CN117247303A - Pesticide fertilizer composition with weeding effect and preparation method thereof - Google Patents
Pesticide fertilizer composition with weeding effect and preparation method thereof Download PDFInfo
- Publication number
- CN117247303A CN117247303A CN202311242265.8A CN202311242265A CN117247303A CN 117247303 A CN117247303 A CN 117247303A CN 202311242265 A CN202311242265 A CN 202311242265A CN 117247303 A CN117247303 A CN 117247303A
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- China
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- parts
- mof
- pesticide
- fertilizer composition
- lignin sulfonate
- Prior art date
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 62
- 239000000575 pesticide Substances 0.000 title claims abstract description 58
- 238000009333 weeding Methods 0.000 title claims abstract description 48
- 239000000203 mixture Substances 0.000 title claims abstract description 44
- 230000000694 effects Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000002363 herbicidal effect Effects 0.000 claims abstract description 64
- 239000005631 2,4-Dichlorophenoxyacetic acid Substances 0.000 claims abstract description 53
- 239000004480 active ingredient Substances 0.000 claims abstract description 43
- 239000004009 herbicide Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002539 nanocarrier Substances 0.000 claims abstract description 29
- 239000002131 composite material Substances 0.000 claims abstract description 26
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 22
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 11
- 239000003899 bactericide agent Substances 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 239000000945 filler Substances 0.000 claims abstract description 11
- 239000000080 wetting agent Substances 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 52
- 239000002105 nanoparticle Substances 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000001291 vacuum drying Methods 0.000 claims description 30
- 239000010410 layer Substances 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 28
- 238000005406 washing Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 23
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 22
- IIDQAAJTECOGEG-UHFFFAOYSA-N 6-bromo-7-hydroxy-4-(hydroxymethyl)chromen-2-one Chemical compound C1=C(O)C(Br)=CC2=C1OC(=O)C=C2CO IIDQAAJTECOGEG-UHFFFAOYSA-N 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 14
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 13
- 230000000361 pesticidal effect Effects 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 230000010355 oscillation Effects 0.000 claims description 10
- VZJJZMXEQNFTLL-UHFFFAOYSA-N chloro hypochlorite;zirconium;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Zr].ClOCl VZJJZMXEQNFTLL-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- ASOKPJOREAFHNY-UHFFFAOYSA-N 1-Hydroxybenzotriazole Chemical compound C1=CC=C2N(O)N=NC2=C1 ASOKPJOREAFHNY-UHFFFAOYSA-N 0.000 claims description 7
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 claims description 7
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 7
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 7
- -1 compound amino acid Chemical class 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 235000019253 formic acid Nutrition 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004440 column chromatography Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000012044 organic layer Substances 0.000 claims description 5
- SUAKHGWARZSWIH-UHFFFAOYSA-N N,N‐diethylformamide Chemical compound CCN(CC)C=O SUAKHGWARZSWIH-UHFFFAOYSA-N 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 239000004576 sand Substances 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- WCXDHFDTOYPNIE-RIYZIHGNSA-N (E)-acetamiprid Chemical compound N#C/N=C(\C)N(C)CC1=CC=C(Cl)N=C1 WCXDHFDTOYPNIE-RIYZIHGNSA-N 0.000 claims description 2
- PGOOBECODWQEAB-UHFFFAOYSA-N (E)-clothianidin Chemical compound [O-][N+](=O)\N=C(/NC)NCC1=CN=C(Cl)S1 PGOOBECODWQEAB-UHFFFAOYSA-N 0.000 claims description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 claims description 2
- IBSREHMXUMOFBB-JFUDTMANSA-N 5u8924t11h Chemical compound O1[C@@H](C)[C@H](O)[C@@H](OC)C[C@@H]1O[C@@H]1[C@@H](OC)C[C@H](O[C@@H]2C(=C/C[C@@H]3C[C@@H](C[C@@]4(O3)C=C[C@H](C)[C@@H](C(C)C)O4)OC(=O)[C@@H]3C=C(C)[C@@H](O)[C@H]4OC\C([C@@]34O)=C/C=C/[C@@H]2C)/C)O[C@H]1C.C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 IBSREHMXUMOFBB-JFUDTMANSA-N 0.000 claims description 2
- 239000005660 Abamectin Substances 0.000 claims description 2
- 239000005875 Acetamiprid Substances 0.000 claims description 2
- 239000005742 Bupirimate Substances 0.000 claims description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000005888 Clothianidin Substances 0.000 claims description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 claims description 2
- NQRFDNJEBWAUBL-UHFFFAOYSA-N N-[cyano(2-thienyl)methyl]-4-ethyl-2-(ethylamino)-1,3-thiazole-5-carboxamide Chemical compound S1C(NCC)=NC(CC)=C1C(=O)NC(C#N)C1=CC=CS1 NQRFDNJEBWAUBL-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 229950008167 abamectin Drugs 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 229940077388 benzenesulfonate Drugs 0.000 claims description 2
- SRSXLGNVWSONIS-UHFFFAOYSA-M benzenesulfonate Chemical compound [O-]S(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-M 0.000 claims description 2
- DSKJPMWIHSOYEA-UHFFFAOYSA-N bupirimate Chemical compound CCCCC1=C(C)N=C(NCC)N=C1OS(=O)(=O)N(C)C DSKJPMWIHSOYEA-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- DUEPRVBVGDRKAG-UHFFFAOYSA-N carbofuran Chemical compound CNC(=O)OC1=CC=CC2=C1OC(C)(C)C2 DUEPRVBVGDRKAG-UHFFFAOYSA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- WZISDKTXHMETKG-UHFFFAOYSA-H dimagnesium;dipotassium;trisulfate Chemical compound [Mg+2].[Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O WZISDKTXHMETKG-UHFFFAOYSA-H 0.000 claims description 2
- CJHXCRMKMMBYJQ-UHFFFAOYSA-N dimethirimol Chemical compound CCCCC1=C(C)NC(N(C)C)=NC1=O CJHXCRMKMMBYJQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 239000004021 humic acid Substances 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229920000120 polyethyl acrylate Polymers 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 229940048842 sodium xylenesulfonate Drugs 0.000 claims description 2
- QUCDWLYKDRVKMI-UHFFFAOYSA-M sodium;3,4-dimethylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1C QUCDWLYKDRVKMI-UHFFFAOYSA-M 0.000 claims description 2
- RUTSRVMUIGMTHJ-UHFFFAOYSA-M sodium;tetradec-1-ene-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCC=CS([O-])(=O)=O RUTSRVMUIGMTHJ-UHFFFAOYSA-M 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims 1
