CN106857557A - A kind of Synergistic mite killing composition of the mite of pyrrole containing nitrile ester - Google Patents
A kind of Synergistic mite killing composition of the mite of pyrrole containing nitrile ester Download PDFInfo
- Publication number
- CN106857557A CN106857557A CN201710088569.1A CN201710088569A CN106857557A CN 106857557 A CN106857557 A CN 106857557A CN 201710088569 A CN201710088569 A CN 201710088569A CN 106857557 A CN106857557 A CN 106857557A
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- CN
- China
- Prior art keywords
- grams
- tdca
- thiadiazoles
- bases
- nitrile pyrrole
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 title claims abstract description 258
- 239000000203 mixture Substances 0.000 title claims abstract description 121
- 230000002195 synergetic effect Effects 0.000 title abstract description 12
- -1 nitrile ester Chemical class 0.000 title description 24
- 150000002148 esters Chemical class 0.000 claims abstract description 127
- 150000002825 nitriles Chemical class 0.000 claims abstract description 127
- BHTRKEVKTKCXOH-UHFFFAOYSA-N Taurochenodesoxycholsaeure Natural products OC1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(=O)NCCS(O)(=O)=O)C)C1(C)CC2 BHTRKEVKTKCXOH-UHFFFAOYSA-N 0.000 claims abstract description 13
- AWDRATDZQPNJFN-VAYUFCLWSA-N taurodeoxycholic acid Chemical compound C([C@H]1CC2)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(=O)NCCS(O)(=O)=O)C)[C@@]2(C)[C@@H](O)C1 AWDRATDZQPNJFN-VAYUFCLWSA-N 0.000 claims abstract description 13
- 229950005578 tidiacic Drugs 0.000 claims abstract description 13
- 239000003905 agrochemical Substances 0.000 claims abstract description 12
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims abstract description 12
- 239000004480 active ingredient Substances 0.000 claims abstract description 10
- 239000000642 acaricide Substances 0.000 claims description 67
- 239000004562 water dispersible granule Substances 0.000 claims description 46
- 150000001875 compounds Chemical class 0.000 claims description 34
- 238000009472 formulation Methods 0.000 claims description 31
- 239000003094 microcapsule Substances 0.000 claims description 30
- 238000002360 preparation method Methods 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 24
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- 241000196324 Embryophyta Species 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- 235000013399 edible fruits Nutrition 0.000 claims description 8
- 235000013311 vegetables Nutrition 0.000 claims description 8
- 239000004563 wettable powder Substances 0.000 claims description 8
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 6
- 244000105624 Arachis hypogaea Species 0.000 claims description 6
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 6
- 235000018262 Arachis monticola Nutrition 0.000 claims description 6
- 229920000742 Cotton Polymers 0.000 claims description 6
- 235000020232 peanut Nutrition 0.000 claims description 6
- 239000000575 pesticide Substances 0.000 claims description 5
- UGUHFDPGDQDVGX-UHFFFAOYSA-N 1,2,3-thiadiazole Chemical class C1=CSN=N1 UGUHFDPGDQDVGX-UHFFFAOYSA-N 0.000 claims description 2
- 241001454293 Tetranychus urticae Species 0.000 claims description 2
- 210000004209 hair Anatomy 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- FEYDZHNIIMENOB-UHFFFAOYSA-N 2,6-dibromopyridine Chemical compound BrC1=CC=CC(Br)=N1 FEYDZHNIIMENOB-UHFFFAOYSA-N 0.000 claims 2
- FILKGCRCWDMBKA-UHFFFAOYSA-N 2,6-dichloropyridine Chemical compound ClC1=CC=CC(Cl)=N1 FILKGCRCWDMBKA-UHFFFAOYSA-N 0.000 claims 2
- MBTGBRYMJKYYOE-UHFFFAOYSA-N 2,6-difluoropyridine Chemical compound FC1=CC=CC(F)=N1 MBTGBRYMJKYYOE-UHFFFAOYSA-N 0.000 claims 2
- 229910052731 fluorine Inorganic materials 0.000 claims 2
- 239000011737 fluorine Substances 0.000 claims 2
- JWTZSVLLPKTZJP-UHFFFAOYSA-N 2-bromo-6-chloropyridine Chemical class ClC1=CC=CC(Br)=N1 JWTZSVLLPKTZJP-UHFFFAOYSA-N 0.000 claims 1
- WAHFYBHQGSHRJD-UHFFFAOYSA-N 2-butyl-1,3,4-thiadiazole Chemical class CCCCC1=NN=CS1 WAHFYBHQGSHRJD-UHFFFAOYSA-N 0.000 claims 1
- 235000009917 Crataegus X brevipes Nutrition 0.000 claims 1
- 235000013204 Crataegus X haemacarpa Nutrition 0.000 claims 1
- 235000009685 Crataegus X maligna Nutrition 0.000 claims 1
- 235000009444 Crataegus X rubrocarnea Nutrition 0.000 claims 1
- 235000009486 Crataegus bullatus Nutrition 0.000 claims 1
- 235000017181 Crataegus chrysocarpa Nutrition 0.000 claims 1
- 235000009682 Crataegus limnophila Nutrition 0.000 claims 1
- 235000004423 Crataegus monogyna Nutrition 0.000 claims 1
- 240000000171 Crataegus monogyna Species 0.000 claims 1
- 235000002313 Crataegus paludosa Nutrition 0.000 claims 1
- 235000009840 Crataegus x incaedua Nutrition 0.000 claims 1
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 claims 1
- 241001454294 Tetranychus Species 0.000 claims 1
- 150000001409 amidines Chemical class 0.000 claims 1
- 229910052740 iodine Inorganic materials 0.000 claims 1
- 239000011630 iodine Substances 0.000 claims 1
- 230000001954 sterilising effect Effects 0.000 claims 1
- 238000004659 sterilization and disinfection Methods 0.000 claims 1
- 229930192474 thiophene Natural products 0.000 claims 1
- 230000008485 antagonism Effects 0.000 abstract description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 abstract description 3
- 238000009533 lab test Methods 0.000 abstract description 2
- 150000004867 thiadiazoles Chemical class 0.000 abstract 2
- OGVLEPMNNPZAPS-UHFFFAOYSA-N 2,3-difluoropyridine Chemical compound FC1=CC=CN=C1F OGVLEPMNNPZAPS-UHFFFAOYSA-N 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 55
- 239000000463 material Substances 0.000 description 40
- 230000000295 complement effect Effects 0.000 description 38
- 239000002202 Polyethylene glycol Substances 0.000 description 30
- 229920001223 polyethylene glycol Polymers 0.000 description 30
- 238000000034 method Methods 0.000 description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- 230000000895 acaricidal effect Effects 0.000 description 24
- 239000004576 sand Substances 0.000 description 24
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 23
- 239000012467 final product Substances 0.000 description 21
- 229920005610 lignin Polymers 0.000 description 21
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 20
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 20
- 239000000440 bentonite Substances 0.000 description 20
- 229910000278 bentonite Inorganic materials 0.000 description 20
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 20
- 238000005469 granulation Methods 0.000 description 20
- 230000003179 granulation Effects 0.000 description 20
- 229920000642 polymer Polymers 0.000 description 18
- 108010010803 Gelatin Proteins 0.000 description 17
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- 235000019322 gelatine Nutrition 0.000 description 17
- 235000011852 gelatine desserts Nutrition 0.000 description 17
- 229920001732 Lignosulfonate Polymers 0.000 description 16
- 239000000543 intermediate Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 14
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 14
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 14
- 239000000375 suspending agent Substances 0.000 description 14
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical class OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 12
- 235000001465 calcium Nutrition 0.000 description 12
- 230000000694 effects Effects 0.000 description 12
- 230000003449 preventive effect Effects 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 11
- 235000010489 acacia gum Nutrition 0.000 description 11
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 11
- 239000011575 calcium Substances 0.000 description 11
- 229910052791 calcium Inorganic materials 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- 239000012153 distilled water Substances 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 9
- 239000005995 Aluminium silicate Substances 0.000 description 8
- 235000012211 aluminium silicate Nutrition 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000010790 dilution Methods 0.000 description 7
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- 150000003871 sulfonates Chemical class 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 241000238876 Acari Species 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 6
- CKLJMWTZIZZHCS-REOHCLBHSA-L aspartate group Chemical group N[C@@H](CC(=O)[O-])C(=O)[O-] CKLJMWTZIZZHCS-REOHCLBHSA-L 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 6
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000006482 condensation reaction Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 239000003814 drug Substances 0.000 description 6
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 5
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
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- GHGZGDGWFWIAQM-UHFFFAOYSA-N 1,3,4-trimethylpyrazole Chemical compound CC1=CN(C)N=C1C GHGZGDGWFWIAQM-UHFFFAOYSA-N 0.000 description 4
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- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 102000019259 Succinate Dehydrogenase Human genes 0.000 description 1
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- MWSJNLRFKBWZRX-UHFFFAOYSA-N [N].C1=CSN=N1 Chemical class [N].C1=CSN=N1 MWSJNLRFKBWZRX-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 229940105329 carboxymethylcellulose Drugs 0.000 description 1
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- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000007265 chloromethylation reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
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- UXADOQPNKNTIHB-UHFFFAOYSA-N clofentezine Chemical compound ClC1=CC=CC=C1C1=NN=C(C=2C(=CC=CC=2)Cl)N=N1 UXADOQPNKNTIHB-UHFFFAOYSA-N 0.000 description 1
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- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000004533 oil dispersion Substances 0.000 description 1
- 239000002420 orchard Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000010627 oxidative phosphorylation Effects 0.000 description 1
- 235000021017 pears Nutrition 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 150000004714 phosphonium salts Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
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- 238000001556 precipitation Methods 0.000 description 1
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- 230000002335 preservative effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 150000003217 pyrazoles Chemical class 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
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- 241000894007 species Species 0.000 description 1
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- ZZYSLNWGKKDOML-UHFFFAOYSA-N tebufenpyrad Chemical compound CCC1=NN(C)C(C(=O)NCC=2C=CC(=CC=2)C(C)(C)C)=C1Cl ZZYSLNWGKKDOML-UHFFFAOYSA-N 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of Synergistic mite killing composition, with N (base of 51,3,4 thiadiazoles of the tert-butyl group 2) N'(2, the base of 6 difluoro pyridine 4) N, the carbonamidine of 41,2,3 thiadiazoles of dimethyl 5（TDCA‑10）It is that acceptable auxiliary element is collectively constituted in active ingredient, with agricultural chemicals with nitrile pyrrole mite ester, wherein TDCA 10 and nitrile pyrrole mite ester part by weight are 80:1 to 1:20.Tested by laboratory experiment and field efficacy, shown after two kinds of combination of active principles without antagonism, and with notable synergistic effect, to crop safety.
