CN115886015A - Rain-wash-resistant tricyclazole suspending agent and preparation method thereof - Google Patents
Rain-wash-resistant tricyclazole suspending agent and preparation method thereof Download PDFInfo
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- CN115886015A CN115886015A CN202211499576.8A CN202211499576A CN115886015A CN 115886015 A CN115886015 A CN 115886015A CN 202211499576 A CN202211499576 A CN 202211499576A CN 115886015 A CN115886015 A CN 115886015A
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- suspending agent
- tricyclazole
- tannic acid
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- 239000000375 suspending agent Substances 0.000 title claims abstract description 123
- DQJCHOQLCLEDLL-UHFFFAOYSA-N tricyclazole Chemical compound CC1=CC=CC2=C1N1C=NN=C1S2 DQJCHOQLCLEDLL-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 238000002360 preparation method Methods 0.000 title abstract description 16
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical class OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 108
- 239000000243 solution Substances 0.000 claims abstract description 56
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 36
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 36
- 229940033123 tannic acid Drugs 0.000 claims abstract description 36
- 235000015523 tannic acid Nutrition 0.000 claims abstract description 36
- 229920002258 tannic acid Polymers 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000080 wetting agent Substances 0.000 claims abstract description 19
- -1 iron ions Chemical class 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 239000010413 mother solution Substances 0.000 claims abstract description 13
- 239000003755 preservative agent Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000002562 thickening agent Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 230000002335 preservative effect Effects 0.000 claims abstract description 12
- 230000000536 complexating effect Effects 0.000 claims abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 46
- 239000012452 mother liquor Substances 0.000 claims description 45
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 42
- 239000004408 titanium dioxide Substances 0.000 claims description 23
- 229920001690 polydopamine Polymers 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 21
- 239000011780 sodium chloride Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 4
- 239000004557 technical material Substances 0.000 claims description 3
- 239000000575 pesticide Substances 0.000 abstract description 15
- 239000003814 drug Substances 0.000 abstract description 12
- 239000007788 liquid Substances 0.000 abstract description 11
- 230000000857 drug effect Effects 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 16
- 241000196324 Embryophyta Species 0.000 description 13
- 241000209094 Oryza Species 0.000 description 11
- 235000007164 Oryza sativa Nutrition 0.000 description 11
- 235000009566 rice Nutrition 0.000 description 11
- 230000000844 anti-bacterial effect Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 230000002265 prevention Effects 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000000361 pesticidal effect Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 229920001864 tannin Polymers 0.000 description 3
- 235000018553 tannin Nutrition 0.000 description 3
- 239000001648 tannin Substances 0.000 description 3
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 2
- 244000052616 bacterial pathogen Species 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 125000000373 fatty alcohol group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 206010059866 Drug resistance Diseases 0.000 description 1
- 230000036579 abiotic stress Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229940009868 aluminum magnesium silicate Drugs 0.000 description 1
- WMGSQTMJHBYJMQ-UHFFFAOYSA-N aluminum;magnesium;silicate Chemical group [Mg+2].[Al+3].[O-][Si]([O-])([O-])[O-] WMGSQTMJHBYJMQ-UHFFFAOYSA-N 0.000 description 1
- 230000002528 anti-freeze Effects 0.000 description 1
- 230000006907 apoptotic process Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 244000000005 bacterial plant pathogen Species 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- UDHMTPILEWBIQI-UHFFFAOYSA-N butyl naphthalene-1-sulfonate;sodium Chemical group [Na].C1=CC=C2C(S(=O)(=O)OCCCC)=CC=CC2=C1 UDHMTPILEWBIQI-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical group OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100001224 moderate toxicity Toxicity 0.000 description 1
- JPMIIZHYYWMHDT-UHFFFAOYSA-N octhilinone Chemical group CCCCCCCCN1SC=CC1=O JPMIIZHYYWMHDT-UHFFFAOYSA-N 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000004563 wettable powder Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The application relates to the technical field of pesticides, and particularly discloses a rain-wash-resistant tricyclazole suspending agent and a preparation method thereof. A rain-wash-resistant tricyclazole suspending agent comprises a tricyclazole suspending agent mother solution and a modified tannic acid solution, wherein the tricyclazole suspending agent mother solution comprises the following raw materials in parts by weight: 30-50 parts of tricyclazole technical product, 0.5-1 part of thickening agent, 5-10 parts of antifreezing agent, 0.5-0.6 part of preservative, 4-6 parts of dispersing wetting agent and 30-40 parts of water; the modified tannic acid solution is a solution obtained by complexing iron ions with tannic acid. The rain-wash-resistant tricyclazole suspending agent has excellent adhesion performance, can effectively resist rain wash, and reduces liquid medicine loss; meanwhile, under the synergistic effect of the modified tannic acid, the suspending agent has better drug effect.
