CN102919231A - Emulsible granule containing spirodiclofen composition and preparation method thereof - Google Patents
Emulsible granule containing spirodiclofen composition and preparation method thereof Download PDFInfo
- Publication number
- CN102919231A CN102919231A CN2012104362483A CN201210436248A CN102919231A CN 102919231 A CN102919231 A CN 102919231A CN 2012104362483 A CN2012104362483 A CN 2012104362483A CN 201210436248 A CN201210436248 A CN 201210436248A CN 102919231 A CN102919231 A CN 102919231A
- Authority
- CN
- China
- Prior art keywords
- ether
- spiral shell
- polyoxyethylene
- shell mite
- mite ester
- 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.)
- Granted
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- DTDSAWVUFPGDMX-UHFFFAOYSA-N spirodiclofen Chemical compound CCC(C)(C)C(=O)OC1=C(C=2C(=CC(Cl)=CC=2)Cl)C(=O)OC11CCCCC1 DTDSAWVUFPGDMX-UHFFFAOYSA-N 0.000 title abstract description 3
- 239000008187 granular material Substances 0.000 title abstract 5
- 239000005664 Spirodiclofen Substances 0.000 title abstract 2
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 238000009736 wetting Methods 0.000 claims abstract description 13
- 239000003463 adsorbent Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000005469 granulation Methods 0.000 claims abstract description 10
- 230000003179 granulation Effects 0.000 claims abstract description 10
- 238000004898 kneading Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 76
- -1 polyoxyethylene formaldehyde Polymers 0.000 claims description 63
- 150000002148 esters Chemical class 0.000 claims description 45
- 238000004945 emulsification Methods 0.000 claims description 34
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 32
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 21
- 239000007859 condensation product Substances 0.000 claims description 18
- 239000005658 Tebufenpyrad Substances 0.000 claims description 16
- 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 claims description 16
- 239000004480 active ingredient Substances 0.000 claims description 14
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000004359 castor oil Substances 0.000 claims description 10
- 235000019438 castor oil Nutrition 0.000 claims description 10
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 229910019142 PO4 Inorganic materials 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 235000021317 phosphate Nutrition 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 7
- 230000005494 condensation Effects 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- 159000000000 sodium salts Chemical class 0.000 claims description 7
- DMAXMXPDVWTIRV-UHFFFAOYSA-N 2-(2-phenylethyl)phenol Chemical compound OC1=CC=CC=C1CCC1=CC=CC=C1 DMAXMXPDVWTIRV-UHFFFAOYSA-N 0.000 claims description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 6
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical group O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229920001568 phenolic resin Polymers 0.000 claims description 6
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 6
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- TWWCNXGLDZPFQV-XXAVUKJNSA-N [Na].CNCCS(=O)(=O)O.C(CCCCCCC\C=C/CCCCCCCC)(=O)O Chemical compound [Na].CNCCS(=O)(=O)O.C(CCCCCCC\C=C/CCCCCCCC)(=O)O TWWCNXGLDZPFQV-XXAVUKJNSA-N 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000005995 Aluminium silicate Substances 0.000 claims description 4
- OWYSSKOUATWAAO-UHFFFAOYSA-N C1(=CC=CC=C1)C=1C(=C(C(=C(C1)O)C=C)C1=CC=CC=C1)C1=CC=CC=C1 Chemical compound C1(=CC=CC=C1)C=1C(=C(C(=C(C1)O)C=C)C1=CC=CC=C1)C1=CC=CC=C1 OWYSSKOUATWAAO-UHFFFAOYSA-N 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 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 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000002671 adjuvant Substances 0.000 claims description 4
- 235000012211 aluminium silicate Nutrition 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 4
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- RQJQQSAYDFANNM-UHFFFAOYSA-N 2,3-dibutylnaphthalene-1-sulfonic acid;formaldehyde Chemical compound O=C.C1=CC=C2C(S(O)(=O)=O)=C(CCCC)C(CCCC)=CC2=C1 RQJQQSAYDFANNM-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 229920005682 EO-PO block copolymer Polymers 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 125000002877 alkyl aryl group Chemical group 0.000 claims description 3
- 150000001450 anions Chemical class 0.000 claims description 3
- 229960000892 attapulgite Drugs 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004305 biphenyl Substances 0.000 claims description 3
- 235000010290 biphenyl Nutrition 0.000 claims description 3
- 125000006267 biphenyl group Chemical group 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- 229940049964 oleate Drugs 0.000 claims description 3
- 229910052625 palygorskite Inorganic materials 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 229920001285 xanthan gum Polymers 0.000 claims description 3
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 2
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 2
- ZITVKGIRQCDOSX-UHFFFAOYSA-N 1h-cyclopropa[a]naphthalene Chemical compound C1=CC=CC2=C3CC3=CC=C21 ZITVKGIRQCDOSX-UHFFFAOYSA-N 0.000 claims description 2
- QZEDXQFZACVDJE-UHFFFAOYSA-N 2,3-dibutylnaphthalene-1-sulfonic acid Chemical class C1=CC=C2C(S(O)(=O)=O)=C(CCCC)C(CCCC)=CC2=C1 QZEDXQFZACVDJE-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- 229920001353 Dextrin Polymers 0.000 claims description 2
- 239000004375 Dextrin Substances 0.000 claims description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 229920001800 Shellac Polymers 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
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000005037 alkyl phenyl group Chemical group 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 229920001400 block copolymer Polymers 0.000 claims description 2
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 2
- OOCMUZJPDXYRFD-UHFFFAOYSA-L calcium;2-dodecylbenzenesulfonate Chemical compound [Ca+2].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O OOCMUZJPDXYRFD-UHFFFAOYSA-L 0.000 claims description 2
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 235000019425 dextrin Nutrition 0.000 claims description 2