Description
Technical field
The present invention relates to a kind of insecticide acaricide composition, concretely relate to a kind of mite ester of pyrrole containing nitrile and the substitutions of N- tri--
The insecticide acaricide composition of 1,2,3- thiadiazoles -5- formamidine compounds, belongs to field of pesticide preparation.
Background technology
Mite class belongs to Arthropoda, and Arachnoidea, Acarina is individual smaller.All ranks are there may be in a colony
The mite of section, including ovum, deutonymph, young mite and into mite.It is mostly intensive to infest fruit tree, vegetables, cotton, peanut and other crops and view and admire plant
The vacuum side of blade of thing, and its breeding is rapid, high these of selfing degree all determine the more difficult preventing and treating of mite class.On the other hand, Nong Minyou
The continuous single acaricide good using miticidal effect of custom, as a result causes acarid that resistance is produced within many time and profit is lost
With value.Therefore, using the different mechanisms of action, different types of acaricide be solve evil mite be also easy to produce resistance effective way it
One.
Nitrile pyrrole mite ester chemical formula C24H31N3O2, CAS accession number 560121-52-0, chemical structural formula is shown below（Formula
1）, English abbreviation Cyenopyrafen, the novel pyrazoles acaricide released in 2009 by the Nissan Chemical company of Japan, and
Registered in Japan and South Korea in the same year.Entitled (E) -2- (the 4-tert-butylphenyl) -2-cyano- of English language Chemical
1-(1,3,4-trim -ethylpyrazol-5-yl)vinyl-2,2-dimethylpropionate.Chinese chemical name
(E) -2- (4- tert-butyl-phenyls) -2- cyano group -1- (1,3,4- trimethylpyrazol -5- bases) alkenyl -2,2- dimethyl propylene acid esters.System
Agent single dose trade name：Starmite, preparation mixture（With the mixture of pyridaben）Trade name：Valuestar.Obtained since 2009
After formal registration, sales volume goes up year by year, and ten million dollar is reached with the sales volume of pyridaben mixture in nitrile pyrrole mite ester in 2010.
Nitrile pyrrole mite ester active compound sterling is white solid, 106.7 ~ 108.2 DEG C of fusing point.Nitrile pyrrole mite ester vapour pressure 5.2 × 10-4 MPa(25
DEG C), relative density 1.11 (20 DEG C).Water is insoluble in, solubility (20 DEG C) 0.30 mg/L in water.Stability in air：
Stabilization in 14 d at 54 DEG C.Nitrile pyrrole mite ester mechanism of action is commonly referred to be:Nitrile pyrrole mite this life of ester does not prevent and treat acarid work
With, but nitrile pyrrole mite ester is by metabolism（There are ester hydrolysis in animal body and form hydroxy compounds）, change into hydroxy compound
Thing（Formula 2）.This hydroxy compounds suppresses line on respiratory electron transport chain by upsetting Complex II (succinate dehydrogenase)
Normal effect of plastochondria, destroys oxidative phosphorylation process, reaches preventive and therapeutic effect.The pharmacy effect mechanism is novel, it is contemplated that with it is current
The main insecticidal/acaricidal agent no interactions resistance for using.Nitrile pyrrole mite ester can be used to prevent and treat all kinds of evil mites on fruit tree, tealeaves, vegetables.
Indoor is 2.5 mg/L to Tetranychus cinnabarinus spraying treatment concentration, and the death rate can reach 100%.Field test shows that nitrile pyrrole mite ester makes
During with concentration for 50 mg/L, preventive effect is up to 98.74%.Active compound acute toxicity：Rat acute LD50The mg/kg of ＞ 5 000.
The percutaneous LD of rat acute50The mg/kg of ＞ 5000.Rat sucks LC50(4 h) ＞ 5.01 mg/L.Ecotoxicological：To Bobwhite urgency
The oral LD of property50The mg/kg of ＞ 2 000；Rainbow trout LC50(96 h)18.3 μg/L.To Predatory Mites, green under 15 g/100 L
Color lacewing, flower bedbug, honeybee and hornet are non-toxic.Environment degradable：The medicament does not have bioconcentration, in animal body
It is interior mainly to pass through dejection degradation (degraded 95% ~ 99% in about 120 h)；Slowly degraded in plant.Can in soil and water
Rapid degraded, the DT in the soil of field50It is 2 ~ 5 d, DT90It is 5 ~ 15 d.Cyenopyrafen can effectively control fruit, oranges and tangerines,
Various evil mites on tealeaves, vegetables, foliage-spray.Interior shows Tetranychus cinnabarinus toxicity test result nitrile pyrrole mite ester
（Cyenopyrafen）With acaricidal activity very high, and acaricidal activity is higher than its Z formula isomers.Field checking test result table
Bright nitrile pyrrole mite ester has preferable quick-acting and lasting effect under 50 mg/L to citrus red mite.As people are to environment, agricultural production
The increasingly raising of product safety requirements, the upgrading of Pesticidal products is also progressively accelerated, domestic some old acaricide kinds (such as three
Chlorbenside alcohol and Spanon etc.) be prohibited from using due to its security and resistance problem, and security is of a relatively high, preventive effect more
Good acaricide (such as tebufenpyrad, pyridaben and clofentezine) kind, also because of long-term use, resistance problem is also different degrees of
Manifest.Although also there is new acaricide to research and develop in recent years, because mite class is the harmful thing of easily generation resistance, therefore difference is needed
The acaricide of mechanism of action is used alternatingly.The features such as nitrile pyrrole mite ester has low toxicity, low consumption and wide mite killing spectrum, can be acaricide
Kind is used alternatingly there is provided a kind of new selection.And its novel mechanism of action, more can effectively prevent and treat the danger of resistance evil mite
Evil.
