of the nano magnesium hydroxide comprises the steps of preparing a magnesium chloride hexahydrate solution, preparing a sodium hydroxide solution, stirring and preparing the nano magnesium hydroxide. The method uses X-ray powder diffraction (XRD) and a scanning electron microscope to characterize the particle size and the morphology of the obtained nano magnesium hydroxide, the particle size of the nano magnesium hydroxide is 10-20 nm, the Zeta potential is +15.2 mV, and the nano magnesium hydroxide is dispersed in water with the concentration of 5-50 mg/mL. The invention opens up the application of nano magnesium hydroxide in tea antifungal. Experiments show that the nano magnesium hydroxide has good antibacterial effect on tea fungus diseases, the concentration and the inhibition rate are in positive correlation, and the inhibition rate is higher when the concentration is higher. The nano magnesium hydroxide provided by the invention is convenient to obtain materials, low in price, green and environment-friendly, and has the characteristics of simple preparation method, high prevention and treatment efficiency and remarkable social and economic benefits.
Description
Technical Field
The invention relates to preparation and application of a tea fungus disease resistant nano material, in particular to preparation and application of tea fungus disease resistant nano magnesium hydroxide, and belongs to the technical field of plant protection.
Background
According to statistics, the tea leaves are exported in 36.47 ten thousand tons in 2018 all the year, and the export amount is $ 17.38 hundred million. Tea fungus diseases are one of the important causes of tea yield reduction, and the tea fungus diseases cause huge economic losses to tea production every year. At present, the means of widely applying tea to preventing and treating fungal diseases is still more traditional chemical prevention and treatment. The chemical preparation has the defects of easy residue, biological toxicity, environmental pollution and the like in long-term use, so that a novel pesticide which can effectively inhibit the tea fungi and has low toxicity and environmental protection needs to be developed and developed.
Currently, with the wide application of high-efficiency and strong-selectivity bactericides, the drug resistance of plant pathogenic bacteria to the bactericides is getting more and more serious. Compared with organic and natural antibacterial agents, the inorganic nano material has the advantages of antibacterial property, low toxicity, small harm to environmental ecology and human health, heat resistance, difficult generation of resistance by pathogenic bacteria and the like. The nano material can be used as a novel bactericide and insecticide and is gradually applied to the field of plant protection. Due to the extraordinary characteristics of surface and interface effects, quantum size effects, small size effects, macroscopic effects and the like, the nano material has wide application in different agricultural fields. Compared with the traditional inorganic antibacterial agent, the nano bactericide has better antibacterial effect.
However, since the nanomaterial itself has some toxicity to organisms, environmental safety should be a major concern when selecting the nanomaterial as an antifungal agent. The nano magnesium hydroxide is used as a safe, green and safe water treatment agent without environmental pollution, has no obvious toxicity to human cells and organisms, and is widely applied to the environment and the actual life. In addition, compared with other nanometer materials, the nanometer magnesium hydroxide has simple source and low cost, so the nanometer magnesium hydroxide can be used as a green, environment-friendly and low-cost nanometer antibacterial agent.
Disclosure of Invention
The invention aims to provide preparation and application of tea fungus disease resistant nano magnesium hydroxide.
The important component of the plant antifungal agent related by the invention is nano magnesium hydroxide. The nano magnesium hydroxide has been commercialized due to the characteristics of low cost, environmental friendliness and the like, and is mainly applied to the aspects of heavy metal removal, printing and dyeing wastewater decolorization treatment, acidic wastewater treatment, wastewater dephosphorization, deamination, flue gas desulfurization and the like. Currently commercially available magnesium hydroxide is mainly used in slurry, cake and powder forms. Currently, research on magnesium hydroxide mainly focuses on how to expand the application of magnesium hydroxide in wastewater, waste gas, flame retardants and the like, and how to combine magnesium hydroxide with other materials to improve the adsorption treatment capacity of magnesium hydroxide, little attention is paid to the antibacterial property of magnesium hydroxide, and especially, the antifungal capacity is not reported.
The invention relates to a preparation method of nano magnesium hydroxide, which is characterized by comprising the following preparation steps:
(1) preparing a magnesium chloride hexahydrate solution: mixing the raw materials according to the mass part, taking 6-8 parts of magnesium chloride hexahydrate, and adding 10 parts of ddH2O, preparing a magnesium chloride hexahydrate solution;
(2) preparing a sodium hydroxide solution: taking 2-3 parts of sodium hydroxide, adding 10 parts of ddH2O, stirring and dissolving to prepare a sodium hydroxide solution;
(3) stirring: putting the magnesium chloride hexahydrate solution obtained in the step (1) into a magnetic stirrer for stirring at 160 r/min, dripping the sodium hydroxide solution obtained in the step (2) into the magnesium chloride hexahydrate solution by using a dropper while stirring, and continuously stirring overnight;
(4) preparing nano magnesium hydroxide: and (4) centrifuging the magnesium chloride hexahydrate solution stirred in the step (3) for 5-6 min at 10000 r/min, and taking the precipitate. By ddH2Washing with O for 3 times, centrifuging at 10000 r/min for 5-6 min each time, collecting precipitate, oven drying at 60 deg.C, and grinding into fine powder in mortar to obtain nanometer magnesium hydroxide.