- AQEFLFZSWDEAIP-UHFFFAOYSA-N di-tert-butyl ether Chemical compound CC(C)(C)OC(C)(C)C AQEFLFZSWDEAIP-UHFFFAOYSA-N 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 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 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 2
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims description 2
- 229940043264 dodecyl sulfate Drugs 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- XUZHLZDRCCUWEV-UHFFFAOYSA-N formaldehyde;methyl naphthalene-1-sulfonate Chemical compound O=C.C1=CC=C2C(S(=O)(=O)OC)=CC=CC2=C1 XUZHLZDRCCUWEV-UHFFFAOYSA-N 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- 125000006353 oxyethylene group Chemical group 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- 239000004208 shellac Substances 0.000 claims description 2
- 235000013874 shellac Nutrition 0.000 claims description 2
- 229940113147 shellac Drugs 0.000 claims description 2
- ZLGIYFNHBLSMPS-ATJNOEHPSA-N shellac Chemical compound OCCCCCC(O)C(O)CCCCCCCC(O)=O.C1C23[C@H](C(O)=O)CCC2[C@](C)(CO)[C@@H]1C(C(O)=O)=C[C@@H]3O ZLGIYFNHBLSMPS-ATJNOEHPSA-N 0.000 claims description 2
- 239000000661 sodium alginate Substances 0.000 claims description 2
- 235000010413 sodium alginate Nutrition 0.000 claims description 2
- 229940005550 sodium alginate Drugs 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000008247 solid mixture Substances 0.000 claims description 2
- 239000000454 talc Substances 0.000 claims description 2
- 235000012222 talc Nutrition 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- 229940104261 taurate Drugs 0.000 claims description 2
- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical compound NCCS(O)(=O)=O XOAAWQZATWQOTB-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical class OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims 1
- LRMHFDNWKCSEQU-UHFFFAOYSA-N ethoxyethane;phenol Chemical compound CCOCC.OC1=CC=CC=C1 LRMHFDNWKCSEQU-UHFFFAOYSA-N 0.000 claims 1
- 230000026731 phosphorylation Effects 0.000 claims 1
- 238000006366 phosphorylation reaction Methods 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 9
- 239000000642 acaricide Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 8
- 230000002045 lasting effect Effects 0.000 abstract description 7
- 229940079593 drug Drugs 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 5
- 239000000969 carrier Substances 0.000 abstract 2
- 230000002147 killing effect Effects 0.000 abstract 1
- 238000009313 farming Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 210000000481 breast Anatomy 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 235000009754 Vitis X bourquina Nutrition 0.000 description 6
- 235000012333 Vitis X labruscana Nutrition 0.000 description 6
- 240000006365 Vitis vinifera Species 0.000 description 6
- 235000014787 Vitis vinifera Nutrition 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 241000607479 Yersinia pestis Species 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000003129 miticidal effect Effects 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 5
- 241000207199 Citrus Species 0.000 description 4
- 235000012216 bentonite Nutrition 0.000 description 4
- 235000020971 citrus fruits Nutrition 0.000 description 4
- 235000013399 edible fruits Nutrition 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 239000000375 suspending agent Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 206010034133 Pathogen resistance Diseases 0.000 description 3
- 241000344246 Tetranychus cinnabarinus Species 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- NHFDKKSSQWCEES-UHFFFAOYSA-N dihydrogen phosphate;tris(2-hydroxyethyl)azanium Chemical compound OP(O)(O)=O.OCCN(CCO)CCO NHFDKKSSQWCEES-UHFFFAOYSA-N 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000238876 Acari Species 0.000 description 2
- 235000002566 Capsicum Nutrition 0.000 description 2
- 240000008574 Capsicum frutescens Species 0.000 description 2
- 102000002322 Egg Proteins Human genes 0.000 description 2
- 108010000912 Egg Proteins Proteins 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 241000819999 Nymphes Species 0.000 description 2
- 241001012098 Omiodes indicata Species 0.000 description 2
- 241000488581 Panonychus citri Species 0.000 description 2
- 240000003768 Solanum lycopersicum Species 0.000 description 2
- 244000061458 Solanum melongena Species 0.000 description 2
- 235000002597 Solanum melongena Nutrition 0.000 description 2
- 241001454295 Tetranychidae Species 0.000 description 2
- 241001454293 Tetranychus urticae Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000001390 capsicum minimum Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000000857 drug effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 210000004681 ovum Anatomy 0.000 description 2
- 230000000361 pesticidal effect Effects 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000003449 preventive effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BOTNFCTYKJBUMU-UHFFFAOYSA-N 2-[4-(2-methylpropyl)piperazin-4-ium-1-yl]-2-oxoacetate Chemical compound CC(C)C[NH+]1CCN(C(=O)C([O-])=O)CC1 BOTNFCTYKJBUMU-UHFFFAOYSA-N 0.000 description 1
- 241000254124 Aleyrodidae Species 0.000 description 1
- 241001124076 Aphididae Species 0.000 description 1
- 241000273311 Aphis spiraecola Species 0.000 description 1
- 241000239290 Araneae Species 0.000 description 1
- 241000272639 Brachycaudus mimeuri Species 0.000 description 1
- 241001643374 Brevipalpus Species 0.000 description 1
- 0 CCc1n[n](C)c(*c2ccc(*C)cc2)c1Cl Chemical compound CCc1n[n](C)c(*c2ccc(*C)cc2)c1Cl 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 240000008853 Datura stramonium Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241001221110 Eriophyidae Species 0.000 description 1
- 241000219146 Gossypium Species 0.000 description 1
- 241000258937 Hemiptera Species 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 241000488583 Panonychus ulmi Species 0.000 description 1
- 241001674048 Phthiraptera Species 0.000 description 1
- 241000952063 Polyphagotarsonemus latus Species 0.000 description 1
- 235000000208 Solanum incanum Nutrition 0.000 description 1
- 241000916145 Tarsonemidae Species 0.000 description 1
- 241000488607 Tenuipalpidae Species 0.000 description 1