Nitrile pyrrole mite Lipase absobed route report is more, and representative synthetic route has following several.Route one：Oxalic acid two
Ethyl ester is that initiation material carries out condensation reaction generation acetopyruvic acid ethylester, the acetopyruvic acid ethylester intermediate for obtaining with acetone
Condensation ring closure reaction is carried out with hydrazine hydrate again and obtains 3- methylpyrazole -5- Ethyl formates, in the middle of 3- methylpyrazole -5- Ethyl formates
Body carries out methylation reaction with dimethyl suflfate and obtains 1,3- dimethyl pyrazole -5- Ethyl formates again, and the intermediate carries out chlorine again
Methylation reaction obtains 1,3- dimethyl -4- chloromethyl pyrazole-5-ethyl formates, 1,3- dimethyl -4- chloromethyl pyrazoles -5- first
Acetoacetic ester intermediate carries out palladium carbon hydrogenation reduction and obtains 1,3,4- trimethylpyrazol -5- Ethyl formates, 1,3,4- front three again
Base pyrazole-5-ethyl formate intermediate again with condensation reaction carried out under basic conditions to tert-butyl benzene acetonitrile obtain hydroxy
Nitrile intermediate, hydroxy nitrile intermediate, then carry out esterification with pivaloyl chloride and finally give nitrile pyrrole mite ester.The conjunction of route two
It is similar with route one into method general thought, simply slightly have difference in the synthesis of indivedual intermediates, its route is summarized as follows：Grass
Diethyl phthalate is that initiation material carries out condensation reaction generation acetopyruvic acid ethylester with acetone, in the acetopyruvic acid ethylester for obtaining
Mesosome carries out condensation ring closure reaction with hydrazine hydrate and obtains 3- methylpyrazole -5- Ethyl formates, 3- methylpyrazole -5- Ethyl formates again
Intermediate carries out methylation reaction with dimethyl suflfate and obtains 1,3- dimethyl pyrazole -5- Ethyl formates again, and the intermediate enters again
Row chloromethylation obtains 1,3- dimethyl -4- chloromethyl pyrazole-5-ethyl formates, and 1,3- dimethyl -4- chloromethyls pyrazoles -
5- Ethyl formates intermediate carries out palladium carbon hydrogenation reduction and obtains 1,3,4- trimethylpyrazol -5- Ethyl formates, 1,3,4- again
Trimethylpyrazol -5- Ethyl formates intermediate obtains 1,3,4- trimethylpyrazol -5- formic acid, 1,3,4- trimethyl pyrrole by hydrolysis
Azoles -5- carboxylic acid intermediates obtain 1,3,4- trimethylpyrazol -5- formyl chloromethylated intermediates again with thionyl chloride, are somebody's turn to do and acid chloride intermediate
Again with condensation reaction carried out under basic conditions to tert-butyl benzene acetonitrile obtain hydroxy nitrile intermediate, in the middle of hydroxy nitrile
Body, then carry out esterification with pivaloyl chloride and finally give nitrile pyrrole mite ester.The synthetic method general thought and route one of route three,
The difference of route two is larger, and its route is simply summarized as follows：4- tert-butylbenzenes acetonitrile is raw material and N- methyl -3,4- dimethyl -5-
After the reaction of carboxylate pyrazoles, then it is obtained with tertiary butyl acyl chloride reaction.
Chinese patent（Application number CN2015100098343, January 9 2015 date of application, denomination of invention：Containing three nitrogen
1,2,3- thiadiazoles -5- formamidines the compound of heterocycle and synthesis）In report the artificial Xihua Univ of patent application（Inventor
Wang Hui towns, Liu Ping, Yang Wei are clear etc.）Formula for TDCA the polysubstituted -1,2,3- thiadiazoles -5- formamidines compounds of N- and its conjunction
Into method（Formula 3）.Chinese patent（Application number CN2015100237806, January 19 2015 date of application）In report patent
Apply for artificial Xihua Univ（Inventor Liu Ping, Yang Wei are clear etc.）Mutual-through type is the polysubstituted -1,2,3- thiadiazoles -5- of N- of TDCA
The novel synthesis of formamidine compound are reported that the new method, using being first cyclized, finally goes up first to the synthesis of target product
The method of base, obtains fine experiment effect.Chinese patent（Application number CN2015103042053, June 9 2015 date of application
Day, denomination of invention：Cyclization method synthesizes polynitrogen heterocycle thiadiazoles -5- formamidine compounds）In report the artificial Xihua of patent application
University（Inventor Yang Wei is clear, Liu Ping etc.）Mutual-through type is the polysubstituted -1,2,3- thiadiazoles -5- formamidine compounds of N- of TDCA
Novel synthesis reported, the new method to the synthesis of target product using first going up methyl, the method being finally cyclized, this is new
Synthetic method high income, catalyst are easily prepared, catalyst is cheap, phosphorus-containing wastewater is few, to more environment-friendly.Chinese patent
（Patent No. ZL201510277765.4, May 28 2015 date of application, 2016 Granted publication dates August 31 days, invention
Title：1,2,3- thiadiazoles -5- formamidines poly-heterocyclic compounds are used as acaricidal purposes）In to report patent application artificially western
Hua Da（Inventor Yang Wei is clear, Liu Ping, Zhang Yuanyuan etc.）Formula for TDCA the polysubstituted -1,2,3- thiadiazoles -5- first of N-
Amidine compound as acaricidal purposes, particularly for the evil of fruit tree, vegetables, cotton, peanut and other crops and ornamental plant
Acarid control.But formula is the murder by poisoning power of the polysubstituted -1,2,3- thiadiazoles -5- formamidines compounds of N- to part adult of TDCA
It is not powerful enough to be used, it is necessary to carry out interworking from the acaricides for killing active high, the different mite killing mechanism of adult.It is well known that desinsection, killing
Mite agent all easy insect during long-term use develops immunity to drugs, and is one usage cycles of new varieties of extension, excellent with other
Different insecticidal/acaricidal agent kind carries out interworking using being a kind of conventional strategy.
The content of the invention
The main object of the present invention is directed to above deficiency, by the acaricidal rational mixture of the different mechanisms of action, there is provided
One kind has synergistic effect, and miticidal effect is good, safety, while can reduce the miticide composition of use cost again.
Chinese patent（Patent No. ZL201510277765.4, May 28 2015 date of application, Granted publication date
On August 31st, 2016, denomination of invention：1,2,3- thiadiazoles -5- formamidines poly-heterocyclic compounds are used as acaricidal purposes）Middle report
Road formula is N- polysubstituted -1,2, the 3- thiadiazoles -5- formamidines compounds of TDCA as acaricidal purposes, is particularly used
In the control of pest mite of fruit tree, vegetables, cotton, peanut and other crops and ornamental plant.The TDCA-6 in formula is for the compound of TDCA
~TDCA-13（The detailed titles of TDCA-6~TDCA-13 and structural formula refer to Chinese Patent Application No. CN2015100098343）Tool
There is preferable acaricidal activity.In TDCA-6~TDCA-13 compounds, under the same terms, miticidal effect most preferably TDCA-10
（Formula 4）；From another angle, production cost, the factor of acaricidal activity two, TDCA-6 are considered（Formula 5）But in being numerous compounds
Comparatively speaking more preferable acaricide.For ease of expression, in following narrations of the invention, mainly with TDCA-10 represent formula as
Polysubstituted -1,2,3- thiadiazoles -5- formamidine the compounds of N- of TDCA.
What the object of the invention was realized in that：
Miticide composition of the present invention (the 5- tert-butyl group -1,3,4- thiadiazoles -2- bases)-N'- (2,6- dichloro pyrroles with Chinese as N-
Pyridine -4- bases)-N, [English name is N- (5-tert-butyl-1,3,4- to 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidines
thiadiazol-2-yl)-N'- (2, 6-difluoropyridin-4-yl)-N,4-dimethyl-1,2,3-
thiadiazole-5-carboxam-idine（Hereinafter referred to as TDCA-10 in the present invention）], the structural formula such as institute of formula 2
The compound and nitrile pyrrole mite ester for showing be active ingredient, with agricultural chemicals in acceptable auxiliary element collectively constitute.
The permission part by weight of TDCA-10 and nitrile pyrrole mite ester is 100 in miticide composition of the present invention:1 to 1:80, preferably compare
Example is 80:1 to 1:20.
Miticide composition compound of the present invention has acaricidal purposes, particularly for fruit tree, vegetables, cotton, peanut
Deng crop and the control of pest mite of ornamental plant.The present composition is applied on crop and/or ornamental plant and is harmful to acarid life
Region long, can effectively prevent and treat evil mite.Present composition time of application can be in each growth phase in acarid, including
Ovum, deutonymph, young mite and into mite.Some representatives for the evil mite that can be prevented and treated for the present composition being mentioned below, enumerate and do not limit
Evil mite on some following crops and/or ornamental plant.
As the mite class for preventing and kill off as the present composition object, can enumerate：Belong to the mite of Ying Pi sections：Japanese blood mite,
Haemaphysalis longicornis, boophilus microplus, dermacentor reticulatus, dermacentor taiwanensis, haemaphysalis flava, ixodes persulcatus etc..Belong to the mite of Eriophyidae：Tea point leaf
Section tick, tealeaves goitre mite, apple rust mite, grape leaf rust mite, tulip aceria, matrimony vine burrknot tick, pseudo- pears rust tick, Pi Shi skin goitre mites
Deng.Belong to the mite of Tyroglyphidae：Hesperidium mite, ellipse dispersion, Acarus siro, the wild fat mite in river, Rhizoylyphus echinopus etc..Belong to Tarsonemidae
Mite：Webster tarsonemid, Polyphagotarsonemus latus Banks, primrose herbivore mite, double leaf tarsonemid.Belong to the mite of Eupodidae：Wheat leaf pawl mite,
Chinese cabbage mite.Belong to the mite of Tetranychidae：It is panonychus citri, panonychus ulmi, mulberry Panonychus citri, Tetranychus urticae, Tetranychus cinnabarinus, purplish red short
Must mite, priet mite, Liu Shi short hairs mite, Asia beginning tetranychid, knee beginning tetranychid, northern beginning tetranychid, Lee's beginning tetranychid, Eotetranychus smithi
Deng.
