CN115989816A - Hymexazol intercalated hydrotalcite nano bactericide and preparation method and application thereof - Google Patents
Hymexazol intercalated hydrotalcite nano bactericide and preparation method and application thereof Download PDFInfo
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- CN115989816A CN115989816A CN202310107544.7A CN202310107544A CN115989816A CN 115989816 A CN115989816 A CN 115989816A CN 202310107544 A CN202310107544 A CN 202310107544A CN 115989816 A CN115989816 A CN 115989816A
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- hymexazol
- bactericide
- hydrotalcite nano
- intercalated
- hydrotalcite
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- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 122
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 119
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 119
- 239000005794 Hymexazol Substances 0.000 title claims abstract description 116
- KGVPNLBXJKTABS-UHFFFAOYSA-N hymexazol Chemical compound CC1=CC(O)=NO1 KGVPNLBXJKTABS-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 239000003899 bactericide agent Substances 0.000 title claims abstract description 88
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 201000010099 disease Diseases 0.000 claims abstract description 29
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 claims abstract description 29
- 239000002689 soil Substances 0.000 claims abstract description 27
- 239000002135 nanosheet Substances 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims description 48
- 229910052751 metal Inorganic materials 0.000 claims description 34
- 239000002184 metal Substances 0.000 claims description 34
- 150000003839 salts Chemical class 0.000 claims description 22
- 239000012266 salt solution Substances 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 13
- 238000009830 intercalation Methods 0.000 claims description 12
- 230000002687 intercalation Effects 0.000 claims description 12
- -1 sulfate radical Chemical class 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
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- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
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- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 3
- 159000000007 calcium salts Chemical class 0.000 claims description 3
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- 159000000003 magnesium salts Chemical class 0.000 claims description 3
- 150000005837 radical ions Chemical class 0.000 claims description 3
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- 150000003751 zinc Chemical class 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 23
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- 239000003337 fertilizer Substances 0.000 abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 4
- 238000002386 leaching Methods 0.000 abstract description 4
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- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 230000006806 disease prevention Effects 0.000 abstract description 2
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- 239000008187 granular material Substances 0.000 description 18
- UHPMCKVQTMMPCG-UHFFFAOYSA-N 5,8-dihydroxy-2-methoxy-6-methyl-7-(2-oxopropyl)naphthalene-1,4-dione Chemical compound CC1=C(CC(C)=O)C(O)=C2C(=O)C(OC)=CC(=O)C2=C1O UHPMCKVQTMMPCG-UHFFFAOYSA-N 0.000 description 13
- 244000068988 Glycine max Species 0.000 description 13
- 235000010469 Glycine max Nutrition 0.000 description 13
- 241000223218 Fusarium Species 0.000 description 12
- 208000015181 infectious disease Diseases 0.000 description 12
- 239000002552 dosage form Substances 0.000 description 8
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- 238000012360 testing method Methods 0.000 description 8
- 239000000969 carrier Substances 0.000 description 7
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- 230000035784 germination Effects 0.000 description 6
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical group [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 241000223221 Fusarium oxysporum Species 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 239000003814 drug Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
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- 238000000926 separation method Methods 0.000 description 2
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- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 240000007124 Brassica oleracea Species 0.000 description 1
- 235000003899 Brassica oleracea var acephala Nutrition 0.000 description 1
- 235000011301 Brassica oleracea var capitata Nutrition 0.000 description 1
- 235000001169 Brassica oleracea var oleracea Nutrition 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 235000002566 Capsicum Nutrition 0.000 description 1
- 240000008574 Capsicum frutescens Species 0.000 description 1
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 description 1
- 208000004770 Fusariosis Diseases 0.000 description 1
- 206010051919 Fusarium infection Diseases 0.000 description 1
- 241000243785 Meloidogyne javanica Species 0.000 description 1
- 240000008790 Musa x paradisiaca Species 0.000 description 1
- 235000018290 Musa x paradisiaca Nutrition 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 241000244206 Nematoda Species 0.000 description 1
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- 235000001231 Streptopus amplexifolius Nutrition 0.000 description 1
- 241000082085 Verticillium <Phyllachorales> Species 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 1
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 1
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- 230000001580 bacterial effect Effects 0.000 description 1
- 230000003542 behavioural effect Effects 0.000 description 1
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- 229910052791 calcium Inorganic materials 0.000 description 1
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- 229960002713 calcium chloride Drugs 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 235000011148 calcium chloride Nutrition 0.000 description 1
- LLSDKQJKOVVTOJ-UHFFFAOYSA-L calcium chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Ca+2] LLSDKQJKOVVTOJ-UHFFFAOYSA-L 0.000 description 1
- 229940052299 calcium chloride dihydrate Drugs 0.000 description 1
- 239000001390 capsicum minimum Substances 0.000 description 1
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- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
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Abstract
The invention provides a hymexazol intercalated hydrotalcite nano bactericide, a preparation method and application thereof, belonging to the technical field of pesticides and fertilizers. According to the invention, the hydrotalcite nano-sheets are used as a structural basis, the hymexazol molecules are intercalated in the hydrotalcite nano-sheet structure, the intercalated structure has good slow release performance, and the hymexazol molecules can be released into soil stably for a long time through soil application, so that degradation and leaching are inhibited, the duration is prolonged, and the soil-borne disease prevention and control effect is enhanced; the invention fully utilizes the abundant hydroxyl structures on the surfaces of hydrotalcite nano-sheets, not only can reduce the occurrence probability of soil-borne diseases caused by fungi such as crop clubroot and root rot by adjusting the pH of soil, but also can respond to the acidic environment brought by germs at the initial stage of outbreak due to the unique hydroxide structure, and can quickly release hymexazol molecules to kill the pathogens in the response form of disintegration of the whole structure.