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- UOAMTSKGCBMZTC-UHFFFAOYSA-N dicofol Chemical compound C=1C=C(Cl)C=CC=1C(C(Cl)(Cl)Cl)(O)C1=CC=C(Cl)C=C1 UOAMTSKGCBMZTC-UHFFFAOYSA-N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000037149 energy metabolism Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003151 ovacidal effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical group OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
Disclosed is an emulsible granule containing spirodiclofen composition and a preparation method thereof. The emulsible granule is composed of components of, by weight, 1-60% of active components, 5-30% of wetting dispersants, 2-15% of solvents, 5-40% of adsorbents, 0-10% of binders and the balance carriers. The active components and liquid auxiliary components in the formula are evenly mixed, and the mixture is absorbed to the carriers; or the active components, the solvents and the liquid auxiliary components are evenly mixed and then mixed with other solid components, an airflow pulverizer is used for smashing the mixture so that granularity of 98% of the mixture reaches 45 mu m, and then the smashed mixture is subjected to kneading and granulation to prepare the emulsible granule. The emulsible granule is reasonable in the components, obvious in mite killing effects instead of simple adding of activity of the components, low in drug use cost, long in lasting period, safe in using, simple in preparation method, safe in storage and transportation, convenient to apply and environment-friendly and is an ideal variety of miticide.
Description
Technical field
But the present invention relates to relate to the emulsification granula that contains spiral shell mite ester composition and its preparation method.
Background technology
Harmful mite kind on China's agricultural is many, and feeding habits are assorted, and host range is wide, and fertility is extremely strong, increases in case evil mite quantity is explosion type, will cause significant damage to crop.Long-term actual agriculture experience shows, on the one hand, repeats and single-mindedly uses a kind of reactive compound and come pest control, can produce resistance to particular active compounds under many circumstances, and the preventive effect of medicament is reduced.
Spiral shell mite ester (spirodiclofen) structure is brand-new, the tool action of contace poison, its mechanism of action is by suppressing the Fatty synthesis in the pest mite body, destroy the energy metabolism activity of acarid, the ovicidal effect is excellent especially, if simultaneously the children mite is also had good action of contace poison, the mite spectrum is wide extremely, the lasting period is long, low toxicity, low-residual, good to people and animals and crop safety, without cross resistance, there is not cross resistance with other existing miticides, be specially adapted to prevent and treat the pest mite class that existing miticide is produced resistance.The mite evil that can be used for the solanaceous crops such as the fruit tree such as citrus, grape and eggplant, capsicum, tomato is administered.Two spotted spider mite, yellow spider, Xiu Pi lice, yellow tea mite, Tetranychus cinnabarinus and Tetranychus urticae etc. are all had fine preventive effect, and the harm of control citrus red mite (crm) reaches 40～50 days.Its main preparation is: the formulations such as missible oil, suspending agent, aqueous emulsion.Its chemical name and structural formula are as follows: 3-(2,4-dichlorophenyl)-2-oxo-1-oxaspiro [4,5]-last of the ten Heavenly stems-3-alkene 4-base-2,2-dimethyl butyrate acid esters.
Tebufenpyrad (tebufenpyrad) belongs to the amide-type miticide. to various mite classes and Semiptera, homoptera pest has tall and erect effect, and the dawn all has immediate effect with efficient to the mite class each vegetative period, and the lasting period is long. such as Tetranychidae (panonychus ulmi, citrus red mite, cotton spider mites, Tetranychus cinnabarinus etc.), Tarsonemidae (the many tarsonemids of side), Eriophyidae (thorn apple rust mite, grape rust mite etc.), Tenuipalpidae (grape brevipalpus), Aphidiadae (black peach aphid, cotten aphid, apple aphid), Aleyrodidae (cassava aleyrodid). with dicofol, fenbutatin oxide, thiazole mite ketone etc. are without cross resistance.Without interior absorption, but osmotically active is arranged, target crop is had splendid selectivity, its main preparation is: the formulations such as suspending agent, missible oil, wetting powder.Its chemical name and structural formula are as follows: N-(4-tertiary butyl benzyl)-4-chloro-3-ethyl-1-methylpyrazole-5-base formamide
And the quality of the formulations of pesticide and preparation is to determine that Pesticidal products is worth and the key factor of effect, adopts different types of auxiliary agent, and a kind of former medicine is processed into the product of different dosage form, different size, the produce an effect difference, even very big-difference is arranged.Missible oil preparation is relatively easy, and good drug efficacy is easy to use, but contains the organic solvents such as a large amount of toluene, dimethylbenzene in the missible oil, and environmental pollution is serious, and all there are hidden danger in production, storage, transportation etc.; Wetting powder has a large amount of dust in producing, using, contaminated environment affects operating personnel's health; Suspending agent then exists bin stability relatively poor, drug effect is not as good as missible oil, therefore, be necessary to develop a kind of environmentally friendly, miticidal effect good, and miticide kind safe to solanaceous crops such as the fruit trees such as citrus, grape and eggplant, capsicum, tomatoes, use cost economy is to satisfy the needs of agricultural production.But the emulsification granula is exactly a kind of novel form that grows up on this basis, advantage with solid pharmaceutical preparation and liquid preparation, be the more comprehensive product of combination property in the current pesticidal preparations, the exploitation of this environmental protection novel form will further strengthen it to the safety of environment, people and animals, crop.But the report of concrete emulsification granula that openly contains spiral shell mite ester composition and preparation method thereof that so far there are no.