Description
Technical Field
The application relates to the technical field of pesticides, in particular to a rain-wash-resistant tricyclazole suspending agent and a preparation method thereof.
Background
Tricyclazole is a special fungicide for preventing and treating rice blast, has special effect on preventing and treating rice blast, has best use effect before rice attack, and can be used for preventing and treating seedling blast, leaf blast and panicle blast. The tricyclazole belongs to a moderate toxicity bactericide, has stable drug effect, can inhibit the formation of melanin of attached spore, can effectively prevent pathogenic bacteria from invading and reduce the generation of rice blast germ spore, and has wide application on rice.
Meanwhile, in actual use, due to the influence of conditions such as wind blowing, rainfall, dew, sunshine and the like, the adhesiveness of tricyclazole on the surface of a plant is further reduced, particularly, the pesticide effect is obviously reduced when the plant meets rainfall after application, and the pesticide effect period is shortened.
At present, common dosage forms of tricyclazole on the market are wettable powder, and then common suspending agents, so that the adverse conditions that the surface adhesion of plants is poor, the liquid medicine is more lost, and the plants are not resistant to water washing, so that the pesticide effect is poor exist in the using process. Therefore, the development of a tricyclazole product with good adhesion effect and rain wash resistance is needed.
Disclosure of Invention
In order to develop a tricyclazole product with good adhesion effect and rain-wash resistance, the application provides a rain-wash resistance tricyclazole suspending agent and a preparation method thereof.
In a first aspect, the application provides a rain-wash-resistant tricyclazole suspending agent, which adopts the following technical scheme: the rain-wash-resistant tricyclazole suspending agent comprises tricyclazole suspending agent mother liquor and a modified tannic acid solution, wherein the tricyclazole suspending agent mother liquor comprises the following raw materials in parts by weight: 30-50 parts of tricyclazole technical product, 0.5-1 part of thickening agent, 5-10 parts of antifreezing agent, 0.5-0.6 part of preservative, 4-6 parts of dispersing wetting agent and 30-40 parts of water; the modified tannic acid solution is obtained by complexing iron ions with tannic acid.
By adopting the technical scheme, the tannin is a plant polyphenol, and has the advantages of low price, good biocompatibility and the like. In addition, a large number of hydrophobic aromatic rings and hydrophilic phenolic hydroxyl groups in the molecular structure of the tannic acid are easy to interact with various materials through hydrogen bonds, hydrophobicity, pi-pi stacking and the like, and the tannic acid has strong adhesion characteristics on the surfaces of various materials. However, tannic acid can complex with various metal ions, and the unfavorable phenomenon that tannic acid tends to aggregate and adhere to the surface of equipment easily occurs in the production process, which is not favorable for actual production.
And the modified tannic acid that obtains after tannic acid complex iron ion adds to the suspending agent system, because tannic acid has complexed iron ion in advance, can be comparatively stable in process of production, and modified tannic acid can tend to keep away from the metal ion on equipment surface under the influence of charge effect, and then can effectively overcome the bad phenomenon that tannic acid tends to gather the adhesion on equipment surface. Meanwhile, the generation and accumulation of hydrogen peroxide are usually existed in the plant pathogenic bacteria, and the accumulated hydrogen peroxide tends to be positioned on the cell wall; and iron ions complexed in the modified tannic acid can generate Fenton reaction with hydrogen peroxide to generate high-toxicity hydroxyl free radicals, so that bacterial apoptosis is induced.
In conclusion, the modified tannic acid solution is used as one of the raw materials for producing the rain-washing-resistant tricyclazole suspending agent, so that the adhesiveness and hydrophobicity of the suspending agent on the surface of a plant body can be effectively improved, the modified tannic acid has good antibacterial capability, the tricyclazole can be effectively cooperated to perform antibiosis, and the modified tannic acid has positive significance for improving the pesticide effect of the suspending agent and reducing the occurrence of drug resistance of germs. In addition, the modified tannic acid can relieve abiotic stress such as pesticide and the like to a certain extent, has positive effect on plant growth, and has strong practical significance.