Description
Technical Field
The invention relates to the technical field of pesticides and fertilizers, in particular to a hymexazol intercalated hydrotalcite nano bactericide, a preparation method and application thereof.
Background
Soil-borne diseases refer to damping-off, epidemic disease, root rot, fusarium wilt, verticillium wilt, sclerotinia, bacterial wilt, root knot nematode and the like caused by invasion of a crop from the root or stem of the crop when the conditions are appropriate, by pathogens such as fungi, bacteria, nematodes and viruses living in the soil along with the disease residues. Particularly, soil-borne diseases using fungi as pathogens, the dormant spores of the soil-borne diseases can survive in the soil for a plurality of years, so that the control of the soil-borne diseases becomes a worldwide problem.
Soil-borne diseases clubroot, represented by clubroot and root rot, are widely present. An outbreak of clubroot will lead to a serious decrease in cruciferous crop yield, while an outbreak of root rot will lead to a substantial decrease in banana yield, even in absolute harvest. The occurrence of soil-borne diseases with fungi as pathogens can be divided into two stages, namely germination of dormant spores in rhizosphere and infection of root hairs; secondly, pathogenic bacteria colonize and proliferate in the cortex of the root. In its spore morphology stage, pathogenic bacteria mainly live through winter or summer in soil with residual tissue of the disease plant as dormant spores. Dormant spores are very resistant to the environment and can survive for years, which is also a main reason that the diseases are difficult to control. It can be spread by means of rainwater, irrigation water, farm work operation or bacteria-carrying soil, disease residue and non-decomposed fertilizer, etc. to become re-infection source. In the germination stage, when the pH value of soil is 5.4-6.5, the growth and propagation of germs are facilitated, diseases are easy to induce, and when the pH value is above 7.2, the diseases are reduced. In addition, the soil and sandy soil with high and dry topography and convenient drainage generally have lighter disease, and the field with heavy soil viscosity or less organic matters and partial fertilizer application has heavier disease, and the field with more pathogenic bacteria residues of clubroot disease has the most serious disease. Therefore, the method has long lasting period, and the development of soil-borne disease control means which can regulate the pH of soil and control the soil has important practical requirements.
In recent years, with development of nano materials and technologies, the appearance of intelligent response type nano pesticides provides a new thought for preventing and controlling soil-borne diseases, wherein nano pesticides taking silicon dioxide, attapulgite and cellulose gel as carriers show good effects in the aspects of prolonging the duration and slowly controlling release, but due to the characteristics of fungal pathogen soil-borne diseases, the carriers cannot regulate and control the pH of soil environment around root systems, respond to different pH environments, and are difficult to accurately match with prevention and control requirements.
Disclosure of Invention
The invention aims to provide a hymexazol intercalated hydrotalcite nano bactericide, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a hymexazol intercalated hydrotalcite nano bactericide, which comprises hydrotalcite nano sheets and hymexazol molecules intercalated in the hydrotalcite nano sheets.
Preferably, the mass content of the hymexazol molecule in the hydrotalcite nano-sheet is 5-60%.
Preferably, the chemical composition of the hymexazol intercalated hydrotalcite nano bactericide is (M 1 ) x (M 2 ) 1-x (OH) 2 A y (C 4 H 5 NO 2 ) m ·zH 2 O；
Wherein M is 1 Is Mg 2+ 、Ca 2+ And Zn 2+ One or more of the following; m is M 2 Is Fe 3+ 、Cr 3+ And Al 3+ One or more of the following; a is one or more of nitrate radical, sulfate radical and hydrochloride radical;
C 4 H 5 NO 2 is hymexazol molecule;
x＝0.2～0.8；m＝0.2～4；z＝1～20；
y is given such that (M 1 ) x (M 2 ) 1-x (OH) 2 A y (C 4 H 5 NO 2 )m·zH 2 The charge of O remains conserved.