Summary of the invention
But the invention provides a kind of emulsification granula that contains spiral shell mite ester composition and preparation method thereof, the present invention is devoted to spiral shell mite ester and tebufenpyrad composition research, with and the research of the novel form of composition, its purpose is: on the one hand, but provide a kind of safety, environmental protection, stable storage, the emulsification granula that contains spiral shell mite ester composition that miticidal effect is good, improve its quick-acting, the service life of lasting period extended period and spiral shell mite ester active component, reduce spraying times, to reach the purpose of the control efficiency that significantly improves crop pests.On the other hand, but a kind of preparation method who contains the emulsification granula of spiral shell mite ester miticide composition is provided.
For addressing the above problem, the present invention adopts following technical scheme:
But a kind of emulsification granula that contains spiral shell mite ester composition, but take the gross weight of emulsification granula as benchmark, its composition forms and the weight percent content of each component is: active ingredient 1～60%, wetting dispersing agent 5～30%, solvent 2～15%, adsorbent 5～40%, binding agent 0～10%, carrier surplus.Effective ingredient is spiral shell mite ester and tebufenpyrad, and the portion rate of spiral shell mite ester and tebufenpyrad weight is 1: 1.Preferably the weight percentage of active ingredient component is the 10%-30% of gross weight in the composition.
Wetting dispersing agent is selected from a kind of in the following material: naphthalenesulfonic acid-formaldehyde condensate (dispersant NNO); the castor oil ethylene oxide adduct; ethylene oxide-propylene oxide block copolymer; the alkylphenol polyoxyethylene formaldehyde condensation products; sodium lignin sulfonate; calcium lignosulfonate; methyl naphthalene sulfonate formaldehyde condensate (Dispersant MF); the sodium salt of alkyl naphthalene sulfonic acid condensation polymer (dispersant D425); N-methyl-fatty acyl group-sodium taurocholate; the alkylphenol polyoxyethylene formaldehyde condensation products; the methanonaphthalene sodium sulfonate; oleic acid methylamino ethylsulfonic acid sodium; epoxidized polyether; to tertbutyl ether; the dibutyl naphthalene sulfonic acid-formaldehyde condensation product; the alkylphenol-polyethenoxy based phosphates; alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate; aralkyl phenol polyethenoxy ether phosphate; alkylphenol polyoxyethylene; the alkylphenol-polyethenoxy polyethenoxy ether; ethoxylated castor oil; polyoxyethylene (n
20) phenethyl phenol ether through reaction oleate, alkylaryl polyoxyethylene poly-oxygen propylene aether, alkylaryl formaldehyde resin APEO, the different thionic acid calcium of oleic acid, triphenyl vinyl phenol polyoxyethylene (n
20) ether phosphoric acid triethanolamine salt, hexichol ethyl phenolic group polyoxyethylene (n
18) ether formaldehyde condensation products, diphenyl phenolic group polyoxyethylene (n
18) polyoxypropylene (n
20) ether, anion and the non-ionic surface active agent compound (agricultural newborn 0201B) of solvent, castor oil polyoxyethylene ether (agricultural newborn BY110), alkyl phenyl APEO (farming breast 100), dibutyl naphthalene sulfonic acids calcium (farming breast 2201), calcium dodecyl benzene sulfonate (farming breast 500), alkyl phenol formaldehyde resin polyoxyethylene ether (Nongru-700), phenethyl phenol polyethenoxy polyethenoxy ether (farming breast 1601), castor oil polyoxyethylene (40) ether (agricultural newborn EL-40), sldium lauryl sulfate, alkylol polyoxyethylene groups ether sodium sulfate, octylphenol polyethylene oxyethylene group ether sulfate, neopelex, Negel, dialkyl succinylsuccinate sulfonate, lauryl alcohol polyethylene glycol oxide base ether sulfonic acid sodium, the alkyl amide taurate, aliphatic alcohol polyethenoxy base ether, alkylphenol-polyethenoxy base ether, the polyoxyethylene poly-oxygen propylene aether block copolymer, in the sorbitan fatty acid ester polyoxyethylene ether one or more; Described adsorbent is selected from a kind of in the following material: one or more in white carbon, bentonite, diatomite, the attapulgite; Described solvent is one or more in 1-METHYLPYRROLIDONE, repefral, dibutyl phthalate, d-hesperidene, diethylene glycol dimethyl ether, solvent naphtha, dimethylbenzene, toluene, the DMF.Described binding agent is a kind of in xanthans, polyethylene glycol, dextrin, gelatin, polyvinyl alcohol, PVP, soluble starch, phenolic resins, shellac, carboxymethyl cellulose, methylcellulose, the sodium alginate.Described carrier is one or more in precipitated calcium carbonate, talcum, potter's clay, kaolin, the atlapulgite.