In a specific embodiment, the modified tannic acid is prepared by the following steps: dissolving tannic acid in water, and adding FeCl 3 ·6H 2 And O, fully mixing and reacting to obtain the modified tannic acid.
In a specific embodiment, tannic acid and FeCl 3 ·6H 2 The concentrations in the system after O dosing were as follows: tannic acid 30-50g/L, feCl 3 ·6H 2 O 5-10g/L。
In a specific possible embodiment, the mass ratio of the tricyclazole suspending agent mother liquor to the modified tannic acid solution is (15-25): 1.
in a specific possible embodiment, the raw materials of the suspending agent further comprise a titanium dioxide carrier, and the mass ratio of the titanium dioxide carrier to the tricyclazole suspending agent mother liquor is 1: (30-50).
By adopting the technical scheme, the stability of the antibacterial ingredients in the suspending agent can be effectively improved by adding the titanium dioxide carrier, and the titanium dioxide has an antibacterial effect and can be cooperatively matched with other antibacterial ingredients in the suspending agent to further improve the drug effect of the suspending agent. In addition, the photocatalytic activity of the titanium dioxide can promote the degradation of organic matters remained on the surface of the plant in the later period of pesticide application, and has a certain positive significance for reducing pesticide residues.
In a specific embodiment, the dispersing wetting agent is fatty alcohol polyoxyethylene ether.
The liquid medicine can be prevented from permeating and absorbing to a certain extent due to the wax layer on the surface of the plant, and the liquid medicine is not easy to adhere due to the wax layer. Therefore, the fatty alcohol-polyoxyethylene ether is used as the dispersing and wetting agent, and the fatty alcohol-polyoxyethylene ether can dissolve the wax layer on the surface of the plant, so that the permeability and the adhesiveness of the suspending agent on the surface of the plant can be effectively improved.
In a specific possible embodiment, the raw materials of the suspending agent further comprise polydopamine, and the mass ratio of the polydopamine to the tricyclazole suspending agent mother liquor is 1: (1000-1200).
By adopting the technical scheme, the polydopamine has excellent water resistance and biocompatibility, and the contained catechol group can promote adhesion in a manner similar to byssus crosslinking, namely, the adhesion and the water resistance of the suspending agent can be further improved by adding the polydopamine. Because the mechanism of the polydopamine for promoting adhesion is different from that of the modified tannic acid, the polydopamine and the modified tannic acid are used in a matched mode, the adhesion promoting effect can reach the degree that one is added to one and is larger than two, and the actual application effect is good.
In a second aspect, the application provides a preparation method of a rain-wash-resistant tricyclazole suspending agent, which adopts the following technical scheme:
a preparation method of a rain-wash-resistant tricyclazole suspending agent comprises the following steps:
preparing a tricyclazole suspending agent mother solution: uniformly mixing the tricyclazole technical product with a dispersing wetting agent, a thickening agent, an antifreezing agent, a preservative and water, and sanding to obtain a tricyclazole suspending agent mother liquor;
preparing a finished product: heating the tricyclazole suspending agent mother liquor to 40-45 ℃, adding the modified tannic acid solution under the stirring state, then adding sodium chloride, wherein the mass ratio of the total mass of the tricyclazole suspending agent mother liquor and the modified tannic acid solution to the sodium chloride is (4-6): 1, and after the sodium chloride is completely dissolved, continuing stirring and preserving heat for 2-3h to obtain the rain-wash-resistant tricyclazole suspending agent.
By adopting the technical scheme, the tricyclazole suspending agent mother liquor and the modified tannic acid solution are respectively prepared, the modified tannic acid is spontaneously deposited on the surface of the tricyclazole technical product under a high-salt system, and the surface modification is carried out on the tricyclazole technical product particles, so that the more stable adhesion of antibacterial ingredients on the surface of a plant can be promoted when the pesticide is applied, and the leaf surface retention rate of the pesticide is effectively improved.
In a specific implementation mode, in the step of preparing the finished product, before the modified tannic acid solution is added, the titanium dioxide carrier is added into the tricyclazole suspending agent mother liquor, the temperature is heated to 40-45 ℃, and the mixture is fully stirred for 10-30min.