Preferably, the particle size of the hymexazol intercalated hydrotalcite nano bactericide is 50-500 nm.
The invention provides a preparation method of hymexazol intercalated hydrotalcite nano bactericide in the technical scheme, which comprises the following steps:
and mixing the soluble metal salt solution, the hymexazol solution and the strong alkali solution, performing intercalation reaction, and separating to obtain the hymexazol intercalated hydrotalcite nano bactericide.
Preferably, the soluble metal salt in the soluble metal salt solution comprises a soluble divalent metal salt and a soluble trivalent metal salt; the soluble divalent metal salt is one or more of magnesium salt, calcium salt and zinc salt; the soluble trivalent metal salt is one or more of ferric salt, trivalent chromium salt and aluminum salt; the acid radical ion in the soluble metal salt solution is one or more of nitrate radical, sulfate radical and hydrochloride radical; the concentration of the soluble metal salt solution and the hymexazol solution is independently 0.005-0.5 mol/L; the concentration of the strong alkali solution is 0.01-1.0 mol/L.
Preferably, the intercalation reaction is carried out under shearing conditions, the shearing speed is 3000-5000 r/min, and the time is 1-3 min.
The invention provides the hymexazol intercalated hydrotalcite nano bactericide in the technical scheme or the application of the hymexazol intercalated hydrotalcite nano bactericide prepared by the preparation method in the technical scheme in the control of crop soil-borne diseases.
Preferably, the hymexazol intercalated hydrotalcite nano bactericide is used in the form of hydrotalcite nano bactericide aqueous dispersion or hydrotalcite nano bactericide solid.
Preferably, the hydrotalcite nano bactericide aqueous dispersion is applied to the surface of a crop leaf; the concentration of the hydrotalcite nano bactericide aqueous dispersion liquid is 0.1-2 g/L; the application amount of the hydrotalcite nano bactericide aqueous dispersion is 5-20 g/mu;
the hydrotalcite nano bactericide solid is applied to soil around the root of crops; the application amount of the hydrotalcite nano bactericide solid is 5-20 g/mu.
The invention provides a hymexazol intercalated hydrotalcite nano bactericide, which comprises hydrotalcite nano sheets and hymexazol molecules intercalated in the hydrotalcite nano sheets. The hymexazol molecule has good sterilization performance and plant growth regulation effect, can effectively inhibit various soil-borne diseases represented by root rot and clubroot, and promote plant growth through metabolites thereof in plants so as to achieve the purpose of soil-borne disease control; hydrotalcite is a Layered Double Hydroxide (LDH) having a two-dimensional layered structure consisting of platelets and intercalated molecules between layers and polyhydroxy character. According to the invention, the hydrotalcite nano-sheets are used as a structural basis, the hymexazol molecules are intercalated into the hydrotalcite nano-sheet structures through hydrogen bonding, the intercalated structures have good slow release performance, and the hymexazol molecules can be released into soil stably for a long time through soil application, so that degradation and leaching are inhibited, the duration is prolonged, and the soil-borne disease prevention and control effect is enhanced; the invention fully utilizes the abundant hydroxyl structures on the surfaces of hydrotalcite nano-sheets, not only can reduce the occurrence probability of soil-borne diseases caused by fungi such as crop clubroot and root rot by adjusting the pH of soil, but also can respond to the acidic environment brought by germs at the initial stage of outbreak due to the unique hydroxide structure, and can quickly release hymexazol molecules to kill the pathogens in the response form of disintegration of the whole structure.
Furthermore, the invention achieves the multi-effect synergistic soil-borne disease control effect with pH response through the control of the hymexazol intercalation structure and the intercalation proportion.
Drawings
FIG. 1 is an XRD pattern of Hymexazol intercalated hydrotalcite nano bactericide, LDH and commercially available Hymexazol obtained in example 1;
FIG. 2 is an infrared absorption spectrum of the Hymexazol intercalated hydrotalcite nano bactericide, LDH and commercially available Hymexazol obtained in example 1;
FIG. 3 is a scanning electron microscope image of the hymexazol intercalated hydrotalcite nano bactericide obtained in example 1;
FIG. 4 shows the slow release effect of the hymexazol intercalated hydrotalcite nano bactericide and the conventional Granule (GR) obtained in example 1;
FIG. 5 shows the pH responsive release effect of the hymexazol intercalated hydrotalcite nano bactericide obtained in example 1;
FIG. 6 shows the experimental effect of the hymexazol intercalated hydrotalcite nano-bactericide obtained in example 1 and Fusarium inhibition zones of different samples;
FIG. 7 is a graph showing experiments on potted cucumber of the hymexazol intercalated hydrotalcite nano bactericide obtained in example 1 and different samples;
FIG. 8 is a graph showing soybean seed germination experiments of the hymexazol intercalated hydrotalcite nano bactericide obtained in example 2 and different samples.