Although the present composition shows outstanding preventing and treating activity to the acarid of various mite sections, to useful crop, such as
Fruit tree, vegetables, cotton, peanut and other crops and/or ornamental plant only have the infringement of small degree or do not damage completely, take
Certainly in the present composition general structure concrete structure of each compound, amount of application, using useful crop object.Here it is this
Invention compound can be applied to the basic reason of control of pest mite on crop and/or ornamental plant.
Acceptable auxiliary element in described agricultural chemicals, including used in agricultural chemicals at present, unfavorable shadow will not be produced
Loud all kinds of common solvents and/or inert filler and/or surfactant and/or preservative and/or antifreezing agent and/or agglomeration resistance
Agent and/or defoamer and/or the corresponding adding ingredient such as cosolvent and/or stabilizer and/or thickener, it is possible to according to being produced
Dosage form do corresponding selection or adjust.
Agrochemical formulations generally comprise the miticide composition of the present invention of 0.1-99 weight %, particularly 2-90 weight %.
Wettable powder（WP）Middle miticide composition concentration is, such as 10-90 weight %, and the remainder in 100 weight % is by routinely making
Agent auxiliary element is constituted.In suspending agent（SC）Middle miticide composition concentration is, such as 1-90 weight %, preferably 5-75 weight %, 100
Remainder in weight % is made up of conventional formulation auxiliary element.In suspension emulsion（SE）Middle miticide composition concentration is, such as 1-
90 weight %, preferably 5-75 weight %, the remainder in 100 weight % are made up of conventional formulation auxiliary element.In water dispersant
（WDG）Middle miticide composition concentration is, such as 1-95 weight %, preferably 10-70 weight %, and the remainder in 100 weight % is by normal
Regulation agent auxiliary element is constituted.The preparation of other powder types includes 1-40 weight % reactive compounds, and preferably 5-20 weight % lives
Property compound, the remainder in 100 weight % is made up of conventional formulation auxiliary element.
Miticide composition of the present invention, using needing or applying Huan Jing ∕ conditions, is given birth to according to different by current conventional pesticide
Product mode, is that raw material is fully mixed by TDCA-10 in the miticide composition and nitrile pyrrole mite ester active ingredient and corresponding auxiliary element
Close, prepare the available corresponding formulation as multi-form.Possible formulation includes：It is wettable powder, water dispersant, outstanding
Floating agent, aqueous emulsion, suspension emulsion, microcapsule formulations etc..Such as several typical common dosage forms and prepare can be with：
Microcapsule formulations（CJ）Refer to and form " core-shell structure copolymer " structure small container using natural or synthesis macromolecular material, by agricultural chemicals
Cladding wherein, and is suspended in the formulations of pesticide in water.Micro-capsule suspension outward appearance is a thick working fluid, with aqueous emulsion
And aqueous suspension agent is similar.Micro- sem observation is used, its profile of microcapsules is spherical in shape, rugby shape, grain or other shapes.Microcapsules
Diameter is general at 3-30 microns.Observed with 400 power microscopes and be about as much as small rice grain and mung bean grain size.Due to microcapsules agriculture
Medical instrument has that the lasting period is long, toxicity is low, safe ready the features such as, just as pesticides new formulation a developing direction.Microcapsules
Customary preparation methods have complex coacervation, Simple coacervation, interfacial polymerization, situ aggregation method, orifice-coagulating bath method etc..It is several recently
There are some novel processing steps, such as molecular inclusion, microchannel emulsification method, supercritical fluid quick expansion method, ferment again in year
Female microcapsule method, self-assembled multilayer film method.Microcapsules often have sodium alginate, shitosan, gelatin, porous-starch etc. with wall material.
Complex coacervation is most popular method in above-mentioned microcapsule preparation method.Complex coacervation preparation principle is to carry opposite charges with two kinds
Material make embedded object, core disperses wherein, to change change pH values, temperature or solution concentration, due to the effect between electric charge, makes two kinds
Wall material solubility declines and is condensed into microcapsules precipitation.A kind of positively charged colloidal solution and another negatively charged colloid
Solution is mixed, and is separated because the interaction between xenogenesis electric charge forms compound polyelectrolyte, is deposited on capsule-core week
Enclose and obtain microcapsules.Complex coacervation is often capsule material with gelatin, Arabic gum.Gelatin is protein, in aqueous, strand
It is upper to contain-NH2With-COOH and its group-the NH that accordingly dissociates3+With-COO-, but contain-NH+3With-COO-How much is ion, by medium
The influence of pH value.Gelatin solution is in pH 4.0 or so, and its positive charge is most.Arabic gum is polysaccharide, in aqueous, point
Contain-COOH and-COO in subchain-, with negative electrical charge.Therefore in the aqueous solution that gelatin mixes with Arabic gum, regulation pH is about
For 4.0 when, gelatin and Arabic gum neutralize to form compound on the contrary because of charged phase, the reduction of its solubility, are condensed into from system
Capsule is separated out.Curing agent formaldehyde is added, formaldehyde produces amine aldehyde condensation reaction with gelatin, and gelatin molecule is cross-linked into network structure, protects
The shape of micro-capsule is held, as irreversible micro-capsule；Plus 2% NaOH regulations medium pH 8 ~ 9, be conducive to the condensation reaction of amine aldehyde to carry out
Completely.
Water dispersant（WDG）Can in water fater disintegration, and can be uniformly dispersed in higher suspension dispersion is formed in water
A kind of granular preparation.The present composition and auxiliary element one can be reinstated into air-flow during preparation to smash or ultra-fine grinding, system
Into wettable powder, this is dry method；By the present composition, auxiliary agent, adjuvant etc., with water as medium, ground in sand mill,
Suspending agent is made, then re-dry granulation, this is wet method.
Wettable powder（WP）, i.e., solid powder preparation that can be dispersed in water.During preparation, can be according to conventional side
Formula, is firstly added the composition of TDCA-10 of the present invention and nitrile pyrrole mite ester, is subsequently adding diatomite, potter's clay, precipitated calcium carbonate, white
The conventional diluent such as carbon black or inert substance, add other conventional auxiliary elements, such as alkylnaphthalene sulfonate, alkyl benzene sulphonate
Salt, aliphatic alcohol sulfate, alkyl bromination ammonium, alkyl ammomium chloride, quaternary alkylphosphonium salts, alkyl polyoxyethylene base ether sulfate, sulfomethylated lignin
One or several in hydrochlorate, lignin, carboxymethylcellulose calcium, sodium carboxymethylcellulose, azone, thiophene ketone, and it is conventional steady
Determine the complementary auxiliary component such as agent, foam inhibitor, anticaking agent.
Suspension emulsion（SE）That is a kind of hybrid dispersions of the insoluble agricultural chemicals of water in water, active ingredient therein is in suspension
State, other active ingredients are in emulsion state.Can be by the present composition and corresponding emulsion, moistening point when being prepared during preparation
The auxiliary elements such as powder, thickener, stabilizer, antifreezing agent, pH adjusting agent, defoamer, conventionally, through wet method Ultramicro-powder
It is broken to be mixed to prepare.Wherein emulsifying agent is APES class（Agriculture breast 100#）, alkylbenzenesulfonate（Agriculture breast 500#）, benzene
Ethyl phenol polyethenoxy ether class（Agriculture breast 600#）, alkyl phenol or aralkyl phenol polyethenoxy ether formaldehyde condensation species（Nongru-700 #）
One or several in.Wherein Ricinate is lignosulfonates, lignin, phosphate polyethers, carboxymethyl fibre
Dimension element, sodium carboxymethylcellulose, crown ether, alkylnaphthalene sulfonate, alkylbenzenesulfonate, aliphatic alcohol sulfate, alkyl ammonium halide, season
One or several in phosphonium salt, alkyl polyoxyethylene base ether sulfate, azone, thiophene ketone；Thickener and stabilizer are polyethylene
One or several in alcohol, condensed phosphate, xanthan gum, Magnesiumaluminumsilicate etc.；Antifreezing agent be sodium chloride, urea, ammonium sulfate,
One or several in ethylene glycol, glycerine etc.；PH adjusting agent be potassium dihydrogen phosphate, dipotassium hydrogen phosphate, citric acid, sodium carbonate,
One or several in potassium carbonate etc..Conventional organosilicon is used as defoamer and foam inhibitor.