Method one of the present invention: as shown in Figure 1, select the raw material of following weight ratio: active ingredient 1～60%, wetting dispersing agent 5～30%, solvent 2～15%, adsorbent 5～40%, binding agent 0～10%, carrier surplus; First active ingredient, liquid adjuvants component in the above prescription are mixed and be adsorbed in first on the carrier afterwards, with after other solid constituent is mixed, pulverize by airslide disintegrating mill again, make it granularity and reach 98% by 45 μ m, then through kneading, granulation, make finished product.Method two: as shown in Figure 2, select the raw material of following weight ratio: active ingredient 1～60%, wetting dispersing agent 5～30%, solvent 2～15%, adsorbent 5～40%, binding agent 0～10%, carrier surplus; In will filling a prescription first behind active ingredient, solvent and the liquid adjuvants mixing, then evenly be adsorbed on the component that is crushed to the carrier of granularity 98% by 45 μ m and solid mixture, then through kneading, granulation.
But above-mentioned containing in the spiral shell mite ester composition emulsification granula prescription, preferred wetting dispersing agent is: naphthalenesulfonic acid-formaldehyde condensate (dispersant NNO); ethylene oxide-propylene oxide block copolymer; the alkylphenol polyoxyethylene formaldehyde condensation products; N-methyl-fatty acyl group-sodium taurocholate; the alkylphenol polyoxyethylene formaldehyde condensation products; oleic acid methylamino ethylsulfonic acid sodium; epoxidized polyether; the dibutyl naphthalene sulfonic acid-formaldehyde condensation product; the alkylphenol-polyethenoxy based phosphates; alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate; aralkyl phenol polyethenoxy ether phosphate; alkylphenol polyoxyethylene; the alkylphenol-polyethenoxy polyethenoxy ether; the sodium salt of alkyl naphthalene sulfonic acid condensation polymer (dispersant D425); anion and the non-ionic surface active agent compound (agricultural newborn 0201B) of solvent; phenethyl phenol polyethenoxy polyethenoxy ether (farming breast 1601); alkyl phenol formaldehyde resin polyoxyethylene ether (Nongru-700); castor oil polyoxyethylene ether (agricultural newborn BY110); polyoxyethylene (n
20) phenethyl phenol ether through reaction oleate, alkylaryl polyoxyethylene poly-oxygen propylene aether, alkylaryl formaldehyde resin APEO, the different thionic acid calcium of oleic acid, triphenyl vinyl phenol polyoxyethylene (n
20) ether phosphoric acid triethanolamine salt, hexichol ethyl phenolic group polyoxyethylene (n
18) ether formaldehyde condensation products, diphenyl phenolic group polyoxyethylene (n
18) polyoxypropylene (n
20) ether; Preferred solvent is d-hesperidene, diethylene glycol dimethyl ether, 1-METHYLPYRROLIDONE, dimethylbenzene, solvent naphtha; Preferred adsorbent is white carbon, bentonite; Preferred binder is polyethylene glycol, carboxymethyl cellulose, PVP, soluble starch, polyvinyl alcohol.Preferred vector is precipitated calcium carbonate, kaolin; But the prescription that preferably contains spiral shell mite ester composition emulsifier granula, but take the gross weight of emulsification granula as benchmark, the content of its composition and each component is: active ingredient 10～30%, wetting dispersing agent 10～20%, solvent 5～10%, adsorbent 10～30%, binding agent 0～5%, the carrier surplus.
But the spiral shell mite ester composition emulsification granula that contains of the present invention can directly be watered the rear spraying use of dilution before use by the user.
Using method of the present invention is: when the mites of the fruit trees such as citrus, grape evil reaches index for control (every leaf worm ovum number reaches 10 or every leaf nymph 3-4 head), but use the medicine liquid spray of 20% spiral shell mite ester tebufenpyrad emulsification granula, 1～2ppm concentration.The field medication is generally the first tenday period of a month in May, or 9, October.
Technique effect of the present invention is: but the spiral shell mite ester composition emulsification granula that contains of the present invention, when dilute with water, can make active ingredient well dispersion energy in water, form a kind of common oil-in-water (O/W) type emulsion, because the emulsion particle diameter that forms is very little, can be absorbed rapidly by plant, thereby so that the drug effect of active ingredient is not fully exerted, reduced using dosage, but of the present inventionly contain spiral shell mite ester composition emulsification granula compared with prior art, have the following advantages: 1) good fluidity, non-caked, do not lump.Be easy to packing and use, production, storage, transportation safety, environmentally friendly, to operator's safety; 2) but its liquid wetability of emulsification granula of preparation is good, liquid deposits at target, biologically active is high, quick-acting is good, the lasting period is long, safety is good; 3) preparation method is simple, uses conveniently; 4) component is reasonable, and its miticidal effect is not the simple addition of each composition activity, but it is remarkable to have a miticidal effect, and drug cost is low, and the lasting period is long, uses safety, and storing and transportation safety are environmentally friendly, are a kind of desirable miticide kinds.