Detailed Description
The invention provides a hymexazol intercalated hydrotalcite nano bactericide, which comprises hydrotalcite nano sheets and hymexazol molecules intercalated in the hydrotalcite nano sheets.
In the present invention, the mass content of the hymexazol molecule in the hydrotalcite nanosheets is preferably 5 to 60%, more preferably 5 to 30%, and still more preferably 5.1 to 7.16%.
In the invention, the chemical composition of the hymexazol intercalated hydrotalcite nano bactericide is preferably (M) 1 ) x (M 2 ) 1-x (OH) 2 A y (C 4 H 5 NO 2 ) m ·zH 2 O；
Wherein M is 1 Is Mg 2+ 、Ca 2+ And Zn 2+ One or more of the following; m is M 2 Is Fe 3+ 、Cr 3+ And Al 3+ One or more of the following; a is one or more of nitrate radical, sulfate radical and hydrochloride radical;
C 4 H 5 NO 2 is hymexazol molecule;
x＝0.2～0.8；m＝0.2～4；z＝1～20；
y is given such that (M 1 ) x (M 2 ) 1-x (OH) 2 A y (C 4 H 5 NO 2 )m·zH 2 The charge of O remains conserved.
In the present invention, when M is 1 、M 2 When A is more than two of the above, the invention has no special limitation on the proportion of the corresponding reagents of different types, and the invention can be adjusted according to actual requirements.
In the present invention, x is preferably 0.66 to 0.75; m is preferably 0.3 to 0.5; z is preferably 3 to 15, more preferably 7 to 10. As a specific embodiment of the invention, the chemical composition of the hymexazol intercalated hydrotalcite nano bactericide is Mg 0.67 Al 0.33 (OH) 2 (NO 3 ) 0.33 (C 4 H 5 NO 2 ) 0.16 ·7H 2 O or Ca 0.75 Al 0.25 (OH) 2 (Cl) 0.25 (C 4 H 5 NO 2 ) 0.13 ·10H 2 O。
In the invention, the particle size of the hymexazol intercalated hydrotalcite nano bactericide is preferably 50-500 nm.
The invention provides a preparation method of hymexazol intercalated hydrotalcite nano bactericide in the technical scheme, which comprises the following steps:
and mixing the soluble metal salt solution, the hymexazol solution and the strong alkali solution, performing intercalation reaction, and separating to obtain the hymexazol intercalated hydrotalcite nano bactericide.
In the present invention, the preparation materials are commercially available as known to those skilled in the art unless otherwise specified.
In the present invention, the soluble metal salt in the soluble metal salt solution preferably includes a soluble divalent metal salt and a soluble trivalent metal salt. In the invention, the molar ratio of the soluble divalent metal salt to the soluble trivalent metal salt is preferably 1-4:1, more preferably 2-3:1, and the chemical composition of the hymexazol intercalated hydrotalcite nano bactericide is satisfied.
In the present invention, the soluble divalent metal salt is preferably one or more of magnesium salt, calcium salt and zinc salt; the soluble trivalent metal salt is preferably one or more of trivalent ferric salt, trivalent chromium salt and aluminum salt; the acid radical ion in the soluble metal salt solution is preferably one or more of nitrate radical, sulfate radical and hydrochloride radical.
In the present invention, the soluble divalent metal salt is preferably one or more of magnesium nitrate, calcium chloride, zinc chloride, magnesium sulfate and zinc acetate; the soluble trivalent metal salt is preferably aluminum nitrate.
In the present invention, the concentration of the soluble metal salt solution and the hymexazol solution is independently preferably 0.005 to 0.5mol/L, more preferably 0.05 to 0.3mol/L, and further preferably 0.1 to 0.2mol/L.
In the invention, the dosage of the hymexazol solution preferably meets the chemical composition of the hymexazol intercalated hydrotalcite nano bactericide.
In the present invention, the strong alkali solution is preferably NaOH solution; the concentration of the strong alkali solution is preferably 0.01 to 1.0mol/L, more preferably 0.05 to 0.8mol/L, and still more preferably 0.1 to 0.6mol/L.
The soluble metal salt solution, the hymexazol solution and the strong alkali solution are all water solutions.
In the present invention, the process of mixing the soluble metal salt solution, the hymexazol solution and the alkali solution is preferably to mix the soluble metal salt solution and the hymexazol solution in a colloid mill and then mix them with the alkali solution.
In the present invention, the intercalation is preferably carried out under shearing conditions, and the shearing rate is preferably 3000 to 5000r/min, more preferably 3500 to 4500r/min, still more preferably 4000 to 4500r/min, and the time is preferably 1 to 3min, still more preferably 2 to 3min. In the shearing process, coprecipitation intercalation reaction occurs among the three solutions, and the growth process is controlled through high-speed shearing, so that the nano-size of the three solutions is achieved.