By adopting the technical scheme, the titanium dioxide carrier is added before the modified tannic acid, and the modified tannic acid is deposited after the antibacterial component is loaded, so that the stability of the antibacterial component can be effectively improved on the basis of not influencing the adhesive property. And from the test result, the adhesion performance of the suspending agent is improved to a certain extent by adding the titanium dioxide carrier, and presumably, the titanium dioxide carrier can promote the surface of the plant to form a nano structure with hydrophobic property after being applied with the pesticide, so that the actual application effect is better.
In a specific embodiment, in the step of preparing the final product, polydopamine is added at the same time as the modified tannic acid solution.
In summary, the present application has the following beneficial effects:
1. according to the method, the surface modification is carried out on the tricyclazole raw pesticide particles by utilizing the characteristic that the modified tannic acid is spontaneously deposited on the surface of the material under a high-salt system, and the tricyclazole raw pesticide subjected to surface modification has a stronger adhesion effect on the leaf surfaces of crops and is more resistant to rainwater washing; meanwhile, the bounce of the pesticide liquid in the contact process with the leaf surfaces of crops can be reduced, the retention rate of the leaf surfaces of the pesticide is effectively improved, the effect lasts longer, and the application prospect is very wide.
2. The modified tannic acid is obtained by complexing tannic acid with iron ions, so that the bad phenomenon that the tannic acid is gathered and adhered to the surface of equipment due to complexing action in the production process can be effectively overcome, and the production is convenient; and the modified tannic acid has unique antibacterial performance and can play a more excellent antibacterial effect in cooperation with the tricyclazole technical product.
3. Adopt fatty alcohol polyoxyethylene ether as dispersion wetting agent in this application, further add polydopamine on this basis, can effectively promote liquid medicine osmotic absorption and adhesion through dissolving plant surface wax layer after giving medicine to the poor free of charge, practical application effect is preferred.
Detailed Description
The present application will be described in further detail with reference to the following examples and comparative examples, and the starting materials referred to in the present application are commercially available, and experimental methods without specifying specific conditions in the following examples are selected according to conventional methods and conditions, or according to the specifications of commercial products. If the temperature is not particularly emphasized, the reaction is usually carried out at room temperature, and room temperature in the present invention means 10 to 30 ℃.
The thickeners, antifreeze, preservatives and dispersing wetters in examples 1 to 3 were of the same type, as follows: the thickening agent is aluminum magnesium silicate; the antifreezing agent is ethylene glycol; the preservative is Kathon; the dispersing and wetting agent is fatty alcohol polyoxyethylene ether.
Example 1
A rain-wash-resistant tricyclazole suspending agent comprises a tricyclazole suspending agent mother solution and a modified tannic acid solution, wherein the mass ratio of the tricyclazole suspending agent mother solution to the modified tannic acid solution is 20:1. the tricyclazole suspending agent mother liquor comprises the following raw materials in parts by weight: 50kg of tricyclazole technical material, 0.5kg of thickening agent, 5kg of antifreezing agent, 0.5kg of preservative, 4kg of dispersing wetting agent and 40kg of water;
the modified tannic acid solution is obtained by complexing iron ions with tannic acid, and the specific preparation method comprises the following steps: dissolving tannic acid in water to obtain tannic acid concentration of 35g/L, and adding FeCl 3 ·6H 2 O, feCl in the System 3 ·6H 2 The concentration of O is 6g/L, and the modified tannic acid is obtained after fully mixing and reacting for 5 h.
The preparation method of the rain-wash-resistant tricyclazole suspending agent comprises the following steps:
(1) Preparing a tricyclazole suspending agent mother solution: putting tricyclazole technical, a dispersing wetting agent, a thickening agent, an antifreezing agent, a preservative and water into a feeding kettle, uniformly shearing, and then sanding by a sanding machine, wherein the grain diameter after sanding is controlled to be D90 less than 3 mu m, so as to obtain tricyclazole suspending agent mother liquor;
(2) And (3) preparing a finished product: heating the tricyclazole suspending agent mother liquor to 40 ℃, and slowly adding the modified tannic acid solution according to the mass ratio of 20; and after the solution system is stirred for 30min, adding sodium chloride particles into the system according to the mass ratio of 5:1, and after the sodium chloride is completely dissolved, continuously stirring and preserving heat for 2h to obtain the rain wash resistant tricyclazole suspending agent.