Suspending agent（SC）That is agricultural chemicals suspension agent（SC）, be water insoluble solids agricultural chemicals or mix liquid pesticidal in water or oil
Dispersion.During preparation, with water or oil as decentralized medium, by TDCA-10 of the present invention and nitrile pyrrole mite ester composition and aid in into
Point（Such as thickener, stabilizer, Ricinate, antifreezing agent, pH adjusting agent, defoamer）Through soybean dietary fiber（Grinding）System
.Wherein Ricinate is phosphate polyethers, alkylnaphthalene sulfonate, alkylbenzenesulfonate, aliphatic alcohol sulfate, alkyl bromide
Change ammonium, alkyl ammomium chloride, crown ether, quaternary alkylphosphonium salts, alkyl polyoxyethylene base ether sulfate, lignosulfonates, lignin, carboxymethyl
One or several in cellulose, sodium carboxymethylcellulose, azone, thiophene ketone；Thickener and stabilizer are polyvinyl alcohol, condensation
One or several in phosphate, xanthan gum, Magnesiumaluminumsilicate etc.；Antifreezing agent be sodium chloride, urea, ammonium sulfate, ethylene glycol,
One or several in glycerine etc.；PH adjusting agent is potassium dihydrogen phosphate, dipotassium hydrogen phosphate, citric acid, sodium carbonate, potassium carbonate etc.
In one or several.Conventional organosilicon is used as defoamer and foam inhibitor.
It should be noted that specific formulation mentioned above is the representative formulation that present composition thing can be prepared, enumerate
It is not limited to these above-mentioned formulations.
Agrochemical formulations generally comprise the present composition thing of 0.1-99 weight %, particularly 0.5-95 weight %.
Wettable powder（WP）Middle activity compound concentration is, such as 1-90 weight %, and the remainder in 100 weight % is by conventional formulation
Auxiliary element is constituted.In suspending agent（SC）Middle activity compound concentration is, such as 1-90 weight %, preferably 5-75 weight %, 100 weights
Remainder in amount % is made up of conventional formulation auxiliary element.In suspension emulsion（SE）Middle activity compound concentration is, such as 1-90
Weight %, preferably 5-75 weight %, the remainder in 100 weight % are made up of conventional formulation auxiliary element.In water dispersant
（WDG）Middle activity compound concentration is, such as 1-95 weight %, preferably 10-70 weight %, and the remainder in 100 weight % is by normal
Regulation agent auxiliary element is constituted.The preparation of other powder types includes 1-40 weight % reactive compounds, and preferably 5-20 weight % lives
Property compound, the remainder in 100 weight % is made up of conventional formulation auxiliary element.
To be administered, if by appropriate formulation, diluted in a usual manner, for example for wettable powder, water dispersant,
Suspending agent, aqueous emulsion, suspension emulsion dilute with water.Pulvis, granule, microcapsule formulations etc. generally no longer use other inert materials using preceding
Matter dilutes.
The amount of application of the compounds of this invention changes according to external condition, and the external condition especially prevents and treats acarid pair
As, temperature, humidity, preparation formulation.It can change in relative broad range, such as 0.1-500g/667m2Or more chemical combination of the present invention
Thing, preferably 1-50g/667m2。
Concrete mode by the following examples is described in further detail to the above of the invention again.But should not
This scope for being interpreted as above-mentioned theme of the invention is only limitted to following example by this.Above-mentioned technological thought feelings of the invention are not being departed from
Under condition, according to various replacements or change that ordinary skill knowledge and customary means are made, all should be included in of the invention
In the range of.Each material proportion of composing is weight % in embodiment.
Specific embodiment：
(1), example of formulations
Embodiment 1：55% miticide composition TDCA-10 nitrile pyrrole mite ester water dispersible granules（WDG）（In 55% finger original ingredient ratio
The mass percent of active component, similarly hereinafter）
Weigh respectively 350 grams of TDCA-10,200 grams of nitrile pyrrole mite esters, 60 grams of lignin, 45 grams of acrylic acid minor matters polymer, 40 gram ten
Dialkyl sulfonates, 55 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 2：50% miticide composition TDCA-10 nitrile pyrrole mite ester water dispersible granules（WDG）
Weigh respectively 300 grams of TDCA-10,200 grams of nitrile pyrrole mite esters, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 gram ten
Dialkyl sulfonates, 55 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 3：50% miticide composition TDCA-13 nitrile pyrrole mite ester water dispersible granules（WDG）
Weigh respectively 300 grams of TDCA-13,200 grams of nitrile pyrrole mite esters, 70 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 gram ten
Dialkyl sulfonates, 60 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 4：50% miticide composition TDCA-10 nitrile pyrrole mite ester water dispersible granules（WDG）
Weigh respectively 200 grams of TDCA-10,300 grams of nitrile pyrrole mite esters, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 30 gram ten
Dialkyl sulfonates, 40 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 5：30% miticide composition TDCA-10TDCA-6 nitrile pyrrole mite ester water dispersible granules（WDG）
100 grams of TDCA-10,100 grams of TDCA-6,100 grams of nitrile pyrrole mite esters, 30 grams of lignin, 40 grams of acrylic acid minor matters are weighed respectively
Polymer, 30 grams of dodecyl sodium sulfates, 40 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 6：60% miticide composition TDCA-10 nitrile pyrrole mite ester water dispersible granules（WDG）
570.0 grams of TDCA-10,30.0 grams of nitrile pyrrole mite esters, 60 grams of lignin, 50 grams of acrylic acid minor matters polymer, 35 are weighed respectively
Gram dodecyl sodium sulfate, 25 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 7：6% miticide composition TDCA-10 nitrile pyrrole mite ester microcapsule formulations（CJ）
Weigh respectively 30 grams of TDCA-10,30 grams of nitrile pyrrole mite esters, 30 grams of gelatin, 20 grams of poly-aspartates, 10 grams of Tween-60s, 50 grams
Arabic gum, 10 grams of polyethylene glycol, 50 gram of 20% formalin, 10% acetums are appropriate（Titer is by preparation process
Titration operation determines usage amount, similarly hereinafter）, 20% NaOH solution（Titer）, distilled water complementary to 1000 grams, it is standby；
Preparation process（1）Poly-aspartate is prepared with gelatin mixed solution：After using distillation appropriate amount of water immersion swelling in gelatin, heating
Dissolving, is heated to 50 DEG C, adds poly-aspartate, and stirring adds appropriate distilled water, and 50 DEG C of insulations are standby.（2）Arabic peptization
The preparation of liquid：Appropriate distilled water is added in reaction unit, Arabic gum powder is added, 80 DEG C or so are heated to, being gently mixed makes
Dissolving, 80 DEG C of insulations are standby.（3）The preparation of TDCA-10 and nitrile pyrrole mite ester active ingredient emulsion：By TDCA-10, nitrile pyrrole mite ester,
Tween-60, polyethylene glycol, the gumwater of above-mentioned preparation, are placed in tissue mashing machine, emulsify 30 seconds, obtain final product emulsion.
（4）Mixing：Under the conditions of 50~55 DEG C, above-mentioned poly-aspartate and gelatin mixed solution are added, being gently mixed makes to be well mixed.
（5）The preparation of micro-capsule：In the case where being stirred continuously, to 10% acetum is added dropwise in foregoing mixed liquor, pH to 3.8~4.0 is adjusted；（6）
The solidification of micro-capsule：In the case where being stirred continuously, during about 30 DEG C of distilled water added into micro-capsule liquid, micro-capsule liquid from 50~55 DEG C of water-baths will be contained
In remove, be stirred continuously, natural cooling, when temperature drops to 32~35 DEG C, add ice cube, continue stir to temperature be 10 DEG C with
Under, 20% formalin is added, continue to stir 15~25min, then its pH 8~9 is adjusted with 20%NaOH solution, continue to stir 20~
30min, to separating out, standing treats that micro-capsule is settled for observation.（7）The filtering and drying of micro-capsule：Treat that micro-capsule sedimentation is complete, cross and filter
Fall supernatant, micro-capsule distillation is washed to formaldehydeless taste, centrifugation, drying.
Embodiment 8：6% miticide composition TDCA-10 nitrile pyrrole mite ester microcapsule formulations（CJ）
Weigh respectively 40 grams of TDCA-10,20 grams of nitrile pyrrole mite esters, 30 grams of gelatin, 20 grams of poly-aspartates, 10 grams of Tween-60s, 50 grams
Arabic gum, 20 grams of polyethylene glycol, 50 gram of 20% formalin, 10% acetums are appropriate（Titer）, 20% NaOH solution（Drop
It is quantitative）, distilled water complementary to 1000 grams, it is standby；
Preparation process is completely same as Example 1.
Embodiment 9：6% miticide composition TDCA-10 nitrile pyrrole mite ester microcapsule formulations（CJ）
Weigh respectively 20 grams of TDCA-10,40 grams of nitrile pyrrole mite esters, 30 grams of gelatin, 20 grams of poly-aspartates, 10 grams of Tween-60s, 50 grams
Arabic gum, 8 grams of polyethylene glycol, 50 gram of 20% formalin, 10% acetums are appropriate（Titer）, 20% NaOH solution（Drop
It is quantitative）, distilled water complementary to 1000 grams, it is standby；
Preparation process is completely same as Example 1.