- 238000011068 loading method Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 35
- 241000196324 Embryophyta Species 0.000 description 12
- 240000008042 Zea mays Species 0.000 description 10
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 10
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 10
- 235000005822 corn Nutrition 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 239000003814 drug Substances 0.000 description 8
- 241000209140 Triticum Species 0.000 description 7
- 235000021307 Triticum Nutrition 0.000 description 7
- 238000005507 spraying Methods 0.000 description 7
- 229940079593 drug Drugs 0.000 description 5
- 230000001965 increasing effect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000001186 cumulative effect Effects 0.000 description 4
- 239000000017 hydrogel Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000002035 prolonged effect Effects 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 241001057636 Dracaena deremensis Species 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 229940088597 hormone Drugs 0.000 description 3
- 239000005556 hormone Substances 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 208000003643 Callosities Diseases 0.000 description 2
- 206010020649 Hyperkeratosis Diseases 0.000 description 2
- 238000012271 agricultural production Methods 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 238000013270 controlled release Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000009331 sowing Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- OVSKIKFHRZPJSS-DOMIDYPGSA-N 2-(2,4-dichlorophenoxy)acetic acid Chemical compound OC(=O)[14CH2]OC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-DOMIDYPGSA-N 0.000 description 1
- 235000007319 Avena orientalis Nutrition 0.000 description 1
- 241000209763 Avena sativa Species 0.000 description 1
- 235000007558 Avena sp Nutrition 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 240000005979 Hordeum vulgare Species 0.000 description 1
- 235000007340 Hordeum vulgare Nutrition 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- 235000019714 Triticale Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 125000000332 coumarinyl group Chemical group O1C(=O)C(=CC2=CC=CC=C12)* 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007884 disintegrant Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000003854 herbicide residue Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 239000013642 negative control Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 241000228158 x Triticosecale Species 0.000 description 1
- GBNDTYKAOXLLID-UHFFFAOYSA-N zirconium(4+) ion Chemical compound [Zr+4] GBNDTYKAOXLLID-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/60—Biocides or preservatives, e.g. disinfectants, pesticides or herbicides; Pest repellants or attractants
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/70—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting wettability, e.g. drying agents
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Plant Pathology (AREA)
- Soil Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a pesticide fertilizer composition with weeding effect and a preparation method thereof, belonging to the technical field of agriculture, wherein the pesticide fertilizer composition comprises the following components in parts by weight: 25-40 parts of functional herbicide, 5-15 parts of pesticide, 5-10 parts of bactericide, 30-50 parts of fertilizer, 5-15 parts of dispersing agent, 1-3 parts of wetting agent, 0.5-3 parts of disintegrating agent, 3-10 parts of filler and 50-70 parts of deionized water; the functional herbicide is a MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with a weeding active ingredient and ammonium sulfate. The invention provides a method for loading 2,4-D into a nanomaterial after covalent connection of the 2,4-D and the photoinduced breaking group, which can realize the light-operated slow release of the 2,4-D, effectively prolong the action time of the 2,4-D, promote the pesticide to reduce the application and the effect and reduce the environmental pollution.
Description
Technical Field
The invention belongs to the technical field of agriculture, and particularly relates to a pesticide fertilizer composition with a weeding effect and a preparation method thereof.
Background
The herbicide plays an important role in weed control, a large amount of herbicide is widely used in agricultural production, the use of the herbicide reduces the labor-intensive work load such as weeding, realizes protective cultivation, and reduces soil and water and production cost; the hormone herbicide is widely used due to the characteristics of high selectivity, broad spectrum, good effect and low cost, wherein 2,4-D, namely 2, 4-dichlorophenoxyacetic acid, is a widely used pre-seedling and post-seedling hormone systemic selective herbicide, is used as foliar spray of wheat, barley, oat, triticale, corn and the like, can effectively control broadleaf weeds in cereal crops and lawns, and the active ingredients of the hormone herbicide are rapidly transferred in plant leaves and roots and play an important role in weed control; however, after the conventional 2,4-D herbicide is sprayed, the soil accumulates a relatively high concentration of 2,4-D in a short period of time, and at the same time, the aquatic food net is polluted due to excessive spraying and drifting of the pesticide, and then the herbicide residue enters the marine environment and finally enters the human body through the feeding of animals; the current pesticide slow release system is greatly concerned, and the slow release type pesticide can lead the drug to be slowly released within a certain time, prolong the drug effect, reduce the pesticide dosage and reduce the pollution; however, most of the drugs are loaded through surface adhesion or electrostatic adsorption, so that the drug loading capacity is low, the drug burst release behavior exists, and most of the slow release pesticides are released only through simple diffusion, so that the controlled release cannot be really realized; the agricultural production uses the pesticides and the fertilizers in combination, so that the two operation steps in the field are combined into one, not only are the labor force and the time saved and the production cost reduced, but also the synergistic effect between the pesticides and the fertilizers can be increased and the dosage of the pesticides and the fertilizers can be reduced, thereby protecting the environment and improving the crop yield.