Example 2
A rain-wash-resistant tricyclazole suspending agent comprises a tricyclazole suspending agent mother solution and a modified tannic acid solution, wherein the mass ratio of the tricyclazole suspending agent mother solution to the modified tannic acid solution is 25:1. the tricyclazole suspending agent mother liquor comprises the following raw materials in parts by weight: 30kg of tricyclazole technical product, 1kg of thickening agent, 5kg of antifreezing agent, 0.6kg of preservative, 6kg of dispersing wetting agent and 30kg of water;
the modified tannic acid solution is obtained by complexing iron ions with tannic acid, and the specific preparation method comprises the following steps: dissolving tannic acid in water to obtain tannic acid concentration of 40g/L, and adding FeCl 3 ·6H 2 O, feCl in the System 3 ·6H 2 The concentration of O is 8g/L, and the modified tannic acid is obtained after fully mixing and reacting for 5 hours.
The preparation method of the rain-wash-resistant tricyclazole suspending agent comprises the following steps:
(1) Preparing a tricyclazole suspending agent mother solution: putting tricyclazole technical, a dispersing wetting agent, a thickening agent, an antifreezing agent, a preservative and water into a feeding kettle, uniformly shearing, and then sanding by a sanding machine, wherein the grain diameter after sanding is controlled to be D90 less than 3 mu m, so as to obtain tricyclazole suspending agent mother liquor;
(2) Preparing a finished product: heating the tricyclazole suspending agent mother liquor to 45 ℃, and slowly adding the modified tannic acid solution according to the mass ratio of 25; after the solution system is stirred for 40min, adding sodium chloride particles into the system according to the mass ratio of 5:1, and after the sodium chloride is completely dissolved, continuously stirring and preserving heat for 3h to obtain the rain wash resistant tricyclazole suspending agent.
Example 3
A rain-wash-resistant tricyclazole suspending agent comprises a tricyclazole suspending agent mother solution and a modified tannic acid solution, wherein the mass ratio of the tricyclazole suspending agent mother solution to the modified tannic acid solution is 15:1. the tricyclazole suspending agent mother liquor comprises the following raw materials in parts by weight: 40kg of tricyclazole technical material, 0.8kg of thickening agent, 8kg of antifreezing agent, 0.6kg of preservative, 5kg of dispersing wetting agent and 35kg of water;
the modified tannic acid solution is obtained by complexing tannic acid with iron ions, and the specific preparation method comprises the following steps: dissolving tannic acid in water to obtain tannic acid concentration of 35g/L, and adding FeCl 3 ·6H 2 O, feCl in the System 3 ·6H 2 The concentration of O is 6g/L, and the modified tannic acid is obtained after fully mixing and reacting for 5 h.
The preparation method of the rain-wash-resistant tricyclazole suspending agent comprises the following steps:
(1) Preparing a tricyclazole suspending agent mother solution: putting tricyclazole technical, a dispersing wetting agent, a thickening agent, an antifreezing agent, a preservative and water into a feeding kettle, uniformly shearing, and then sanding by a sanding machine, wherein the grain diameter after sanding is controlled to be D90 less than 3 mu m, so as to obtain tricyclazole suspending agent mother liquor;
(2) And (3) preparing a finished product: heating the tricyclazole suspending agent mother liquor to 43 ℃, and slowly adding the modified tannic acid solution according to the mass ratio of 15; and after the solution system is stirred for 50min, adding sodium chloride particles into the system according to the mass ratio of 5:1, and after the sodium chloride is completely dissolved, continuously stirring and preserving heat for 2.5h to obtain the rain-wash-resistant tricyclazole suspending agent.
Example 4
The difference between the embodiment and the embodiment 1 is that the mass ratio of the tricyclazole suspending agent mother liquor to the modified tannic acid solution is 15:1.
example 5
The difference between the embodiment and the embodiment 1 is that the mass ratio of the tricyclazole suspending agent mother liquor to the modified tannic acid solution is 25:1.
example 6
The difference between the embodiment and the embodiment 1 is that the mass ratio of the tricyclazole suspending agent mother liquor to the modified tannic acid solution is 10:1.
example 7
The difference between the embodiment and the embodiment 1 is that the mass ratio of the tricyclazole suspending agent mother liquor to the modified tannic acid solution is 30:1.
example 8
The present embodiment is different from embodiment 1 in thatThe modified tannic acid solution is obtained by complexing iron ions with tannic acid, and the specific preparation method is as follows: dissolving tannic acid in water to obtain tannic acid concentration of 30g/L, and adding FeCl 3 ·6H 2 O, feCl in the System 3 ·6H 2 The concentration of O is 5g/L, and the modified tannic acid is obtained after fully mixing and reacting for 5 h.