After the intercalation reaction is completed, the obtained product is preferably subjected to solid-liquid separation, and the solid-liquid separation mode is preferably centrifugation; the rate of the centrifugation is preferably 3000 to 8000rpm, more preferably 4000 to 6000rpm, still more preferably 8000rpm, and the time is preferably 5 to 10 minutes.
After the centrifugation is completed, the present invention preferably disperses the resulting solid in water and repeats the centrifugation until the centrifuged liquid is neutral. When solids are desired, the present invention preferably dries the resulting centrifuged liquid to a solid powder.
The invention preferably stores the hymexazol intercalated hydrotalcite nano bactericide in the form of nano solution or solid powder according to the requirement.
The invention provides the hymexazol intercalated hydrotalcite nano bactericide in the technical scheme or the application of the hymexazol intercalated hydrotalcite nano bactericide prepared by the preparation method in the technical scheme in the control of crop soil-borne diseases.
In the present invention, the crop is preferably one or more of cucumber, cabbage, capsicum and soybean.
In the invention, the hymexazol intercalated hydrotalcite nano bactericide is preferably used in the form of hydrotalcite nano bactericide aqueous dispersion or hydrotalcite nano bactericide solid.
In the invention, the hydrotalcite nano bactericide aqueous dispersion is preferably applied to the surface of a crop leaf; the concentration of the hydrotalcite nano bactericide aqueous dispersion is preferably 0.1-2 g/L, more preferably 0.5-1.5 g/L; the application amount of the hydrotalcite nano bactericide aqueous dispersion is preferably 5-20 g/mu, more preferably 10-15 g/mu;
in the invention, the hydrotalcite nano bactericide solid is preferably applied to soil around the root of crops; the application amount of the hydrotalcite nano bactericide solid is preferably 5-20 g/mu, more preferably 10-15 g/mu.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) 25.6g of magnesium nitrate, 18.75g of aluminum nitrate and 24.75g of hymexazol (molar ratio Mg: al: C) were weighed out 4 H 5 NO 2 =2:1:0.5) are respectively dissolved in 500mL deionized water to prepare solutions with the concentration of 0.2mol/L, 0.1mol/L and 0.05mol/L respectively, and then the solutions are mixed to form a mixed solution;
(2) 12g of sodium hydroxide is weighed and dissolved in 500mL of deionized water to prepare NaOH solution with the concentration of 0.6 mol/L;
(3) Rapidly mixing the mixed solution and the NaOH solution in a colloid mill, keeping the rotating speed of 3000r/min, and reacting for 2min to obtain the hymexazol intercalated hydrotalcite nanosheet solution;
(4) Centrifuging the hymexazol intercalated hydrotalcite nanosheet solution at high speed, maintaining the rotation speed of 8000r/min, centrifuging for 5min, removing supernatant, adding water for redispersion, centrifuging again, repeating centrifuging operation for 3 times, and collecting supernatant as neutral to obtain hymexazol intercalated hydrotalcite nanoscaled bactericide (Mg) 0.67 Al 0.33 (OH) 2 (NO 3 ) 0.33 (C 4 H 5 NO 2 ) 0.16 ·7H 2 The mass content of the O, hymexazol molecules in the hydrotalcite nano-sheets is 7.16 percent.
Example 2
(1) 8.82g of calcium chloride dihydrate, 4.82g of aluminum chloride hexahydrate and 0.99g of hymexazol (molar ratio Ca: al: C) 4 H 5 NO 2 =3:1:0.5) are respectively dissolved in 200mL deionized water to prepare solutions with the concentration of 0.3mol/L, 0.1mol/L and 0.05mol/L respectively, and then the solutions are mixed to form a mixed solution;
(2) 6.4g of sodium hydroxide is weighed and dissolved in 200mL of deionized water to prepare NaOH solution with the concentration of 0.8 mol/L;
(3) Rapidly mixing the mixed solution and the NaOH solution in a colloid mill, maintaining the rotation speed of 5000r/min, and reacting for 1min to obtain a hydrotalcite nanosheet solution;
(4) Centrifuging the prepared hydrotalcite nanosheet solution at high speed, maintaining the rotation speed of 8000r/min, reacting for 10min, removing supernatant, adding water for redispersion, centrifuging, and repeating the processRe-centrifuging for 3 times until the supernatant is neutral to obtain hymexazol intercalated hydrotalcite nanometer bactericide (Ca) 0.75 Al 0.25 (OH) 2 (Cl) 0.25 (C 4 H 5 NO 2 ) 0.13 ·10H 2 The mass content of the O, hymexazol molecules in the hydrotalcite nano-sheets is 5.1 percent.