Description of drawings
Fig. 1 is the flow chart of manufacture method one;
Fig. 2 is the flow chart of manufacture method two.
Embodiment
The below is described in detail the present invention with best embodiment.
Embodiment one
The part by weight of component is:
First with 2 parts of naphthalenesulfonic acid-formaldehyde condensates, 1.5 part lauryl sodium sulfate, the sodium salt of 3 parts of alkyl naphthalene sulfonic acid condensation polymers, 3 parts of alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate, 20 parts of white carbons and 50.5 parts of diatomite mix mixing in beaker, then at normal temperature, under the condition of normal pressure, add while stirring by 5 parts of spiral shell mite esters, 5 parts of tebufenpyrads, 4 parts of newborn 0201B of farming, 3 parts of d-hesperidenes, 3 parts of mixtures that diethylene glycol dimethyl ether forms, mix, pulverize by airslide disintegrating mill, make it granularity and reach 98% by 45 μ m, at last, add in the material of a certain amount of 2% ethanol water after the above-mentioned pulverizing, through mediating, the scraper plate granulation; But can obtain 10% spiral shell mite ester tebufenpyrad emulsification granula.
Embodiment two
The part by weight of component is:
First with 1 part of carboxymethyl cellulose, 8 parts of bentonites, 1 part of neopelex, 3 parts of N-methyl-fatty acyl group-sodium taurocholates, the sodium salt of 3 parts of alkyl naphthalene sulfonic acid condensation polymers and 49 parts of atlapulgites mix mixing in beaker, then at normal temperature, under the condition of normal pressure, add while stirring by 7.5 parts of spiral shell mite esters, 7.5 part tebufenpyrad, 2 parts of castor oil polyoxyethylene ethers, 2 parts of phenethyl phenol polyethenoxy polyethenoxy ethers, 6 parts of newborn 0201B of farming, 5 parts of 1-METHYLPYRROLIDONEs, 5 parts of mixtures that dimethylbenzene forms, mix, pulverize by airslide disintegrating mill, make it granularity and reach 98% by 45 μ m, at last, add in the material of a certain amount of distilled water after the above-mentioned pulverizing, through mediating, the scraper plate granulation; But can obtain 15% spiral shell mite ester tebufenpyrad emulsification granula.
Embodiment three
The part by weight of component is:
First with 20 parts of white carbons and 36.5 parts of kaolin mixing mixings, pulverize by airslide disintegrating mill, make it granularity and reach 98% by 45 μ m, then under normal temperature, condition of normal pressure, add while stirring by 10 parts of spiral shell mite esters, 10 parts of tebufenpyrads, 3 parts of oleic acid methylamino ethylsulfonic acid sodium, 5 parts of aralkyl phenol polyethenoxy ether phosphates, 5 parts of triphenyl vinyl phenol polyoxyethylene (n
20) ether phosphoric acid triethanolamine salt, 1.5 parts of alkyl phenol formaldehyde resin polyoxyethylene ethers, 3 parts of d-hesperidenes, 5 parts of 1-METHYLPYRROLIDONEs, 1 part of mixture that PEG400 forms, mix, at last, add in the material of a certain amount of distilled water after the above-mentioned pulverizing, through kneading, the scraper plate granulation; But can obtain 20% spiral shell mite ester tebufenpyrad emulsification granula.
Embodiment four
The part by weight of component is:
First with 4 parts of naphthalenesulfonic acid-formaldehyde condensates, 20 parts of white carbons, 10 parts of bentonites, 0.5 part of PVP and 8.5 parts of attapulgite mixing mixings, pulverize by airslide disintegrating mill, make it granularity and reach 98% by 45 μ m, then under normal temperature, condition of normal pressure, add while stirring by 15 parts of spiral shell mite esters, 15 parts of tebufenpyrads, 3 parts of oleic acid methylamino ethylsulfonic acid sodium, 6 parts of hexichol ethyl phenolic group polyoxyethylene (n
18) ether formaldehyde condensation products, 3 parts of alkylaryl formaldehyde resin APEOs, 5 parts of newborn 0201B of farming, 5 parts of diethylene glycol dimethyl ethers, 5 parts of mixtures that dimethylbenzene forms, mix, at last, add in the material of a certain amount of 2% ethanol water after the above-mentioned pulverizing, through kneading, the scraper plate granulation; But can obtain 30% spiral shell mite ester tebufenpyrad emulsification granula.
Embodiment five
First with the sodium salt of 4 parts of alkyl naphthalene sulfonic acid condensation polymers, 25 parts of white carbons, 5 portions of soluble starches and 13 parts of precipitated calcium carbonate mixing mixings, pulverize by airslide disintegrating mill, make it granularity and reach 98% by 45 μ m, then at normal temperature, under the condition of normal pressure, add while stirring by 15 parts of spiral shell mite esters, 15 parts of tebufenpyrads, 4 parts of alkylphenol polyoxyethylene formaldehyde condensation products, 3 parts of aralkyl phenol polyethenoxy ether phosphates, 5 parts of newborn 0201B of farming, 2 parts of farming breasts 1601,4 parts of diethylene glycol dimethyl ethers, 5 parts of mixtures that 1-METHYLPYRROLIDONE forms, mix, at last, add in the material of a certain amount of distilled water after the above-mentioned pulverizing, through mediating, the scraper plate granulation; But can obtain 20% spiral shell mite ester tebufenpyrad emulsification granula.