The existing herbicide technology mainly has the following problems: the first, traditional formulation has higher loss rate in use, and more residual quantity, and causes harm to the environment and the health; secondly, most pesticide slow-release systems load pesticides through surface adhesion or electrostatic adsorption, so that the drug loading rate is low, and the pesticide burst release behavior exists; thirdly, most of the slow-release pesticides only diffuse active ingredients simply, and can not realize the controlled release really.
Disclosure of Invention
The invention provides a pesticide fertilizer composition with weeding effect, and aims to solve the problems of high loss rate and high residual quantity of 2,4-D in use.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the invention provides a pesticide fertilizer composition with a weeding effect, which comprises the following components in parts by weight: 25-40 parts of functional herbicide, 5-15 parts of pesticide, 5-10 parts of bactericide, 30-50 parts of fertilizer, 5-15 parts of dispersing agent, 1-3 parts of wetting agent, 0.5-3 parts of disintegrating agent, 3-10 parts of filler and 50-70 parts of deionized water.
Preferably, the functional herbicide is a MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with a weeding active ingredient and ammonium sulfate;
preferably, the weeding active ingredient is a compound formed by covalently connecting 2,4-D and 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin;
preferably, the preparation method of the functional herbicide specifically comprises the following steps:
s1, adding zirconium oxychloride octahydrate into N, N-dimethylformamide, carrying out ultrasonic oscillation for 45min, adding 2-amino terephthalic acid, carrying out ultrasonic oscillation for 30min, adding formic acid into the solution, stirring for 30min at room temperature, transferring the mixed solution into a reaction kettle, reacting for 2-3 days under the heating condition of 120-150 ℃, cooling to room temperature after the reaction is finished, filtering, collecting crystals, washing with N, N-dimethylformamide for 5 times, washing with acetone to remove residual N, N-diethylformamide, and carrying out vacuum drying for 48 hours in a vacuum drying box at 120 ℃ to obtain MOF-3 nano particles;
s2, dissolving 2,4-D in N, N-dimethylformamide, adding a catalyst of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 1-hydroxybenzotriazole, stirring for 30min under ice bath, adding 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin, reacting for 12h at room temperature, adding water and ethyl acetate for extraction after the reaction is finished, drying an organic layer, concentrating, and performing column chromatography to obtain a compound formed by covalently connecting a weeding active ingredient of 2,4-D and 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin;
s3, adding the weeding active ingredient prepared in the step S2 into an ethanol solution, stirring uniformly at room temperature, adding the MOF-3 nano particles prepared in the step S1, heating to 45-60 ℃, reacting for 3-5h, washing the product with ethanol for 3 times, and vacuum drying for 5h at 50 ℃ in a vacuum drying oven to obtain MOF-3 nano particles loaded with the weeding active ingredient;
s4, adding the MOF-3 nano particles loaded with the weeding active ingredients prepared in the step S3 into a sodium lignin sulfonate aqueous solution, adding glacial acetic acid, stirring for 1.5-3 hours at room temperature, centrifuging, washing with deionized water, and drying to obtain the MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with the weeding active ingredients;
s5, dissolving the MOF-3@sodium lignin sulfonate double-layer composite nano carrier prepared in the step S4 in an ammonium sulfate aqueous solution, stirring for 3-5 hours at room temperature, centrifuging after the reaction is finished, washing with deionized water, and vacuum drying for 6 hours at 70 ℃ in a vacuum drying oven to obtain the MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with the weeding active ingredients and ammonium sulfate.
Preferably, in S1, the molar concentration of zirconium oxychloride octahydrate in N, N-dimethylformamide is: 18-25mmol/L;
preferably, in S1, the molar ratio of zirconium oxychloride octahydrate to 2-aminoterephthalic acid is: 1.5-3:1;
preferably, in S1, the volume ratio of N, N-dimethylformamide to formic acid is: 15-20:1;
preferably, in S2, the molar concentration of 2,4-D in N, N-dimethylformamide is: 50-60mmol/L;
preferably, in S2, the molar ratio of 2,4-D, 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 1-hydroxybenzotriazole is: 1:1.5-2:1:1.3;
preferably, in S3, the concentration of the herbicidal active ingredient in the ethanol solution is: 5-10mg/mL;
preferably, in S3, the mass ratio of the herbicidal active ingredient to the MOF-3 nanoparticle is: 3-5:1;
preferably, in S4, the concentration of the aqueous solution of sodium lignin sulfonate is: 9-20mg/mL;
preferably, in S4, the mass ratio of the MOF-3 nanoparticle loaded with the herbicidal active ingredient to the sodium lignin sulfonate is: 1:1.5-3;
preferably, in S4, the mass ratio of MOF-3 nanoparticles loaded with herbicidal active ingredients to glacial acetic acid is: 1:0.5-0.7;
preferably, in S5, the concentration of the aqueous solution of ammonium sulfate is 10-15mg/mL;
preferably, in S5, the mass ratio of the MOF-3@sodium lignin sulfonate double-layer composite nano carrier to the ammonium sulfate is 1:1.5-3.5.
The invention also provides a preparation method of the pesticide fertilizer composition with the weeding effect, which comprises the following steps: weighing functional herbicide, fertilizer, pesticide, bactericide, dispersing agent, wetting agent, disintegrating agent and filler according to parts by weight, uniformly stirring in water, grinding in a sand mill, spray drying, and screening to obtain the pesticide fertilizer composition with weeding effect.