Preferably, the nano magnesium hydroxide has the particle size of 10-20 nm, the Zeta potential of +15.2 mV, and the concentration of 5-50 mg/mL after being dispersed in water. Experiments show that the physical nano magnesium hydroxide has obvious killing effect on tea pathogenic bacteria.
The invention has the advantages and benefits that:
1. the nano magnesium hydroxide has good antibacterial effect on the tea fungus diseases, the concentration and the inhibition rate are in positive correlation, and the inhibition rate is higher when the concentration is higher.
2. The nano magnesium hydroxide provided by the invention is convenient to obtain materials, low in price, green and environment-friendly, and has the characteristics of simple preparation method, high prevention and treatment efficiency and high social and economic benefits.
3. The application of the magnesium hydroxide in the field of antifungal agents is expanded, and theoretical basis and technical support are provided for applying the nano magnesium hydroxide to prevention and treatment of tea pathogenic bacteria in the future.
Drawings
FIG. 1 shows nano Mg (OH)2X-ray powder diffraction analysis and scanning electron microscope imaging;
FIG. 2 is a plate diagram of the bacterial black spot after being respectively acted with nano-magnesium hydroxide with different concentrations for 3-7 days.
Detailed Description
In order to further illustrate the invention, but not to limit it, reference is made to the following examples. The experimental procedures described in the following examples are conventional unless otherwise specified.
Example 1: a preparation method of nano magnesium hydroxide comprises the following steps:
the nanometer magnesium hydroxide is synthesized by utilizing the action of magnesium chloride hexahydrate and sodium hydroxide to generate precipitate. 7g of magnesium chloride hexahydrate are weighed out and 10ml of ddH are added2O is stirred and dissolved; 2.76g of sodium hydroxide are weighed into 10ml of ddH2O and stirring to dissolve. Putting the magnesium chloride hexahydrate solution into a magnetic stirrer, stirring at 160 r/min, dripping the sodium hydroxide solution into the magnesium chloride hexahydrate solution by using a dropper while stirring, and continuously stirring overnight; centrifuging at 10000 r/min for 5-6 min, and collecting precipitate. By ddH2Washing with O for 3 times, centrifuging at 10000 r/min for 5-6 min each time, collecting precipitate, oven drying at 60 deg.C, grinding into fine powder in mortar, and storing in a drier.
The size of the nano magnesium hydroxide is calculated by adopting X-ray powder diffraction, and the appearance of the nano magnesium hydroxide is observed by utilizing SEM. As shown in fig. 1, the magnesium hydroxide synthesized by the co-precipitation method completely coincides with the characteristic peak of the standard database card (JCPDF 044-1482), and the size of the nano magnesium hydroxide on the (101) surface is 14.5nm (fig. 1 a) according to the scherrer equation, and the synthesized nano magnesium hydroxide has a regular sheet structure and an agglomeration behavior (fig. 1 b).
Example 2 antibacterial experiment of Nano magnesium hydroxide on pathogenic bacteria of tea blackboard
The antifungal experiment was performed by a plate coating method. 0.005g, 0.025g and 0.05g of nano-magnesium hydroxide are weighed and added into 1ml of ddH2O, performing ultrasonic treatment for 40min by using an ultrasonic cleaning instrument to prepare 5mg/ml, 25mg/ml and 50mg/ml nano magnesium hydroxide aqueous solution; after the PDA culture medium is solidified, 100 microliter of nano magnesium hydroxide solution with different concentrations is respectively injected into the center of the culture medium, the nano magnesium hydroxide solution is uniformly coated by a coating rod, and fungi are grafted on the middle part of the flat plate after the nano magnesium hydroxide solution is dried in the air. The experiment was repeated with PDA plates without any substance as blank control, pH =11 sodium hydroxide positive control and nano magnesium hydroxide aqueous solution of each concentration as experimental group. And (3) placing the culture dish in a thermostat with the temperature of 26 ℃ in an inverted mode, continuously culturing for 3-7 days, measuring the diameter of the fungus by using a cross method, and observing the growth condition of the fungus. Further, according to formula I = [ (C-E)/C]And calculating the inhibition rate of 100%, wherein I is the inhibition rate (%) of the nano magnesium hydroxide on alternaria alternata, and C and E are the diameter (cm) of a blank group colony and the diameter (cm) of an experimental group colony respectively. Record data and calculate EC50。
Uniformly coating 5mg/ml, 25mg/ml and 50mg/ml nano magnesium hydroxide aqueous solution on a PDA culture medium, and inoculating the alternaria alternata in the middle of the culture medium. The observation shows that the nano magnesium hydroxide has higher inhibiting effect on the growth of the alternaria alternata, compared with a blank group, the growth diameter of the alternaria alternata grown on a PDA (personal digital assistant) plate containing the nano magnesium hydroxide is obviously reduced, and the growth diameter of the alternaria alternata is reduced along with the increase of the concentration of the nano magnesium hydroxide, so that the close contact degree of a bacterial colony and a culture medium is reduced, and a transparent ring appears (figure 2).