Comparative example 1
Weighing 25.6g of magnesium nitrate and 18.75g of aluminum nitrate, respectively dissolving in 500mL of deionized water, and preparing into solutions with the concentration of 0.2mol/L and 0.1mol/L respectively, and mixing to obtain a mixed solution;
(2) 12g of sodium hydroxide is weighed and dissolved in 500mL of deionized water to prepare NaOH solution with the concentration of 0.6 mol/L;
(3) Rapidly mixing the mixed solution and the NaOH solution in a colloid mill, keeping the rotating speed of 3000r/min, and reacting for 2min to obtain a hydrotalcite nano-sheet solution;
(4) And (3) carrying out high-speed centrifugation on the hydrotalcite nanosheet solution, keeping the rotating speed at 8000r/min, centrifuging for 5min, removing supernatant, adding water for redispersion, continuing centrifuging, repeating the centrifuging operation for 3 times, and obtaining a hydrotalcite carrier which is marked as LDH (layered double hydroxide). According to the experimental requirements, the powder is stored in a solution form or dried in a powder state.
Characterization and performance testing
1) X-ray diffraction analysis was performed on the Hymexazol intercalated hydrotalcite nano bactericide (hereinafter referred to as H-LDH) obtained in example 1, and compared with hydrotalcite carriers (hereinafter referred to as LDH) and commercial Hymexazol (Hymexazol), and the obtained XRD patterns were shown in FIG. 1, (a) as H-LDH, (b) as LDH, and (c) as Hymexazol; the result shows that the H-LDH structure has complete crystal form, ideal crystallinity and high purity, and the effect on the interlayer spacing is not obvious due to smaller molecular size of hymexazol, so that the (003) diffraction peak of the structure slightly moves, and on the basis, the intercalation structure presents the superposition of the main diffraction peaks of two structural units of the hydrotalcite carrier and the hymexazol molecule, thereby realizing the effective intercalation of the hymexazol molecule.
2) Infrared spectrum test was performed on the Hymexazol intercalated hydrotalcite nano fungicide obtained in example 1, and compared with LDH and hypxazol,the results obtained are shown in FIG. 2, (a) is LDH, (b) is H-LDH, and (c) is Hymexazol; wherein 3450cm -1 The characteristic absorption peak of hydroxyl group at wavenumber is widened by the hydrogen bond of hydroxyl group between hymexazol molecule and hydrotalcite carrier. 1630 and 1380cm -1 The characteristic peak at wave number is ascribed to the absorption peak of heterocyclic structure in hymexazol molecule, 1350cm -1 The absorption peak at the wave number is attributed to the nitrate structure in the hydrotalcite structure, and the result shows that the hymexazol intercalated hydrotalcite structure has main functional groups of two structural units, and after a composite structure is formed by taking hydrogen bonds as acting forces, the structural stability of each functional group is effectively maintained, and the guarantee is provided for the physiological function of the hymexazol intercalated hydrotalcite structure.
3) The oxazamate intercalated hydrotalcite nano bactericide obtained in example 1 is subjected to scanning electron microscope test, and the obtained result is shown in figure 3, wherein the oxazamate intercalated hydrotalcite nano bactericide has a regular hexagonal plate structure, uniform particle size distribution and an average particle size of 50nm.
4) The slow release evaluation of the hymexazol intercalated hydrotalcite nano bactericide obtained in the example 1 is carried out and compared with GR, and the result is shown in the figure 4, wherein (a) is H-LDH, (b) the traditional hymexazol granule formulation (GR for short) is sold in the market; for the traditional Granule (GR), the hymexazol molecules are rapidly released due to good water solubility (85 g/L), the accumulated release proportion reaches a level of about 80.47%, and for the nano dosage form H-LDH, the accumulated release proportion is stabilized at a level of about 50.48% due to the existence of LDH carrier and supermolecule acting force, so that the free movement and release of the hymexazol molecules are effectively inhibited, and the potential of the hymexazol molecules in a soil environment along with water leaching is improved.
5) Because the LDH carrier has a unique hydroxide structure, the LDH carrier can respond to the acidic environment brought by the pathogen in the early stage of the outbreak of the pathogen, and the hymexazol molecule can be rapidly released through the response form of the disintegration of the whole structure. The pH response release behavior of the hymexazol intercalated hydrotalcite nano-bactericide obtained in example 1 was evaluated. The release behavior under different pH environments is simulated by using a soil column experiment, and the release behavior is specifically as follows: sequentially drying, grinding and sieving soil, and filling the soil into a polyvinyl chloride column. The nano-preparation obtained in example 1 was spread on the surface of soil and covered with 1cm thick quartz sand. The column was separately leached with leaching solutions having different pH, and the leacheate was collected under the column and tested for the concentration of hymexazol per 10mL of leacheate. The results are shown in fig. 5, where (a) is ph=5.0, (b) is ph=6.5, and (c) is ph=8.0; by simulation of three different pH leaches, the cumulative release rate of hymexazol molecules reached about 90.41% rapidly at ph=5.0 and 76.30% and 52.06% at ph=6.5 and ph=8.0, respectively. The difference is that the hydrotalcite nano-sheet structure can be subjected to carrier etching dissolution under the condition of acidity regulation, so that the quick release of hymexazol molecules is achieved. In the outbreak period of fusarium, the metabolite of fusarium can cause local pH reduction, so that hymexazol molecules are released rapidly and massively, and the aim of effective control is achieved.