Embodiment six
With the sodium salt of 15 parts of spiral shell mite esters, 15 parts of tebufenpyrads, 4 parts of naphthalenesulfonic acid-formaldehyde condensates, 2 parts of alkyl naphthalene sulfonic acid condensation polymers, 5 parts of newborn 0201B of farming, 1601,0.1 parts of xanthans of 2 parts of farming breasts, 0.5 part of white carbon, 5 parts of ethylene glycol, 51.4 part deionized water is mixed, start high-shear emulsion machine, after stirring corase grind, under cooling condition, carry out the sand mill fine grinding, grind situation with particles distribution instrument monitoring material, (common d after raw meal particle size is qualified
97Till during less than 10 μ m), can obtain 30% spiral shell mite ester tebufenpyrad suspending agent
Embodiment seven
The test of pesticide effectiveness:
Using method: when the mites of the fruit trees such as citrus, grape evil reaches index for control (every leaf worm ovum number reaches 10 or every leaf nymph 3-4 head), but use the medicine liquid spray of 20% spiral shell mite ester tebufenpyrad emulsification granula, 1～2ppm concentration.The field medication is generally the first tenday period of a month in May, or 9, October.
Indoor biological activity test measurement result (control Tetranychus cinnabarinus)
The characteristics such as the test of pesticide effectiveness result by upper table can find out, but the emulsification granula that contains spiral shell mite ester composition of the present invention compared with prior art, and it is remarkable to have a miticidal effect, and biologically active is high, and the lasting period is long, and cost is low.But the spiral shell mite ester composition emulsification granula that contains provided by the invention, safety in production, use, storage, transportation not only, and the advantage such as it is simple to have processing technology, uses conveniently, environmentally friendly are a kind of desirable miticide kinds.
It should be noted that at last: obviously, above-described embodiment only is for example of the present invention clearly is described, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all embodiments exhaustive.And the apparent variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (9)
1. but emulsification granula that contains spiral shell mite ester composition, it is characterized in that, but take the gross weight of emulsification granula as benchmark, its composition forms and the weight percent content of each component is: active ingredient 1～60%, wetting dispersing agent 5～30%, solvent 2～15%, adsorbent 5～40%, binding agent 0～10%, the carrier surplus.
2. but a kind of emulsification granula that contains spiral shell mite ester composition as claimed in claim 1 is characterized in that described effective ingredient is spiral shell mite ester and tebufenpyrad, and the portion rate of spiral shell mite ester and tebufenpyrad weight is 1: 1.
3. but a kind of emulsification granula that contains spiral shell mite ester composition as claimed in claim 1; it is characterized in that described wetting dispersing agent is selected from naphthalenesulfonic acid-formaldehyde condensate (dispersant NNO); the castor oil ethylene oxide adduct; ethylene oxide-propylene oxide block copolymer; the alkylphenol polyoxyethylene formaldehyde condensation products; sodium lignin sulfonate; calcium lignosulfonate; methyl naphthalene sulfonate formaldehyde condensate; the sodium salt of alkyl naphthalene sulfonic acid condensation polymer; N-methyl-fatty acyl group-sodium taurocholate; the alkylphenol polyoxyethylene formaldehyde condensation products; the methanonaphthalene sodium sulfonate; oleic acid methylamino ethylsulfonic acid sodium; epoxidized polyether; to tertbutyl ether; the dibutyl naphthalene sulfonic acid-formaldehyde condensation product; the alkylphenol-polyethenoxy based phosphates; alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate; aralkyl phenol polyethenoxy ether phosphate; alkylphenol polyoxyethylene; the alkylphenol-polyethenoxy polyethenoxy ether; ethoxylated castor oil; polyoxyethylene phenethyl phenol ether through reaction oleate; the alkylaryl polyoxyethylene poly-oxygen propylene aether; alkylaryl formaldehyde resin APEO; the different thionic acid calcium of oleic acid; triphenyl vinyl phenol APEO phosphorylation triethanolamine salt; hexichol ethyl phenolic group APEO formaldehyde condensation products; diphenyl phenolic group polyoxyethylene poly-oxygen propylene aether; anion and the non-ionic surface active agent compound of solvent; castor oil polyoxyethylene ether; the alkyl phenyl APEO; dibutyl naphthalene sulfonic acids calcium; calcium dodecyl benzene sulfonate; alkyl phenol formaldehyde resin polyoxyethylene ether; phenethyl phenol polyethenoxy polyethenoxy ether; castor oil polyoxyethylene; ether; sldium lauryl sulfate; alkylol polyoxyethylene groups ether sodium sulfate; octylphenol polyethylene oxyethylene group ether sulfate; neopelex; Negel; dialkyl succinylsuccinate sulfonate; lauryl alcohol polyethylene glycol oxide base ether sulfonic acid sodium; the alkyl amide taurate; aliphatic alcohol polyethenoxy base ether; alkylphenol-polyethenoxy base ether; the polyoxyethylene poly-oxygen propylene aether block copolymer; in the sorbitan fatty acid ester polyoxyethylene ether one or more.
4. but a kind of emulsification granula that contains spiral shell mite ester composition as claimed in claim 1 is characterized in that described adsorbent is selected from one or more in white carbon, bentonite, diatomite, the attapulgite.