Calculated, the inhibition rate of 5mg/ml nano magnesium hydroxide on hypha growth can reach 48.78% at 3 days, the inhibition rate of 50mg/ml nano magnesium hydroxide on hypha is 100% (table 1), and EC is50It was 7.63 mg/ml. In addition, since the nano magnesium hydroxide is alkaline, in order to further verify whether the alkalinity has an effect on the growth inhibition of alternaria alternata, alkaline conditions (sodium hydroxide solution with pH = 11) are set as positive controls, and the plate is coated and then inoculated with fungi. The result shows that the growth difference of the alternaria alternata under the alkaline condition and the blank control is small, which indicates that the alkalinity is applied to the alternaria alternataThe growth of the germs has no obvious influence, and the nano magnesium hydroxide has strong inhibition effect on the bacterial alternaria alternata.
TABLE 1 different concentrations of NanoMg (OH)2Bacteriostasis rate to black spot pathogenic bacteria
Claims (3)
1. A preparation method of nano magnesium hydroxide is characterized by comprising the following preparation steps:
(1) preparing a magnesium chloride hexahydrate solution: mixing according to the mass portion, taking 6-8 portions of magnesium chloride hexahydrate, adding 10 portions of ddH2O, preparing a magnesium chloride hexahydrate solution;
(2) preparing a sodium hydroxide solution: taking 2-3 parts of sodium hydroxide, adding 10 parts of ddH2O, stirring and dissolving to prepare a sodium hydroxide solution;
(3) stirring: putting the magnesium chloride hexahydrate solution obtained in the step (1) into a magnetic stirrer for stirring at 160 r/min, dripping the sodium hydroxide solution obtained in the step (2) into the magnesium chloride hexahydrate solution by using a dropper while stirring, and continuously stirring overnight;
(4) preparing nano magnesium hydroxide: centrifuging the magnesium chloride hexahydrate solution stirred in the step (3) for 5-6 min at 10000 r/min, taking the precipitate, and adding ddH2Washing with O for 3 times, centrifuging at 10000 r/min for 5-6 min each time, collecting precipitate, oven drying at 60 deg.C, and grinding into fine powder in mortar to obtain nanometer magnesium hydroxide; the particle size of the nano magnesium hydroxide is 10-20 nm, and the nano magnesium hydroxide is in a regular sheet structure.
2. The method for preparing nano magnesium hydroxide according to claim 1, wherein the Zeta potential of the nano magnesium hydroxide in the step (4) is +15.2 mV.
3. The method for preparing nano magnesium hydroxide according to claim 1, wherein the nano magnesium hydroxide in the step (4) is dispersed in water at a concentration of 5-50 mg/mL.
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| WO2004065300A1 (en) * | 2003-01-21 | 2004-08-05 | Yazaki Corporation | Magnesium hydroxide, magnesium hydroxide/silica composite particle, processes for producing these, method of surface treatment of these, and resin composition and electric wire containing or produced with these |
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| CN107114405A (en) * | 2017-05-05 | 2017-09-01 | 华东师范大学第附属中学 | Nano Silver/hydroxide nanoparticle assembling ball compound disinfectant and preparation method thereof |
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Patent Citations (12)
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| US2576731A (en) * | 1948-11-19 | 1951-11-27 | Alfred M Thomsen | Method of preparing a fungicidal preparation utilizing magnesium hydroxide |
| WO1989010071A1 (en) * | 1988-04-20 | 1989-11-02 | P.H. Glatfelter Company | Cigarette wrappers containing freshly precipitated magnesium hydroxide |
| CN1359853A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | Acidular or flaky nano magnesium hydroxide and its preparing process |
| WO2004065300A1 (en) * | 2003-01-21 | 2004-08-05 | Yazaki Corporation | Magnesium hydroxide, magnesium hydroxide/silica composite particle, processes for producing these, method of surface treatment of these, and resin composition and electric wire containing or produced with these |
| CN101219801A (en) * | 2007-01-11 | 2008-07-16 | 天津城市建设学院 | Process for producing nano-flame-proof magnesium hydroxide |
| CN101234769A (en) * | 2008-03-04 | 2008-08-06 | 贵州大学 | Technique for preparing high purity ultra-fine magnesium hydroxide by sodium hydroxide method |
| CN102101684A (en) * | 2009-12-16 | 2011-06-22 | 中国科学院过程工程研究所 | Method for preparing submicron lamellar magnesium hydroxide by intensifying alkali |
| CN103508474A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院大连化学物理研究所 | Method for preparing magnesium hydroxide flame retardant by microchannel precipitation-hydrothermal process |
| CN103193254A (en) * | 2013-03-12 | 2013-07-10 | 广西大学 | Novel technology for simultaneously preparing rodlike and sheetlike nano-sized magnesium hydroxide |
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| CN107114405A (en) * | 2017-05-05 | 2017-09-01 | 华东师范大学第附属中学 | Nano Silver/hydroxide nanoparticle assembling ball compound disinfectant and preparation method thereof |
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