6) The effect of controlling fusarium of the hymexazol intercalated hydrotalcite nano bactericide obtained in the example 1 and different samples is evaluated by using a bacteriostasis zone experiment. In a culture dish with the diameter of 10cm, pouring potato culture mediums mixed with different medicines, inoculating fusarium and culturing for 7 days, and evaluating the antibacterial effect of each sample through measuring the radius of a bacteriostasis ring. The results are shown in FIG. 6, wherein A is a blank without any added sample, B is a commercial hymexazol Granule (GR) sample, C is a hydrotalcite carrier sample, and D is a nano bactericide sample obtained in example 1; as can be seen from FIG. 6, for the conventional hymexazol Granule (GR), the inhibition zone has a diameter of about 4.48cm, and can inhibit the growth of Fusarium. For hydrotalcite carriers without bactericides, the pH environment of the culture medium can be influenced, so that the hydrotalcite carriers are kept at an alkaline level, are unfavorable for the growth of fusarium, and can achieve the antibacterial effect to a certain extent, so that the diameter of an antibacterial circle is about 6.02cm. For the H-LDH nano dosage form, the H-LDH nano dosage form has synergistic effects of slow release, pH adjustment and the like, so that the H-LDH nano dosage form shows the best antibacterial effect, and the diameter of an antibacterial ring is only 2.24cm.
The test results of XRD, scanning electron microscope, transmission electron microscope, pH response release behavior and antibacterial effect of the hymexazol intercalated hydrotalcite nano bactericide obtained in example 2 are similar to those of example 1.
Test example 1
Cucumber is used as experimental crop, and the flowerpot size is 10cm×10cm. The effect of the nano-bactericide prepared in example 1 was evaluated and compared with various samples. The testing method comprises the following steps: fusarium oxysporum serving as a root rot disease source is taken as a control object, hymexazol intercalated hydrotalcite nano bactericide is prepared into aqueous dispersion with the concentration of 1.0g/L, after cucumber seedlings are transplanted, a culture medium solution containing Fusarium is used for irrigating the cucumber, meanwhile, the nano bactericide is utilized to irrigate roots every 3 days, the application amount of the nano bactericide is 20 mL/basin each time, and the infection proportion (20 strains per group) of the nano bactericide and other three treatment groups is counted on the 15 th day after application. The results are shown in Table 1 and FIG. 7.
In FIG. 7, A is the effect graph of the hymexazol intercalated hydrotalcite nano bactericide of example 1, B is the effect graph of the commercial hymexazol granule, C is the effect graph of the hydrotalcite carrier, and D is the effect graph of the blank group (without using any medicament).
TABLE 1 cucumber root rot control results for different samples
| Number of infections/strain | Infection ratio/% | |
| Blank control group | 14 | 70 |
| Example 1 | 2 | 10 |
| Commercially available granule | 5 | 25 |
| Hydrotalcite support | 13 | 65 |
As can be seen from table 1, the use of the nano dosage form effectively inhibits the infection of fusarium on soybeans, and ensures that the cucumber has good growth effect in the soil in the presence of fusarium; the commercially available granules can also prevent and treat fusarium infection to a certain extent, but the prevention and treatment effect is reduced along with the time extension, and plants begin to wilt; for hydrotalcite carriers and blank control groups, the growth and infection of fungi cannot be inhibited, plants are seriously wilted, and the growth state is obviously inferior to that of a treatment group to which the nanometer dosage form is applied.
Test example 2
The effect of the nano-bactericide prepared in example 2 was evaluated using soybean as an experimental crop, and compared with different samples. The testing method comprises the following steps: the method comprises the steps of taking fusarium oxysporum as a disease source of root rot as a control object, soaking soybeans in a flowerpot for 12 hours, placing 20g of soil in the flowerpot with the size of 10cm multiplied by 10cm, and watering with a culture medium solution containing fusarium. The hymexazol intercalated hydrotalcite nano bactericide solid powder was applied around soybeans at a ratio of 1.0 g/pot, and after 7 days, seed germination ratio and infection ratio (20 grains per group) of the soil-applied nano bactericide and the control group without the nano bactericide were counted. The results are shown in Table 2 and FIG. 8.