Example 9
The difference between this example and example 1 is that the modified tannic acid solution is obtained by complexing iron ions with tannic acid, and the specific preparation method is as follows: dissolving tannic acid in water to obtain tannic acid concentration of 50g/L, and adding FeCl 3 ·6H 2 O, feCl in the System 3 ·6H 2 The concentration of O is 10g/L, and the modified tannic acid is obtained after fully mixing and reacting for 5 hours.
Example 10
The difference between the embodiment and the embodiment 1 is that the raw materials of the suspending agent also comprise a titanium dioxide carrier with the particle size of 20-40nm, and the mass ratio of the titanium dioxide carrier to the tricyclazole suspending agent mother liquor is 1:40, and the finished product in the step (2) is prepared as follows:
heating the tricyclazole suspending agent mother liquor to 40 ℃, adding the titanium dioxide carrier under the stirring of 500rpm, stirring for 15min, and slowly adding the modified tannic acid solution according to the mass ratio of 20; and after the solution system is stirred for 30min, adding sodium chloride particles into the system according to the mass ratio of 5:1, and after the sodium chloride is completely dissolved, continuously stirring and preserving heat for 2h to obtain the rain wash resistant tricyclazole suspending agent.
Example 11
The difference between the embodiment and the embodiment 10 is that the mass ratio of the titanium dioxide carrier to the tricyclazole suspending agent mother liquor is 1:30.
example 12
The difference between the embodiment and the embodiment 10 is that the mass ratio of the titanium dioxide carrier to the tricyclazole suspending agent mother liquor is 1:50.
example 13
The difference between the embodiment and the embodiment 1 is that the raw materials of the suspending agent also comprise polydopamine with the number average molecular weight of 2000-3000, and the mass ratio of the polydopamine to the tricyclazole suspending agent mother liquor is 1:1000, parts by weight; and the finished product in the step (2) is prepared as follows:
heating the tricyclazole suspending agent mother liquor to 40 ℃, slowly adding the modified tannic acid solution according to the mass ratio of 20 to 1 under the stirring of 500rpm, and then adding polydopamine; and after the solution system is stirred for 30min, adding sodium chloride particles into the system according to the mass ratio of 5:1, and after the sodium chloride is completely dissolved, continuously stirring and preserving heat for 2h to obtain the rain wash resistant tricyclazole suspending agent.
Example 14
The difference between the embodiment and the embodiment 13 is that the mass ratio of the polydopamine to the tricyclazole suspending agent mother liquor is 1:1100.
example 15
The difference between the embodiment and the embodiment 13 is that the mass ratio of the polydopamine to the tricyclazole suspending agent mother liquor is 1:1200.
example 16
This example differs from example 1 in that the dispersion wetting agent is tween 80.
Example 17
This example differs from example 1 in that the dispersing wetting agent is sodium butylnaphthalenesulfonate.
Example 18
The difference between the present example and example 1 is that in the step (2) of preparing the finished product, the mass ratio of the total mass of the tricyclazole suspending agent mother liquor and the modified tannic acid solution to the mass of the sodium chloride is 4:1.
Example 19
The difference between the present example and example 1 is that in the step (2) of preparing the finished product, the mass ratio of the total mass of the tricyclazole suspending agent mother liquor and the modified tannic acid solution to the mass of the sodium chloride is 6:1.
Example 20
The difference between the embodiment and the embodiment 1 is that the raw materials of the suspending agent also comprise a titanium dioxide carrier with the particle size of 20-40nm and polydopamine with the number average molecular weight of 2000-3000, and the mass ratio of the titanium dioxide carrier to the tricyclazole suspending agent mother liquor is 1:40, the mass ratio of the polydopamine to the tricyclazole suspending agent mother liquor is 1:1000; and the finished product in the step (2) is prepared as follows:
heating the tricyclazole suspending agent mother liquor to 40 ℃, adding a titanium dioxide carrier and stirring for 15min under the stirring of 500rpm, then slowly adding the modified tannic acid solution according to the mass ratio of 20; and after the solution system is stirred for 30min, adding sodium chloride particles into the system according to the mass ratio of 5:1, and after the sodium chloride is completely dissolved, continuously stirring and preserving heat for 2h to obtain the rain wash resistant tricyclazole suspending agent.