Preferably, the fertilizer comprises: urea, potassium chloride, humic acid, compound amino acid, potassium magnesium sulfate;
preferably, the insecticide comprises: one or more of abamectin, carbofuran, methyl pyrifos, acetamiprid and clothianidin;
preferably, the bactericide comprises: one or more of bupirimate, ethaboxam, dimethirimol, furazoles and copper sulfate;
preferably, the dispersant comprises: one or more of alkyl naphthalene sulfonate, organic phosphate, sodium lignin sulfonate, ethoxylated fatty alcohol;
preferably, the wetting agent comprises: one or more of disodium methylenedinaphthyl sulfonate, benzenesulfonate, sodium xylenesulfonate, sodium tetradecene sulfonate, sodium lauryl sulfate;
preferably, the disintegrant: one or more of ammonium sulfate, calcium chloride, anhydrous sodium sulfate, sodium carboxymethyl cellulose and polyethyl acrylate;
preferably, the filler comprises: one or more of bentonite, diatomite and activated carbon powder.
The beneficial effects obtained by the invention are as follows: according to the invention, nano-particles MOF-3 are prepared by a hydrothermal method, and the amino groups of the MOF-3 are chemically crosslinked with the sulfonic groups of the sodium lignin sulfonate, so that the MOF-3@sodium lignin sulfonate double-layer composite nano-carrier is successfully prepared, and the nano-carrier has higher pesticide loading capacity and good slow release effect, can promote pesticide application reduction and synergy, and reduces environmental pollution; in the invention, carboxyl of herbicide 2,4-D is covalently connected with alcoholic hydroxyl on photoinduced rupture group 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin methylene to form herbicide active ingredient compound, meanwhile, 2,4-D is connected into MOF-3 nano particles through coordination of phenolic hydroxyl of 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin and zirconium ion, under the stimulation of ultraviolet light, the 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin group in the compound absorbs photon energy, C-O at methylene on coumarin group breaks, namely C-O connected with 2,4-D covalently breaks, and 2,4-D carboxylic acid anion pair is released to generate corresponding 2,4-D to be released; through chemical crosslinking of sulfonic groups of sodium lignin sulfonate and amino groups on MOF-3 organic ligands, sodium lignin sulfonate is coated on the surfaces of MOF-3 nano particles loaded with weeding active ingredients, and ammonium sulfate is loaded on a porous structure on lignin through physical adsorption, so that the synergistic effect of 2,4-D and ammonium sulfate can be realized, sodium lignin sulfonate hydrogel has flexibility and adhesiveness, the attaching time and attaching strength of nano particles on the surfaces of leaves can be increased, the MOF-3 nano particles are prevented from drifting due to the influence of field environment, the effective time of 2,4-D is further prolonged, the waxy structure on the surfaces of the leaves can be damaged by ammonium sulfate, and the absorption of 2,4-D by weeds is promoted; the pesticide fertilizer compound provided by the invention has good weed control effect, the preparation method is simple, the cost is low, the release rate of herbicide can be effectively controlled, the action time is prolonged, the loss caused by volatilization and degradation is reduced, and the environmental pollution is reduced.
Drawings
FIG. 1 is a scanning electron microscope image of a MOF-3@sodium lignin sulfonate double-layer composite nano carrier prepared in step S5 in example 1 of the invention.
FIG. 2 is a graph showing the result of light-controlled slow release of the active ingredient-supporting nanocarriers prepared in examples 1 to 3, comparative example 1 and comparative example 2 according to the present invention.
FIG. 3 is a graph showing evaluation of safety of pesticide fertilizer compositions prepared in examples 1 to 3, comparative example 1 and comparative example 2 according to the present invention on wheat seedlings.
FIG. 4 is a graph showing the effect of crop growth of the pesticidal fertilizer compositions prepared in examples 1 to 3, comparative example 1 and comparative example 2 according to the present invention.
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described 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.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present invention. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the scope of the present application.
The experimental methods in the following examples are all conventional methods unless otherwise specified; the test materials and test strains used in the examples described below, unless otherwise specified, were commercially available.
Example 1
The pesticide fertilizer composition with the weeding effect comprises the following components in parts by weight: 25 parts of functional herbicide, 5 parts of pesticide, 5 parts of bactericide, 30 parts of fertilizer, 5 parts of dispersing agent, 1 part of wetting agent, 0.5 part of disintegrating agent, 3 parts of filler and 50 parts of deionized water.
The preparation method of the functional herbicide specifically comprises the following steps:
s1, adding 3mmol of octahydrated zirconium oxychloride into 120mLN, N-dimethylformamide, carrying out ultrasonic oscillation for 45min, adding 2mmol of 2-amino terephthalic acid, carrying out ultrasonic oscillation for 30min, adding 8mL of formic acid into the solution, stirring at room temperature for 30min, transferring the mixed solution into a reaction kettle, heating at 120 ℃ for 2 days, cooling to room temperature after the reaction is finished, filtering, collecting crystals, washing with N, N-dimethylformamide for 5 times, washing with acetone to remove residual N, N-dimethylformamide, and carrying out vacuum drying at 120 ℃ for 48 hours in a vacuum drying oven to obtain MOF-3 nano particles;
s2, 3 mmole of 2,4-D is dissolved in 50 mmole of N-dimethylformamide, 3 mmole of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 3.9 mmole of 1-hydroxybenzotriazole are added, stirring is carried out for 30min under ice bath, 4.5 mmole of 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin is added, reaction is carried out for 12h at room temperature, water and ethyl acetate are added after the reaction is finished, the organic layer is dried and concentrated, and column chromatography is carried out, so that a compound formed by covalently connecting the herbicidal active ingredients 2,4-D and 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin is obtained;
s3, adding the weeding active ingredient obtained in the step S2 into 10mL of ethanol to form 5mg/mL of ethanol solution, stirring uniformly at room temperature, adding 16mg of MOF-3 nano particles prepared in the step S1, heating to 45 ℃, reacting for 3 hours, washing the product with ethanol for 3 times, and vacuum drying for 5 hours at 50 ℃ in a vacuum drying oven to obtain MOF-3 nano particles loaded with weeding active molecules;
s4, adding 30mg of MOF-3 nano particles loaded with the herbicide active molecules and prepared in the step S3 into 5mL of sodium lignin sulfonate aqueous solution with the concentration of 9mg/mL, adding 15mg of glacial acetic acid, stirring for 1.5h at room temperature, centrifuging, washing with deionized water, and drying to obtain the MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with the herbicide active components;
s5, dissolving 20mg of the MOF-3@sodium lignin sulfonate double-layer composite nano carrier prepared in the step S4 into 3mL of ammonium sulfate aqueous solution with the concentration of 10mg/mL, stirring for 3 hours at room temperature, centrifuging after the reaction is finished, washing with deionized water, and vacuum drying for 6 hours at 70 ℃ in a vacuum drying oven to obtain the MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with the weeding active ingredients and ammonium sulfate.