Embodiment 10：10% miticide composition TDCA-10 nitrile pyrrole mite ester microcapsule formulations（CJ）
Weigh respectively 50 grams of TDCA-10,50 grams of nitrile pyrrole mite esters, 40 grams of gelatin, 30 grams of poly-aspartates, 20 grams of Tween-60s, 60 grams
Arabic gum, 30 grams of polyethylene glycol, 100 gram of 20% formalin, 10% acetums are appropriate（Titer）, 20% NaOH solution
（Titer）, distilled water complementary to 1000 grams, it is standby；
Preparation process is similar to Example 1.
Embodiment 11：10% miticide composition TDCA-10 nitrile pyrrole mite ester microcapsule formulations（CJ）
Weigh respectively 33 grams of TDCA-10,67 grams of nitrile pyrrole mite esters, 40 grams of gelatin, 30 grams of poly-aspartates, 20 grams of Tween-60s, 60 grams
Arabic gum, 25 grams of polyethylene glycol, 100 gram of 20% formalin, 10% acetums are appropriate（Titer）, 20% NaOH solution
（Titer）, distilled water complementary to 1000 grams, it is standby；
Preparation process is similar to Example 1.
Embodiment 12：10% miticide composition TDCA-10 nitrile pyrrole mite ester microcapsule formulations（CJ）
Weigh respectively 67 grams of TDCA-10,33 grams of nitrile pyrrole mite esters, 40 grams of gelatin, 30 grams of poly-aspartates, 20 grams of Tween-60s, 60 grams
Arabic gum, 50 grams of polyethylene glycol, 100 gram of 20% formalin, 10% acetums are appropriate（Titer）, 20% NaOH solution
（Titer）, distilled water complementary to 1000 grams, it is standby；
Preparation process is similar to Example 1.
Embodiment 13：50% miticide composition TDCA-10TDCA-6 nitrile pyrrole mite ester water dispersible granules（WDG）
240 grams of TDCA-10,60 grams of TDCA-6,200 grams of nitrile pyrrole mite esters, 50 grams of lignin, 50 grams of acrylic acid minor matters are weighed respectively to gather
Compound, 40 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 14：30% miticide composition TDCA-10TDCA-6TDCA-13 nitrile pyrrole mite ester water dispersible granules
（WDG）
Weigh respectively 110 grams of TDCA-10,90 grams of TDCA-6,50 grams of TDCA-13,50 grams of nitrile pyrrole mite esters, 50 grams of lignin, 50 grams
Acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 15：50% miticide composition TDCA-10TDCA-6TDCA-13 nitrile pyrrole mite ester water dispersible granules
（WDG）
Weigh respectively 250 grams of TDCA-10,50 grams of TDCA-6,50 grams of TDCA-13,150 grams of nitrile pyrrole mite esters, 50 grams of lignin, 50 grams
Acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 16：60% miticide composition TDCA-10TDCA-6TDCA-13 nitrile pyrrole mite ester water dispersible granules
（WDG）
Weigh respectively 100 grams of TDCA-10,50 grams of TDCA-6,50 grams of TDCA-13,400 grams of nitrile pyrrole mite esters, 60 grams of lignin, 40 grams
Acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 17：60% miticide composition TDCA-10TDCA-6TDCA-13 nitrile pyrrole mite ester water dispersible granules
（WDG）
100 grams of TDCA-10,100 grams of TDCA-6,100 grams of TDCA-13,300 grams of nitrile pyrrole mite esters, 60 grams of lignin, 40 are weighed respectively
Gram acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 18：60% miticide composition TDCA-10TDCA-6TDCA-13 nitrile pyrrole mite ester water dispersible granules
（WDG）
150 grams of TDCA-10,150 grams of TDCA-6,150 grams of TDCA-13,150 grams of nitrile pyrrole mite esters, 60 grams of lignin, 40 are weighed respectively
Gram acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 19：30% miticide composition TDCA-10 nitrile pyrrole mite ester water dispersible granules（WDG）
Weigh respectively 200 grams of TDCA-10,100 grams of nitrile pyrrole mite esters, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 gram ten
Dialkyl sulfonates, 30 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 20：40% miticide composition TDCA-10 nitrile pyrrole mite ester water dispersible granules（WDG）
Weigh respectively 250 grams of TDCA-10,150 grams of nitrile pyrrole mite esters, 60 grams of lignin, 50 grams of acrylic acid minor matters polymer, 40 gram ten
Dialkyl sulfonates, 60 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 21：30% miticide composition TDCA-13 nitrile pyrrole mite ester water dispersible granules（WDG）
Weigh respectively 200 grams of TDCA-13,100 grams of nitrile pyrrole mite esters, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 gram ten
Dialkyl sulfonates, 40 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 22：40% miticide composition TDCA-10 nitrile pyrrole mite ester wettable powders（WP）
360.0 grams of TDCA-10,40.0 grams of nitrile pyrrole mite esters, 30 grams of lignosulfonates calcium, 30 grams of carboxymethylcellulose calciums are weighed respectively
Sodium, 30 grams of Magnesiumaluminumsilicates, 20 grams of neopelexes, 20 grams of TBABs, kaolin complementaries are standby to 1000 grams
With；
Prepare：During each material sequentially added into reactor, stirring is sufficiently mixed it, is crushed to 5~20 μm.
Embodiment 23：30% miticide composition TDCA-10 nitrile pyrrole mite ester wettable powders（WP）
Weigh respectively 200 grams of TDCA-10,100 grams of nitrile pyrrole mite esters, 30 grams of lignosulfonates calcium, 30 grams of sodium carboxymethylcelluloses,
30 grams of Magnesiumaluminumsilicates, 20 grams of neopelexes, 20 grams of TBABs, kaolin complementaries are standby to 1000 grams；
Prepare：During each material sequentially added into reactor, stirring is sufficiently mixed it, is crushed to 5~20 μm.
Embodiment 24：20% miticide composition TDCA-10 nitrile pyrrole mite ester wettable powders（WP）
Weigh respectively 100 grams of TDCA-10,100 grams of nitrile pyrrole mite esters, 35 grams of lignosulfonates calcium, 30 grams of sodium carboxymethylcelluloses,
40 grams of Magnesiumaluminumsilicates, 20 grams of neopelexes, 20 grams of TBABs, kaolin complementaries are standby to 1000 grams；
Prepare：During each material sequentially added into reactor, stirring is sufficiently mixed it, is crushed to 5~20 μm.
Embodiment 25：30% miticide composition TDCA-10 nitrile pyrrole mite ester wettable powders（WP）
Weigh respectively 100 grams of TDCA-10,200 grams of nitrile pyrrole mite esters, 30 grams of lignosulfonates calcium, 30 grams of sodium carboxymethylcelluloses,
30 grams of Magnesiumaluminumsilicates, 20 grams of neopelexes, 20 grams of TBABs, kaolin complementaries are standby to 1000 grams；
Prepare：During each material sequentially added into reactor, stirring is sufficiently mixed it, is crushed to 5~20 μm.
Embodiment 26：50% miticide composition TDCA-10 nitrile pyrrole mite ester wettable powders（WP）
Weigh respectively 100 grams of TDCA-10,400 grams of nitrile pyrrole mite esters, 40 grams of lignosulfonates calcium, 40 grams of sodium carboxymethylcelluloses,
40 grams of Magnesiumaluminumsilicates, 30 grams of neopelexes, 20 grams of TBABs, kaolin complementaries are standby to 1000 grams；
Prepare：During each material sequentially added into reactor, stirring is sufficiently mixed it, is crushed to 5~20 μm.
Embodiment 27：20% reactive compound（TDCA-10）Water dispersible granules（WDG）
Weigh respectively 200 grams of TDCA-10,70 grams of lignin, 60 grams of acrylic acid minor matters polymer, 50 grams of dodecyl sodium sulfates,
80 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 28：20% nitrile pyrrole mite ester water dispersible granules（WDG）
Weigh respectively 200 grams of nitrile pyrrole mite esters, 70 grams of lignin, 60 grams of acrylic acid minor matters polymer, 50 grams of dodecyl sodium sulfates,
80 grams of polyethylene glycol, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 29：35% nitrile pyrrole mite ester suspending agent（SC）
Weigh respectively 350 grams of nitrile pyrrole mite esters, 40 grams of lignosulfonates calcium, 50 grams of sodium carboxymethylcelluloses, 30 grams of Magnesiumaluminumsilicates,
40 grams of neopelexes, 60 grams of polyethylene glycol, water complementaries are standby to 1000 grams；
During each material sequentially added into reactor, just dispersion is carried out using high-speed shearing machine, be then ground in sand mill
Effect grain diameter of components is at 2~5 μm.
Embodiment 30：30% nitrile pyrrole mite ester wettable powder（WP）
Weigh respectively 300 grams of nitrile pyrrole mite esters, 40 grams of lignosulfonates calcium, 40 grams of sodium carboxymethylcelluloses, 50 grams of Magnesiumaluminumsilicates,
30 grams of neopelexes, 25 grams of TBABs, kaolin complementaries are standby to 1000 grams；
Prepare：During each material sequentially added into reactor, stirring is sufficiently mixed it, is crushed to 5~20 μm.