In FIG. 8, A is the effect diagram of the nano-bactericide of example 2, B is the effect diagram of the commercially available hymexazol granules, C is the effect diagram of the hydrotalcite carrier, and D is the effect diagram of the blank group.
TABLE 2 prevention and treatment results of soybean root rot of different samples
| Germination count/grain | Germination proportion/% | Number of infections/granule | Infection ratio/% | |
| Blank control group | 7 | 35 | 13 | 65 |
| Example 2 | 19 | 95 | 1 | 5 |
| Commercially available granule | 17 | 85 | 3 | 15 |
| |
10 | 50 | 10 | 50 |
As can be seen from table 2, the use of the nano dosage form obtained in example 2 effectively inhibits infection of fusarium on soybeans, and greatly improves soybean germination proportion; commercial granules can also effectively prevent and control pathogen infection, but have inferior effects compared with the nano dosage form of the example 2, so that soybean germination state is poor; in hydrotalcite carriers and blank control groups, most soybeans are infected and wilted due to pathogen infection, so that the soybeans are difficult to germinate normally, and the growth of the soybeans is seriously influenced.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The hymexazol intercalated hydrotalcite nanometer bactericide comprises hydrotalcite nanometer sheets and hymexazol molecules intercalated in the hydrotalcite nanometer sheets.
2. The hymexazol intercalated hydrotalcite nano bactericide according to claim 1, wherein the mass content of the hymexazol molecules in the hydrotalcite nano sheet is 5 to 60%.
3. The hymexazol intercalated hydrotalcite nano bactericide according to claim 1, wherein the chemical composition of the hymexazol intercalated hydrotalcite nano bactericide is (M) 1 ) x (M 2 ) 1-x (OH) 2 A y (C 4 H 5 NO 2 ) m ·zH 2 O；
Wherein M is 1 Is Mg 2+ 、Ca 2+ And Zn 2+ One or more of the following; m is M 2 Is Fe 3+ 、Cr 3+ And Al 3+ One or more of the following; a is one or more of nitrate radical, sulfate radical and hydrochloride radical;
C 4 H 5 NO 2 is hymexazol molecule;
x＝0.2～0.8；m＝0.2～4；z＝1～20；
y is given such that (M 1 ) x (M 2 ) 1-x (OH) 2 A y (C 4 H 5 NO 2 )m·zH 2 The charge of O remains conserved.
4. The hymexazol intercalated hydrotalcite nano bactericide according to any one of claims 1 to 3, wherein the particle size of the hymexazol intercalated hydrotalcite nano bactericide is 50 to 500nm.
5. The method for preparing the hymexazol intercalated hydrotalcite nano bactericide according to any one of claims 1 to 4, comprising the following steps:
and mixing the soluble metal salt solution, the hymexazol solution and the strong alkali solution, performing intercalation reaction, and separating to obtain the hymexazol intercalated hydrotalcite nano bactericide.
6. The method of claim 5, wherein the soluble metal salts in the soluble metal salt solution comprise soluble divalent metal salts and soluble trivalent metal salts; the soluble divalent metal salt is one or more of magnesium salt, calcium salt and zinc salt; the soluble trivalent metal salt is one or more of ferric salt, trivalent chromium salt and aluminum salt; the acid radical ion in the soluble metal salt solution is one or more of nitrate radical, sulfate radical and hydrochloride radical; the concentration of the soluble metal salt solution and the hymexazol solution is independently 0.005-0.5 mol/L; the concentration of the strong alkali solution is 0.01-1.0 mol/L.
7. The method according to claim 5, wherein the intercalation is carried out under shearing conditions, the shearing rate being 3000-5000 r/min, the time being 1-3 min.
8. The use of the hymexazol intercalated hydrotalcite nano bactericide according to any one of claims 1 to 4 or the hymexazol intercalated hydrotalcite nano bactericide prepared by the preparation method according to any one of claims 5 to 7 in the prevention and treatment of soil-borne diseases of crops.
9. The use according to claim 8, wherein the hymexazol intercalated hydrotalcite nano-bactericide is used in the form of an aqueous hydrotalcite nano-bactericide dispersion or a hydrotalcite nano-bactericide solid.
10. The use according to claim 9, wherein the aqueous hydrotalcite nano-bactericide dispersion is applied to the surface of the crop leaves; the concentration of the hydrotalcite nano bactericide aqueous dispersion liquid is 0.1-2 g/L; the application amount of the hydrotalcite nano bactericide aqueous dispersion is 5-20 g/mu;
the hydrotalcite nano bactericide solid is applied to soil around the root of crops; the application amount of the hydrotalcite nano bactericide solid is 5-20 g/mu.
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