The invention also provides a preparation method of the pesticide fertilizer composition with the weeding effect, which comprises the following specific steps: weighing functional herbicide, fertilizer, pesticide, bactericide, dispersing agent, wetting agent, disintegrating agent and filler according to parts by weight, uniformly stirring in water, grinding in a sand mill, spray drying, and screening to obtain the pesticide fertilizer composition with weeding effect.
Example 2
The pesticide fertilizer composition with the weeding effect comprises the following components in parts by weight: 35 parts of functional herbicide, 10 parts of pesticide, 7 parts of bactericide, 40 parts of fertilizer, 10 parts of dispersing agent, 2 parts of wetting agent, 2 parts of disintegrating agent, 7 parts of filler and 60 parts of deionized water.
The preparation method of the functional herbicide specifically comprises the following steps:
s1, adding 3mmol of zirconium oxychloride octahydrate into 150mLN, N-diethyl formamide, carrying out ultrasonic oscillation for 45min, adding 1.5mol of 2-amino terephthalic acid, carrying out ultrasonic oscillation for 30min, adding 9mL of formic acid into the solution, stirring at room temperature for 30min, transferring the mixed solution into a reaction kettle, heating at 135 ℃ for 2.5 days, cooling to room temperature after the reaction is finished, filtering, collecting crystals, washing with N, N-diethyl formamide for 5 times, washing with acetone to remove residual N, N-diethyl formamide, and carrying out vacuum drying at 120 ℃ for 48 hours in a vacuum drying oven to obtain MOF-3 nano particles.
S2, 3 mmole of 2,4-D is dissolved in 55 mmole of N-diethyl formamide, 3 mmole of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 3.9 mmole of 1-hydroxybenzotriazole are added, stirring is carried out for 30min under ice bath, 5.1 mmole of 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin is added, reaction is carried out for 12h at room temperature, water and ethyl acetate are added after the reaction is finished, the organic layer is dried and concentrated, and column chromatography is carried out, so that a compound formed by covalently connecting the herbicidal active ingredients 2,4-D and 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin is obtained.
S3, adding the weeding active ingredient obtained in the step S2 into 10mL of ethanol to form 7mg/mL of ethanol solution, stirring uniformly at room temperature, adding 18mg of MOF-3 nano particles prepared in the step S1, heating to 45 ℃, reacting for 3 hours, washing the product with ethanol for 3 times, and vacuum drying for 5 hours at 50 ℃ in a vacuum drying oven to obtain MOF-3 nano particles loaded with weeding active molecules.
S4, adding 50mg of MOF-3 nano particles loaded with the herbicide active molecules and prepared in the step S3 into 7mL of sodium lignin sulfonate aqueous solution with the concentration of 15mg/mL, adding 30mg of glacial acetic acid, stirring for 1.5h at room temperature, centrifuging, washing with deionized water, and drying to obtain MOF-3@sodium lignin sulfonate double-layer composite nano particles loaded with the herbicide active components.
S5, dissolving 30mg of the MOF-3@sodium lignin sulfonate double-layer composite nano carrier prepared in the step S4 into 4mL of ammonium sulfate aqueous solution with the concentration of 12mg/mL, stirring for 3 hours at room temperature, centrifuging after the reaction is finished, washing with deionized water, and vacuum drying for 6 hours at 70 ℃ in a vacuum drying oven to obtain the MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with the weeding active ingredients and ammonium sulfate.
The present invention also provides a method for preparing a pesticidal fertilizer composition having herbicidal effect, which is different from example 1 in the parts by weight of the respective components.
Example 3
The pesticide fertilizer composition with the weeding effect comprises the following components in parts by weight: 40 parts of functional herbicide, 15 parts of pesticide, 10 parts of bactericide, 50 parts of fertilizer, 15 parts of dispersing agent, 3 parts of wetting agent, 3 parts of disintegrating agent, 10 parts of filler and 70 parts of deionized water.
The preparation method of the functional herbicide specifically comprises the following steps:
s1, adding 3mmol of zirconium oxychloride octahydrate into 165mLN, N-dimethylformamide, carrying out ultrasonic oscillation for 45min, adding 1mmol of 2-amino terephthalic acid, carrying out ultrasonic oscillation for 30min, adding 8mL of formic acid into the solution, stirring at room temperature for 30min, transferring the mixed solution into a reaction kettle, heating at 150 ℃ for 3 days, cooling to room temperature after the reaction is finished, filtering, collecting crystals, washing with N, N-dimethylformamide for 5 times, washing with acetone to remove residual N, N-dimethylformamide, and carrying out vacuum drying at 120 ℃ for 48 hours in a vacuum drying oven to obtain MOF-3 nano particles.