Comparative example 1
This comparative example differs from example 1 in that no modified tannic acid solution was added.
Comparative example 2
This comparative example differs from example 1 in that the modified tannic acid solution was replaced with an equivalent amount of tannic acid solution of equal concentration.
Comparative example 3
This comparative example is different from example 1 in that the modified tannic acid solution was not added and polydopamine in example 13 was added.
Comparative example 4
This comparative example differs from example 1 in that no sodium chloride was added in the preparation of the final product in step (2).
Performance detection test method
1. The rain erosion resistance test method comprises the following steps:
1) Preparing a liquid medicine: adding water to the rain-wash-resistant tricyclazole suspending agent samples obtained in examples 1-20 and comparative examples 1-4 to prepare 40% tricyclazole SC, and adding water to dilute 300 times to prepare uniform liquid medicine;
2) Sample treatment: sucking 1 microliter of each treatment medicine liquid on clean rice leaves by using a liquid transfer gun, putting three rice leaves of each treatment medicine liquid in an incubator at 30 ℃ for drying for 3 hours, and taking a picture of the dried glass slide under a microscope;
3) And (3) rain wash treatment: placing the rice leaves under a spraying tower at an inclination of 60 degrees, spraying 1L of water, drying the rice leaves in an incubator at 30 ℃ after spraying, and taking a picture under a microscope;
4) Data processing and calculation: and (3) calculating the areas of the pesticide spots on the rice leaves before and after the spray washing by using software, and obtaining the rain wash resistant effect by the ratio of the areas of the pesticide spots after washing to the areas of the pesticide spots before washing.
2. Prevention and treatment test
The test is carried out in paddy field with serious rice blast over the years, and each plot is not less than 40m 2 The test was repeated 4 times, and the investigation method and the evaluation of the drug effect were carried out in accordance with GB/T17980.19-2000.
TABLE 2 test data sheet
According to the test data in table 2 and the specific combination of the test results of example 1 and comparative examples 1-2, the area ratio of the drug spot before and after flushing of the tricyclazole suspending agent in example 1 can reach 93.32%, while the area ratio of the drug spot before and after flushing of the tricyclazole suspending agent in comparative example 1 is only 60.29%. Analysis shows that the addition of the modified tannic acid solution can effectively improve the adhesion performance and the rain wash resistance of the suspending agent; and further compared with the unmodified common tannic acid solution in the comparative example 2, the area ratio of the pesticide stain before and after the flushing of the suspending agent in the comparative example 2 is 88.30%, which shows that the modified tannic acid solution has better effect of improving the adhesion performance and the rain wash resistance of the suspending agent compared with the unmodified tannic acid solution.
And from the actual prevention effect, the prevention effect of the modified tannin is obviously superior to that of the comparative examples 1-2, and analysis shows that the iron ions complexed in the modified tannin can play a better role in synergistic prevention and control.
According to the test results of the embodiment 1 and the embodiments 10-12, the addition of the titanium dioxide carrier has positive significance for further improving the rain wash resistance of the suspending agent, and the titanium dioxide carrier probably forms a special hydrophobic nanostructure on the leaf surface; and the control effect is further improved, which shows that the titanium dioxide can play a role in synergistic antibiosis.
In combination with the test results of example 1 and examples 13-15, the addition of polydopamine can synergistically modify tannic acid to achieve better rain wash resistance and also has certain improvement effect on the prevention effect. Further comparison with comparative example 3 shows that the effect of improving the rainfastness of the suspending agent when polydopamine is used alone is lower than that of examples 1 and 13, indicating that polydopamine and modified tannic acid have a better synergistic effect.
According to the test results of the embodiment 1 and the embodiments 16 to 17, the rainwash resistance and the prevention effect of the suspending agent in the embodiment 1 are obviously better than those of the embodiments 16 to 17, which shows that the fatty alcohol-polyoxyethylene ether has an obvious positive effect compared with other dispersing and wetting agents, and the analysis shows that the characteristic of dissolving the wax layer of the fatty alcohol-polyoxyethylene ether has an obvious positive significance for improving the rainwash resistance and the prevention effect of the suspending agent except for the conventional dispersing and wetting effect.