Embodiment 31：30% TDCA-10 wettable powders（WP）
Weigh respectively 300 grams of TDCA-10,35 grams of lignosulfonates calcium, 35 grams of sodium carboxymethylcelluloses, 30 grams of Magnesiumaluminumsilicates,
25 grams of neopelexes, 25 grams of TBABs, kaolin complementaries are standby to 1000 grams；
Prepare：During each material sequentially added into reactor, stirring is sufficiently mixed it, is crushed to 5~20 μm.
Embodiment 32：10% nitrile pyrrole mite ester suspending agent（SC）
100 grams of nitrile pyrrole mite esters are weighed respectively, (Huntsman Corporation of the U.S. produces 50 grams of TERSPERSE 2020, alkylnaphthalene sulfonate
Class), 80 grams of lignosulfonates calcium, 30 grams of sodium carboxymethylcelluloses, 70 grams of Magnesiumaluminumsilicates, 55 grams of neopelexes,
50 grams of polyethylene glycol, water complementaries are standby to 1000 grams；
During each material sequentially added into reactor, just dispersion is carried out using high-speed shearing machine, be then ground in sand mill
Effect grain diameter of components is at 2~5 μm.
Embodiment 33：5% TDCA-10 suspending agents（SC）
50 grams of TDCA-10,50 grams of AEOs, 40 grams of lignosulfonates calcium, 55 grams of carboxymethyl fibres are weighed respectively
The plain sodium of dimension, 75 grams of Magnesiumaluminumsilicates, 60 grams of neopelexes, 60 grams of polyethylene glycol, water complementaries are standby to 1000 grams；
During each material sequentially added into reactor, just dispersion is carried out using high-speed shearing machine, be then ground in sand mill
Effect grain diameter of components is at 2~5 μm.
Embodiment 34：50% nitrile pyrrole mite ester water dispersible granules（WDG）
500 grams of nitrile pyrrole mite esters, 40 grams of sodium lignin sulfonates, 50 grams of acrylic acid minor matters polymer, 30 grams of polyethylene pyrroles are weighed respectively
Pyrrolidone, 20 grams of ammonium sulfate, 40 grams of dodecyl sodium sulfates, 35 grams of polyethylene glycol, 25 grams of sodium carboxymethylcelluloses, 100 grams of silicon
Diatomaceous earth, bentonite complementary are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 35：50% TDCA-10 water dispersible granules（WDG）
500 grams of TDCA-10,30 grams of sodium lignin sulfonates, 40 grams of acrylic acid minor matters polymer, 50 grams of polyvinyl pyrroles are weighed respectively
Alkanone, 15 grams of ammonium sulfate, 50 grams of dodecyl sodium sulfates, 25 grams of polyethylene glycol, 30 grams of sodium carboxymethylcelluloses, 50 grams of diatoms
Soil, bentonite complementary are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 36：40% miticide composition TDCA-10 nitrile pyrrole mite ester water dispersible granules（WDG）
363.6 grams of TDCA-10,36.4 grams of nitrile pyrrole mite esters, 50 grams of sodium lignin sulfonates, 40 grams of acrylic acid minor matters polymerizations are weighed respectively
Thing, 40 grams of dodecyl sodium sulfates, 55 grams of polyethylene glycol, 45 grams of ammonium sulfate, bentonite complementaries are standby to 1000 grams；
During each material sequentially added into reactor, it is well mixed, is then ground in sand mill, add suitable quantity of water, granulation is dried
Obtain final product water dispersible granules.
Embodiment 37：20% miticide composition TDCA-10 nitrile pyrrole mite ester wettable powders（WP）
295 grams of TDCA-10,5 grams of nitrile pyrrole mite esters, 35 grams of lignosulfonates calcium, 60 grams of sodium carboxymethylcelluloses, 70 are weighed respectively
Gram Magnesiumaluminumsilicate, 50 grams of neopelexes, 45 grams of TBABs, kaolin complementaries are standby to 1000 grams；
Prepare：During each material sequentially added into reactor, stirring is sufficiently mixed it, is crushed to 5~20 μm.
By following experiment it can be shown that two active ingredient TDCA-10 and nitrile pyrrole in above-mentioned miticide composition of the invention
The compounding of mite ester can have obvious synergistic effect.
(2), biological Examples
Embodiment 38：TDCA-10 and nitrile pyrrole mite ester composite formula screening experiment
First, reagent agent（A represents nitrile pyrrole mite ester in following reagents；B represents TDCA-10）
A agent：50% nitrile pyrrole mite ester water dispersible granules（WDG）（Prepared by the method for embodiment 34）
B agent：50% TDCA-10 water dispersible granules（WDG）（Prepared by the method for embodiment 35）
AB1：Nitrile pyrrole mite ester TDCA-10（A：B=20:1）
AB2：Nitrile pyrrole mite ester TDCA-10（A：B=10:1）
AB3：Nitrile pyrrole mite ester TDCA-10（A：B=1:1）
AB4：Nitrile pyrrole mite ester TDCA-10（A：B=1:10）
AB5：Nitrile pyrrole mite ester TDCA-10（A：B=1:20）
AB6：Nitrile pyrrole mite ester TDCA-10（A：B=1:40）
AB7：Nitrile pyrrole mite ester TDCA-10（A：B=1:60）
AB8：Nitrile pyrrole mite ester TDCA-10（A：B=1:70）
2nd, for examination insect
For examination insect using the red spider adopted in the citrus trees of field, raised for 3 generations indoors as test worm.
3rd, experimental technique
Experiment uses dip slide method.Every kind of reagent tests 5 kinds of concentration（Every kind of specific concentration of reagent refers to table 1）, each repeats treatment 4
It is secondary, 120 (four times, altogether 480) are repeated every time, 72 hours microscopy results after medicine obtain the death rate for test worm, calculate
LC50And co-toxicity coefficient（CTC）.
4th, computational methods
The death rate of every kind of reagent is converted to correspondence niqueMin（y）It is ordinate, and with the right of the various concentrations of various reagents
Numerical value lgx is abscissa, using least square method, obtains virulence equation（y=a+blgx）Middle coefficient a, b.According to virulence equation,
As y=5.000（NiqueMin when i.e. the death rate is 50%）, calculate the LC of the reagent50.Calculated using the abundant equations of Sun Yun mixed
Close the co-toxicity coefficient of medicament（CTC）（Bibliography：Tan Genjia, wish Jianping etc., " fungicide bioassay computational methods and should
With ", Anhui agronomy circular, 1998,4（1）, 27-28）.The CTC values calculated using the abundant equations of Sun Yun, China is generally acknowledged that
CTC has synergistic effect more than 150（Wherein：CTC has notable synergistic effect more than 200）, CTC is 50~150 for addition is made
With CTC is antagonism less than 50.
5th, result and analysis
TDCA-10 and nitrile pyrrole mite ester composition series proportioning mixture are to citrus red mite Toxicity Determination result, LC50With altogether
Malicious coefficient（CTC）It is shown in Table 1, table 2.
Laboratory experiment result shows that TDCA-10 and nitrile pyrrole mite ester composition series proportioning mixture do not show to citrus red mite
Go out antagonism, major part has certain synergistic effect（The CTC values of AB4~AB6 both greater than 180, show there is synergistic effect）,
AB4, AB5 its CTC value is all higher than 210, shows there is notable synergistic effect.The co-toxicity coefficient of wherein AB4 mixtures is maximum（CTC=
225）, illustrate that its synergistic effect is maximum.
Table 1, TDCA-10 and nitrile pyrrole mite ester match mixture to citrus red mite Toxicity Determination result
The LC of table 250And co-toxicity coefficient（CTC）
The death rate corresponding probit value when y represents composition series proportioning mixture various concentrations in table 2, x represents concentration（C）It is right
Numerical value lgC（That is x=lgC）.
Embodiment 39：Nitrile pyrrole mite ester TDCA-10 composition for preventing and controlling citrus red mites field efficacy is tested
First, reagent agent
1st, 40% miticide composition nitrile pyrrole mite ester water dispersible granules（TDCA-10:Nitrile pyrrole mite ester=10:1）（WDG）（According to reality
It is prepared by the method for applying example 36）；
2nd, 20% miticide composition TDCA-10 nitrile pyrrole mite ester wettable powders（WP）（Wherein TDCA-10:Nitrile pyrrole mite ester=
59:1）（It is prepared by the method according to embodiment 37）；
3rd, 10% nitrile pyrrole mite ester suspending agent（SC）（It is prepared by the method according to embodiment 32）；
4th, 5% TDCA-10 suspending agents（SC）（It is prepared by the method according to embodiment 33）.