S2, 3mmol of 2,4-D is dissolved in 60mLN, N-dimethylformamide, 3mmol of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 3.9mmol of 1-hydroxybenzotriazole are added, stirring is carried out for 30min under ice bath, 6mmol of 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin is added, reaction is carried out for 12h at room temperature, water and ethyl acetate are added after the reaction is finished, the organic layer is dried and concentrated, and column chromatography is carried out, so that a compound formed by covalently connecting the herbicidal active ingredient 2,4-D and the 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin is obtained.
S3, adding the weeding active ingredient obtained in the step S2 into 10mL of ethanol to form 10mg/mL of ethanol solution, stirring uniformly at room temperature, adding 20mg of MOF-3 nano particles prepared in the step S1, heating to 45 ℃, reacting for 3 hours, washing the product with ethanol for 3 times, and vacuum drying for 5 hours at 50 ℃ in a vacuum drying oven to obtain MOF-3 nano particles loaded with weeding active molecules.
S4, adding 50mg of MOF-3 nano particles loaded with the herbicide active molecules and prepared in the step S3 into 10mL of sodium lignin sulfonate aqueous solution with the concentration of 15mg/mL, adding 35mg of glacial acetic acid, stirring for 1.5h at room temperature, centrifuging, washing with deionized water, and drying to obtain the MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with the herbicide active components.
S5, dissolving 30mg of the MOF-3@sodium lignin sulfonate double-layer composite nano carrier prepared in the step S4 into 6mL of ammonium sulfate aqueous solution with the concentration of 15mg/mL, stirring for 3 hours at room temperature, centrifuging after the reaction is finished, washing with deionized water, and vacuum drying for 6 hours at 70 ℃ in a vacuum drying oven to obtain the MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with the weeding active ingredients and ammonium sulfate.
The present invention also provides a method for preparing a pesticidal fertilizer composition having herbicidal effect, which is different from example 1 in the parts by weight of the respective components.
Comparative example 1
This comparative example a pesticide fertilizer composition was prepared, which differs from example 1 in that: in the functional herbicide described in this comparative example, the herbicidal active ingredient was only 2,4-D, and the preparation method of this comparative example did not include step S2 of example 1.
Comparative example 2
This comparative example a pesticide fertilizer composition was prepared, which differs from example 1 in that: in the functional herbicide of the comparative example, the MOF-3 nanoparticle is not coated with sodium lignin sulfonate, and the preparation method of the comparative example does not comprise steps S4 and S5 of example 1.
Comparative example 3
This comparative example, which is different from example 1 in that a pesticidal fertilizer composition having a herbicidal effect was prepared: in the functional herbicide of the comparative example, the herbicidal active ingredient was only 2,4-D, and the MOF-3 nanoparticle was not coated with sodium lignin sulfonate, and the preparation method of the comparative example did not include steps S2, S4 and S5 of example 1.
Experimental example 1
The MOF-3@sodium lignin sulfonate double-layer composite nano carrier prepared in the step S5 in the embodiment 1 is firstly and uniformly dispersed by ethanol in an ultrasonic manner, then a sample suspension is dripped on an aluminum foil, fixed on a conductive adhesive, and morphology analysis is carried out by adopting a scanning electron microscope; FIG. 1 is a scanning electron microscope image of a MOF-3@sodium lignin sulfonate double-layer composite nano carrier prepared in step S5 in example 1 of the invention, and it can be seen from the image that MOF-3 and sodium lignin sulfonate are chemically crosslinked, and the surface of MOF-3 nano particles is coated by natural polymers with irregular morphology, so that a uniform and compact whole is formed.
Experimental example 2
In the test example, the pesticide fertilizer compositions described in the examples and the comparative examples were subjected to a light response release test, in which 20mg of the functional herbicide prepared in the invention examples 1 to 3 and the functional herbicide prepared in the invention examples 1 to 3 were accurately weighed at room temperature, dispersed in 100mL of a medium of methanol/water (25:75, v/v), and after ultrasonic dispersion, the functional herbicide was placed on a magnetic stirrer with a rotation speed of 200rpm, and subjected to ultraviolet light (ultraviolet lamp 365nm, 0.4W/cm) 2 ) Under the irradiation of the above, 1mL of solution supernatant was collected at a fixed time point, the same volume of culture solution was supplemented after each sampling, the obtained sample was centrifuged, the concentration of 2,4-D in the supernatant was measured, and the system was calculatedThe cumulative release rate of 2,4-D in (2, 4-D) was calculated by using the following formula with the same culture release system under dark conditions as a negative control e ）：
N e =R t/ R 0 ；
Wherein: n (N) e To accumulate the release amount, R t R for releasing the amount of 2,4-D in the culture broth 0 The total amount of 2,4-D in the obtained MOF-3@lignin double-layer composite nano carrier is calculated.
FIG. 2 is a graph showing the light-operated slow release results of the nano-carriers loaded with the active ingredients prepared in examples 1-3 and comparative examples 1-3, wherein the MOF-3@sodium lignin sulfonate double-layer composite nano-carrier loaded with the herbicidal active ingredients prepared in examples 1-3 shows good light-operated slow release performance under ultraviolet irradiation, acid or alkali accelerates ester bond hydrolysis, and under the condition of nearly neutral pH, 2,4-D release is much slower, meanwhile, the release time of the active ingredients can be effectively prolonged by coating the sodium lignin sulfonate hydrogel, and 2,4-D in examples 1-3 starts to be released after 3 hours of illumination, and the accumulated release amount of 2,4-D is more than 90% after 96 hours; the active weeding component of the comparative example 1 is only 2,4-D, and compared with the active weeding component of the examples 1-3, the release rate of the 2,4-D in the comparative example 1 is faster, the cumulative release rate of the 2,4-D after 20 hours is about 50%, and better control release is not realized, so that the photo-induced breaking group plays an important role in the 2,4-D control release process; comparative example 2 is MOF-3 single-layer nano-carrier with the outer layer not encapsulating sodium lignin sulfonate, compared with examples 1-3, the release time of 2,4-D in comparative example 2 is advanced, and the cumulative release rate of 2,4-D after 20 hours exceeds 70%, which indicates that lignin hydrogel is encapsulated on the outer layer of MOF-3 to effectively prolong the 2,4-D slow release time; in comparative example 3, the photosensitive group is not connected, and the outer layer of the nanoparticle is not coated with sodium lignin sulfonate, the overall release rate of comparative example 3 is fastest, the 2,4-D cumulative release rate is close to 90% after 5 hours, and the slow release effect is poor compared with other examples and comparative examples in the light-controlled slow release process.