The specific embodiments are only for explaining the present application and are not limiting to the present application, and those skilled in the art can make modifications to the embodiments without inventive contribution as required after reading the present specification, but all the embodiments are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The rain-wash-resistant tricyclazole suspending agent is characterized by comprising tricyclazole suspending agent mother liquor and a modified tannic acid solution, wherein the tricyclazole suspending agent mother liquor comprises the following raw materials in parts by weight: 30-50 parts of tricyclazole technical material, 0.5-1 part of thickening agent, 5-10 parts of antifreezing agent, 0.5-0.6 part of preservative, 4-6 parts of dispersing wetting agent and 30-40 parts of water; the modified tannic acid solution is obtained by complexing iron ions with tannic acid.
2. The rain-wash-resistant tricyclazole suspending agent as claimed in claim 1, wherein the modified tannic acid is prepared by the following steps: dissolving tannic acid in water, and adding FeCl 3 ·6H 2 And O, fully mixing and reacting to obtain the modified tannic acid.
3. The stormwater-washability type tricyclazole suspending agent as claimed in claim 2, wherein said suspending agent comprises tannic acid and FeCl 3 ·6H 2 The concentrations in the system after O dosing were as follows: tannic acid 30-50g/L, feCl 3 ·6H 2 O 5-10g/L。
4. The rain-wash-resistant tricyclazole suspending agent as claimed in claim 3, wherein the mass ratio of the tricyclazole suspending agent mother liquor to the modified tannic acid solution is (15-25): 1.
5. the rain-wash-resistant tricyclazole suspending agent as claimed in claim 1, wherein the suspending agent further comprises a titanium dioxide carrier, and the mass ratio of the titanium dioxide carrier to the tricyclazole suspending agent mother liquor is 1: (30-50).
6. The stormwater-resistant tricyclazole suspending agent as claimed in claim 1 or 5, wherein the dispersing wetting agent is fatty alcohol-polyoxyethylene ether.
7. The rainfastness tricyclazole suspending agent as claimed in claim 6, wherein the suspending agent raw material further comprises polydopamine, and the mass ratio of polydopamine to tricyclazole suspending agent mother liquor is 1: (1000-1200).
8. The process for preparing a stormwater-resistant tricyclazole suspending agent as claimed in any one of claims 1 to 7, comprising the steps of:
preparing a tricyclazole suspending agent mother solution: uniformly mixing the tricyclazole technical product with a dispersing wetting agent, a thickening agent, an antifreezing agent, a preservative and water, and sanding to obtain a tricyclazole suspending agent mother liquor;
and (3) preparing a finished product: heating the tricyclazole suspending agent mother liquor to 40-45 ℃, adding the modified tannic acid solution under stirring, then adding sodium chloride, wherein the mass ratio of the total mass of the tricyclazole suspending agent mother liquor and the modified tannic acid solution to the sodium chloride is (4-6): 1, and after the sodium chloride is completely dissolved, continuously stirring and preserving heat for 2-3h to obtain the rain-wash-resistant tricyclazole suspending agent.
9. The method for preparing the rain-wash-resistant tricyclazole suspending agent as claimed in claim 8, wherein the step of preparing the final product comprises adding the titanium dioxide carrier into the tricyclazole suspending agent mother liquor before adding the modified tannic acid solution, heating to 40-45 ℃, and fully stirring for 10-30min.
10. The method for preparing the rain-wash-resistant tricyclazole suspending agent as claimed in claim 8, wherein the step of preparing the final product comprises adding polydopamine while adding the modified tannic acid solution.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108378048A (en) * | 2018-04-23 | 2018-08-10 | 江苏邦盛生物科技有限责任公司 | A kind of white tricyclazole suspending agent and preparation method thereof |
| CN110050787A (en) * | 2019-04-26 | 2019-07-26 | 中国农业科学院农业环境与可持续发展研究所 | A kind of preparation method of tannic acid modification blade face adhesion type pesticide |
| CN111869661A (en) * | 2020-08-20 | 2020-11-03 | 蚌埠格润生物科技有限公司 | High-concentration tricyclazole suspending agent and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108378048A (en) * | 2018-04-23 | 2018-08-10 | 江苏邦盛生物科技有限责任公司 | A kind of white tricyclazole suspending agent and preparation method thereof |
| CN110050787A (en) * | 2019-04-26 | 2019-07-26 | 中国农业科学院农业环境与可持续发展研究所 | A kind of preparation method of tannic acid modification blade face adhesion type pesticide |
| CN111869661A (en) * | 2020-08-20 | 2020-11-03 | 蚌埠格润生物科技有限公司 | High-concentration tricyclazole suspending agent and preparation method thereof |
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