2nd, experimental subjects
1st, experimental period：June 21 2015 time started；
1st, place is tested：Mianyang City Nong Ke areas of Sichuan Province live kwan-yin village Citrus Orchard；
2nd, crop is tested：Sweet orange；
3rd, controlling object：Citrus red mite.
3rd, experimental technique
1st, processing item：40% miticide composition TDCA-10 nitrile pyrrole mite ester water dispersible granules（WDG）8000 times of dilution；20%
Miticide composition TDCA-10 nitrile pyrrole mite ester wettable powders（WP）4000 times of dilution；10% nitrile pyrrole mite ester suspending agent（SC）
2000 times of dilution；5% TDCA-10 suspending agents（SC）1000 times of dilution.Blank：Using clear water.
2nd, cell is set：Each cell seeds, the age of tree, growing way and rich water quality management condition are basically identical.Each cell is fixed 3
Set, four repetitions, totally 24 cell；And cell is arranged according to random area.
3rd, spraying time and method：In citrus red mite peak of occurrence period（June 21）Dispenser is once.Using pressure manually
Contracting sprayer even spraying, to squirt blade as degree.
4th, control time and method：Before dispenser and 3 days after dispenser, respectively investigate once within 10 days, 20 days, 30 days.Method is
Each tree wins 30 leaves at random in four orientation, and 360 are won per cell, and mite quantity living on record blade calculates mite mouthful and subtracts
Move back rate and preventive effect.
4th, mite mouthful decline rate and preventive effect computational methods
PT=mites mouthful decline rate（%）=（Mite number living after mite number-dispenser living before dispenser）/ (mite number living before dispenser) * 100
Preventive effect（%）=(PT-CK)/wherein CK of (100-CK) * 100 are blank district mite mouthful decline rate
5th, experimental result
40% miticide composition TDCA-10 nitrile pyrrole mite ester water dispersible granules（WDG）（TDCA-10:Nitrile pyrrole mite ester=10:1）It is dilute
Release 8000 times；20% miticide composition TDCA-10 nitrile pyrrole mite ester wettable powders（WP）（Wherein TDCA-10:Nitrile pyrrole mite ester
=60:1）4000 times of dilution, is respectively 98.37% and 97.19% in 3 days after dispenser to citrus red mite preventive effect；After dispenser 10 days to mandarin orange
Orange spider preventive effect is respectively 95.14% and 93.01%；87.98% He was respectively to citrus red mite preventive effect in 20 days after dispenser
86.64%；81.38% and 81.04% were respectively to citrus red mite preventive effect in 30 days after dispenser.The nitrile pyrrole mite ester of comparison medicament 10% hangs
Floating agent（SC）2000 times of dilution, 3 days after dispenser, 10 days, 20 days, 30 days four times investigation preventive effects be respectively 91.99%, 88.87%,
81.12%、71.53%.The TDCA-10 suspending agents of comparison medicament 5%（SC）Dilution 1000 times, 3 days after dispenser, 10 days, 20 days, 30
It four times investigation preventive effect is respectively 89.61%, 84.70%, 78.96%, 70.28%（Refer to table 3）.Observed according to field experiment, not
It was found that TDCA-10 nitrile pyrrole mite ester miticide compositions produce poisoning phenomenon to experiment crop.
The TDCA-10 of table 3 and nitrile pyrrole mite ester series proportioning mixture are to citrus red mite field experiment result statistical form
Claims (8)
1. miticide composition, with the N- for being referred to as TDCA polysubstituted -1,2,3- thiadiazoles -5- formamidine compounds and nitrile pyrrole mite ester are
Acceptable auxiliary element is collectively constituted in active ingredient, with agricultural chemicals, wherein the referred to as compound of TDCA and nitrile pyrrole mite ester
Part by weight is 100:1 to 1:80.
2. miticide composition according to claim 1, it is characterized in that the active ingredient is referred to as the compound and nitrile of TDCA
Pyrrole mite ester part by weight is 80:1 to 1:20.
3. miticide composition according to claim 1, it is characterized in that referred to as the compound of TDCA can be referred to as TDCA-
6 compound N-(the 5- tert-butyl group -1,3,4- thiadiazoles -2- bases)-N'- (2,6- dichloropyridine -4- bases)-N, 4- dimethyl -1,
Compound N-(the 5- tert-butyl group -1,3,4- thiadiazoles -2- bases)-N'- (2- of 2,3- thiadiazoles -5- carbonamidines, referred to as TDCA-7
Chloro- 6- fluorine pyridin-4-yl)-N, compound N-(uncle 5- of 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidines, referred to as TDCA-8
Butyl -1,3,4- thiadiazoles -2- bases)-N'- (the chloro- 6- bromopyridines -4- bases of 2-)-N, 4- dimethyl -1,2,3- thiadiazoles -5- first
Compound N-(the 5- tert-butyl group -1,3,4- thiadiazoles -2- bases)-N'- (chloro- 6- iodine pyridines -4- of 2- of amidine, referred to as TDCA-9
Base)-N, the compound N-(the 5- tert-butyl group -1,3,4- thiophenes of 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidines, referred to as TDCA-10
Diazole -2- bases)-N'- (2,6- difluoro pyridine -4- bases)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidines, referred to as TDCA-
11 compound N-(the 5- tert-butyl group -1,3,4- thiadiazoles -2- bases)-N'- (the bromo- 6- fluorine pyridin-4-yls of 2-)-N, 4- dimethyl -
Compound N-(the 5- tert-butyl group -1,3,4- thiadiazoles -2- bases)-N'- of 1,2,3- thiadiazoles -5- carbonamidines, referred to as TDCA-12
The compound N of (the fluoro- 6- iodine pyridines-4- bases of 2-)-N, 4- dimethyl-1,2,3- thiadiazoles-5- carbonamidines, referred to as TDCA-13-
(the 5- tert-butyl group -1,3,4- thiadiazoles -2- bases)-N'- (2,6- dibromo pyridine -4- bases)-N, 4- dimethyl -1,2,3- thiadiazoles -
Any one in 5- carbonamidines.
4. miticide composition according to claim 1, by the current conventional pesticide mode of production, prepares as multi-form
Available microcapsule formulations（CJ）, suspension emulsion（SE）, water dispersible granules（WDG）, wettable powder（WP）, aqueous emulsion, suspension
Any one formulation in the preparation formulations such as agent.
5. miticide composition according to claim 1, for the evil of fruit tree, vegetables, cotton, peanut and other crops and ornamental plant
Acarid control.
6. miticide composition according to claim 1, can also be N- (the 5- tert-butyl group -1,3,4- thiadiazoles -2- bases)-N'-
(2,6- dichloropyridine -4- bases)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidines, N- (the 5- tert-butyl group -1,3,4- thiadiazoles -
2- yls)-N'- (2,6- difluoro pyridine -4- bases)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidines, N- (the 5- tert-butyl group -1,3,
4- thiadiazoles -2- bases) three kinds of-N'- (2,6- dibromo pyridine -4- bases)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidines appoint
The mixture of meaning ratio is collectively constituted with acceptable auxiliary element in nitrile pyrrole mite ester composition active ingredient, with agricultural chemicals again.
7. the miticide composition according to claim 4 containing TDCA-10 and nitrile pyrrole mite ester is in preventing and treating citrus red mite, apple
Full pawl is full, hawthorn Tetranychus urticae, the purposes on tetranychus vinenensis zacher.
8. miticide composition according to claim 1, this hair is also fallen into for the otherwise biological use such as desinsection, sterilization
Within bright protection domain.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530040A (en) * | 2015-01-19 | 2015-04-22 | 西华大学 | Novel method for synthesizing 1,2,3-thiadiazole-5-formamidine compound |
| CN104610250A (en) * | 2015-01-09 | 2015-05-13 | 西华大学 | 1,2,3-thiadiazole-5-formamidine compound containing three N-heterocycles and synthesis |
| CN104860938A (en) * | 2015-06-08 | 2015-08-26 | 西华大学 | Multi-nitrogen heterocycle thiadiazoles-5-formamidine compound by cyclization method |
| CN104886079A (en) * | 2015-05-28 | 2015-09-09 | 西华大学 | Application of 1,2,3-thiadiazole-5-formamidine heterocyclic compound as acaricide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610250A (en) * | 2015-01-09 | 2015-05-13 | 西华大学 | 1,2,3-thiadiazole-5-formamidine compound containing three N-heterocycles and synthesis |
| CN104530040A (en) * | 2015-01-19 | 2015-04-22 | 西华大学 | Novel method for synthesizing 1,2,3-thiadiazole-5-formamidine compound |
| CN104886079A (en) * | 2015-05-28 | 2015-09-09 | 西华大学 | Application of 1,2,3-thiadiazole-5-formamidine heterocyclic compound as acaricide |
| CN104860938A (en) * | 2015-06-08 | 2015-08-26 | 西华大学 | Multi-nitrogen heterocycle thiadiazoles-5-formamidine compound by cyclization method |
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