Experimental example 3
The pesticide fertilizer compound prepared in the example and the comparative example is subjected to safety evaluation through an indoor wheat potting experiment, and test wheat seeds with uniform and full size are selectedSterilizing with sodium hypochlorite solution, washing with distilled water for several times, soaking for 12 hr, sowing seeds into plastic flowerpot, sowing 5 seeds per pot, covering soil for 1cm, moistening soil completely, culturing in greenhouse, and spraying pesticide fertilizer composition 35mg/m in liquid medicine with small-sized quantitative sprayer after seeds emerge and 1 pair of true leaves grow 2 Spraying the stem and leaf after seedling, spraying water as blank control, spraying medicine for 3D and 7D, and measuring 2,4-D concentration on the stem and leaf by high performance liquid chromatography.
FIG. 3 is a graph showing the evaluation of the safety of the pesticide fertilizer composition prepared in examples 1-3 and comparative examples 1-3 on wheat seedlings, wherein after 3D of pesticide spraying, the residual concentration of the example 1-3 on the stems and leaves of the wheat seedlings is about 0.4mg/kg, which is lower than that of the comparative examples 1-3, and the functional herbicide prepared in the example has better slow release effect, so that the release time of 2,4-D is prolonged, and the residual concentration on the stems and leaves of crops is lower; after 7D of spraying, the stem and leaf concentration of the embodiment 1-3 is very similar to that of the embodiment 3D, and the 2,4-D slow release rate of the embodiment 1-3 is slower and is not easy to be absorbed by the stem and leaf of crops; the concentration of 2,4-D in the stems and leaves after 7D of the comparative examples 1-3 is obviously lower than 3D, and the release rate of 2,4-D in the slow release process is faster and is easier to be absorbed by the stems and leaves of crops due to the lack of photosensitive groups or sodium lignin sulfonate hydrogel in the structures of the comparative examples 1-3; in summary, examples 1-3 have good safety for the growth of wheat seedlings.
Experimental example 4
Taking a corn field as a test field, adopting a seedling transplanting mode, arranging 6 medicament treatment areas and 1 clear water comparison area in the corn field, wherein the area of each treatment area is 20m 2 The pesticide fertilizer composition is sprayed on the surfaces of the stems and leaves of the corns for 1 time according to the test design in 7-8 leaf stage and 2-5 leaf stage of the corns, the pesticide liquid is uniformly sprayed on the surfaces of the stems and leaves of the weeds, and the dosage of the pesticide fertilizer composition in the pesticide liquid is 51.5g/hm 2 Wherein, the control group is to spray the same amount of clear water; randomly selecting and fixing 3 sample formulas in each treatment area for investigation and sampling of weed control effect, randomly selecting 10 corn plants in each treatment area 45d after application, measuring the plant height, and simultaneously, when 85d crops are harvested after application, singly selecting the corn plants in each treatment areaThe fresh weight of the corn ear bud is recorded independently, the yield is converted, and compared with a clear water control group, the yield is calculated according to the following formula:
S/%=(O T −O C )/O C ×100；
wherein S represents an increased yield; o (O) T Representing process throughput; o (O) C The control yields are indicated.
FIG. 4 is a graph showing the effect of the pesticide-fertilizer compositions prepared in examples 1-3 and comparative examples 1-3 on corn yield in test fields, wherein the corn plant heights in each treatment area are significantly higher than that of the clear water control without grass when measured 50d after application, the pesticide-fertilizer compositions prepared in examples 1-3 are higher in plants treated with the pesticide-fertilizer compositions, the plant height increase range is about 5-9cm, and the pesticide-fertilizer compositions prepared in examples 1-3 have yield increasing effects on corn, and the yield increases are 16.21%, 17.45% and 15.76% respectively, so that the pesticide-fertilizer compositions prepared in examples 1-3 can obviously promote crop growth; the pesticide fertilizer compound prepared in the comparative examples 1-3 can also increase the plant height and the yield of corn in a test field, and the increased yield is respectively 10.82%, 11.79% and 9.55%, compared with the pesticide fertilizer compound prepared in the comparative examples 1-3, the promotion effect on the corn growth is lower than that of the pesticide fertilizer compound prepared in the examples 1-3, which indicates that the nano slow-release carrier prepared in the examples 1-3 plays an important role in the crop growth process.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
The invention and its embodiments have been described above with no limitation, and the invention is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the invention can be practiced without the specific details disclosed herein.
Claims (10)
1. A pesticide fertilizer composition with weeding effect is characterized in that: the pesticide fertilizer composition comprises the following components in parts by weight: 25-40 parts of functional herbicide, 5-15 parts of pesticide, 5-10 parts of bactericide, 30-50 parts of fertilizer, 5-15 parts of dispersing agent, 1-3 parts of wetting agent, 0.5-3 parts of disintegrating agent, 3-10 parts of filler and 50-70 parts of deionized water; the functional herbicide is a MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with a weeding active ingredient and ammonium sulfate; the weeding active ingredient is a compound formed by covalently connecting 2,4-D and 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin.
2. A pesticidal fertilizer composition having herbicidal effect according to claim 1, characterized in that: the fertilizer comprises: urea, potassium chloride, humic acid, compound amino acid, potassium magnesium sulfate; the pesticide comprises: one or more of abamectin, carbofuran, methyl pyrifos, acetamiprid and clothianidin; the bactericide comprises: one or more of bupirimate, ethaboxam, dimethirimol, furazoles and copper sulfate; the dispersant comprises: one or more of alkyl naphthalene sulfonate, organic phosphate, sodium lignin sulfonate, ethoxylated fatty alcohol; the wetting agent comprises: one or more of disodium methylenedinaphthyl sulfonate, benzenesulfonate, sodium xylenesulfonate, sodium tetradecene sulfonate, sodium lauryl sulfate; the disintegrating agent: one or more of ammonium sulfate, calcium chloride, anhydrous sodium sulfate, sodium carboxymethyl cellulose and polyethyl acrylate; the filler comprises: one or more of bentonite, diatomite and activated carbon powder.
3. A method for preparing the pesticidal fertilizer composition having herbicidal effect as defined in claim 1 or 2, characterized in that: weighing functional herbicide, fertilizer, pesticide, bactericide, dispersing agent, wetting agent, disintegrating agent and filler, stirring uniformly in water, grinding in a sand mill, spray drying, and sieving to obtain the pesticide fertilizer composition with weeding effect.
4. A method for preparing a pesticidal fertilizer composition having herbicidal effect according to claim 3, characterized in that: the preparation method of the functional herbicide specifically comprises the following steps:
s1, adding zirconium oxychloride octahydrate into N, N-dimethylformamide, carrying out ultrasonic oscillation for 45min, adding 2-amino terephthalic acid, carrying out ultrasonic oscillation for 30min, adding formic acid into the solution, stirring for 30min at room temperature, transferring the mixed solution into a reaction kettle, reacting for 2-3 days under the heating condition of 120-150 ℃, cooling to room temperature after the reaction is finished, filtering, collecting crystals, washing with N, N-dimethylformamide for 5 times, washing with acetone to remove residual N, N-diethylformamide, and carrying out vacuum drying for 48 hours in a vacuum drying box at 120 ℃ to obtain MOF-3 nano particles;
s2, dissolving 2,4-D in N, N-dimethylformamide, adding a catalyst of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 1-hydroxybenzotriazole, stirring for 30min under ice bath, adding 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin, reacting at room temperature for 12h, adding water and ethyl acetate for extraction after the reaction is finished, drying an organic layer, concentrating, and performing column chromatography to obtain a weeding active ingredient;
s3, adding the weeding active ingredient prepared in the step S2 into an ethanol solution, stirring uniformly at room temperature, adding the MOF-3 nano particles prepared in the step S1, heating to 45-60 ℃, reacting for 3-5h, washing the product with ethanol for 3 times, and vacuum drying for 5h at 50 ℃ in a vacuum drying oven to obtain MOF-3 nano particles loaded with the weeding active ingredient;
s4, adding the MOF-3 nano particles loaded with the weeding active ingredients prepared in the step S3 into a sodium lignin sulfonate aqueous solution, adding glacial acetic acid, stirring for 1.5-3 hours at room temperature, centrifuging, washing with deionized water, and drying to obtain the MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with the weeding active ingredients;
s5, dissolving the MOF-3@sodium lignin sulfonate double-layer composite nano carrier prepared in the step S4 in an ammonium sulfate aqueous solution, stirring for 3-5 hours at room temperature, centrifuging after the reaction is finished, washing with deionized water, and vacuum drying for 6 hours at 70 ℃ in a vacuum drying oven to obtain the MOF-3@sodium lignin sulfonate double-layer composite nano carrier loaded with the weeding active ingredients and ammonium sulfate.
5. The method for producing a pesticidal fertilizer composition having herbicidal effect according to claim 4, characterized in that: in S1, the molar concentration of zirconium oxychloride octahydrate in N, N-dimethylformamide is: 18-25mmol/L; the molar ratio of zirconium oxychloride octahydrate to 2-amino terephthalic acid is: 1.5-3:1; the volume ratio of the N, N-dimethylformamide to the formic acid is as follows: 15-20:1.
6. The method for producing a pesticidal fertilizer composition having herbicidal effect according to claim 5, characterized in that: in S2, the molar concentration of 2,4-D in N, N-dimethylformamide is: 50-60mmol/L.
7. The method for producing a pesticidal fertilizer composition having herbicidal effect according to claim 6, characterized in that: in S2, the molar ratio of 2,4-D to 6-bromo-7-hydroxy-4- (hydroxymethyl) coumarin, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 1-hydroxybenzotriazole is: 1:1.5-2:1:1.3.
8. The method for producing a pesticidal fertilizer composition having herbicidal effect according to claim 7, characterized in that: in S3, the concentration of the herbicidal active ingredient in the ethanol solution is: 5-10mg/mL; the mass ratio of the weeding active ingredient to the MOF-3 nano particles is as follows: 3-5:1.
9. The method for producing a pesticidal fertilizer composition having herbicidal effect according to claim 8, characterized in that: in S4, the concentration of the sodium lignin sulfonate aqueous solution is: 9-20mg/mL; the mass ratio of the MOF-3 nano particles loaded with the weeding active ingredients to the sodium lignin sulfonate is as follows: 1:1.5-3; the mass ratio of the MOF-3 nano particles loaded with the weeding active ingredient to glacial acetic acid is as follows: 1:0.5-0.7.
10. The method for producing a pesticidal fertilizer composition having herbicidal effect according to claim 9, characterized in that: in S5, the concentration of the ammonium sulfate aqueous solution is 10-15mg/mL; the mass ratio of the MOF-3@sodium lignin sulfonate double-layer composite nano carrier to the ammonium sulfate is 1:1.5-3.5.
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