5. but a kind of emulsification granula that contains spiral shell mite ester composition as claimed in claim 1, it is characterized in that, described solvent is selected from one or more in 1-METHYLPYRROLIDONE, repefral, dibutyl phthalate, d-hesperidene, diethylene glycol dimethyl ether, solvent naphtha, dimethylbenzene, toluene, the DMF.
6. but a kind of emulsification granula that contains spiral shell mite ester composition as claimed in claim 1, it is characterized in that described binding agent is selected from a kind of in xanthans, polyethylene glycol, dextrin, gelatin, polyvinyl alcohol, PVP, soluble starch, phenolic resins, shellac, carboxymethyl cellulose, methylcellulose and the sodium alginate.
7. but a kind of emulsification granula that contains spiral shell mite ester composition as claimed in claim 1 is characterized in that described carrier is selected from one or more in precipitated calcium carbonate, talcum, potter's clay, kaolin, the atlapulgite.
8. but a preparation method who contains the emulsification granula of spiral shell mite ester composition is characterized in that, selects the raw material of following weight ratio: active ingredient 1～60%, wetting dispersing agent 5～30%, solvent 2～15%, adsorbent 5～40%, binding agent 0～10%, the carrier surplus; First active ingredient, liquid adjuvants component in the above prescription are mixed and be adsorbed in first on the carrier afterwards, with after other solid constituent is mixed, pulverize by airslide disintegrating mill again, make it granularity and reach 98% by 45 μ m, then through kneading, granulation, make finished product.
9. but a preparation method who contains the emulsification granula of spiral shell mite ester composition is characterized in that, selects the raw material of following weight ratio: active ingredient 1～60%, wetting dispersing agent 5～30%, solvent 2～15%, adsorbent 5～40%, binding agent 0～10%, the carrier surplus; In will filling a prescription first behind active ingredient, solvent and the liquid adjuvants mixing, then evenly be adsorbed on the component that is crushed to the carrier of granularity 98% by 45 μ m and solid mixture, then through kneading, granulation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210436248.3A CN102919231B (en) | 2012-11-06 | 2012-11-06 | Emulsible granule containing spirodiclofen composition and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210436248.3A CN102919231B (en) | 2012-11-06 | 2012-11-06 | Emulsible granule containing spirodiclofen composition and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102919231A true CN102919231A (en) | 2013-02-13 |
| CN102919231B CN102919231B (en) | 2015-06-10 |
Family
ID=47634281
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210436248.3A Active CN102919231B (en) | 2012-11-06 | 2012-11-06 | Emulsible granule containing spirodiclofen composition and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102919231B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105104390A (en) * | 2015-08-19 | 2015-12-02 | 天峨县平昌生态农业有限公司 | Anti-mite composition containing cycloxaprid and spirodiclofen |
| CN105854728A (en) * | 2016-04-21 | 2016-08-17 | 允发化工（上海）有限公司 | Synthesis method of non-ionic surfactant |
| CN107047548A (en) * | 2017-03-28 | 2017-08-18 | 黑龙江华夏统联农业技术开发有限公司 | A kind of anti-drift agent and the spray adjuvantses including it and its preparation method and application |
| CN111264551A (en) * | 2020-03-30 | 2020-06-12 | 江西汇和化工有限公司 | Method for preparing prochloraz emulsifiable granules by novel feeding machine |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101406192A (en) * | 2008-11-28 | 2009-04-15 | 深圳诺普信农化股份有限公司 | Compositional acaricide and uses thereof |
| CN101406185A (en) * | 2008-10-31 | 2009-04-15 | 淄博新农基农药化工有限公司 | Compositional agent for killing insects and mites with synergistic interaction containing spirodiclofen |
| CN101543213A (en) * | 2008-03-25 | 2009-09-30 | 山东京博控股发展有限公司 | Composition of insecticide and acaricide |
| CN101999346A (en) * | 2010-12-17 | 2011-04-06 | 山西绿海农药科技有限公司 | Emulsifiable granule containing etofenprox composition and preparation method thereof |
| WO2012042002A1 (en) * | 2010-10-01 | 2012-04-05 | Syngenta Participations Ag | Methods for controlling varro mites |
-
2012
- 2012-11-06 CN CN201210436248.3A patent/CN102919231B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101543213A (en) * | 2008-03-25 | 2009-09-30 | 山东京博控股发展有限公司 | Composition of insecticide and acaricide |
| CN101406185A (en) * | 2008-10-31 | 2009-04-15 | 淄博新农基农药化工有限公司 | Compositional agent for killing insects and mites with synergistic interaction containing spirodiclofen |
| CN101406192A (en) * | 2008-11-28 | 2009-04-15 | 深圳诺普信农化股份有限公司 | Compositional acaricide and uses thereof |
| WO2012042002A1 (en) * | 2010-10-01 | 2012-04-05 | Syngenta Participations Ag | Methods for controlling varro mites |
| CN101999346A (en) * | 2010-12-17 | 2011-04-06 | 山西绿海农药科技有限公司 | Emulsifiable granule containing etofenprox composition and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105104390A (en) * | 2015-08-19 | 2015-12-02 | 天峨县平昌生态农业有限公司 | Anti-mite composition containing cycloxaprid and spirodiclofen |
| CN105854728A (en) * | 2016-04-21 | 2016-08-17 | 允发化工（上海）有限公司 | Synthesis method of non-ionic surfactant |
| CN107047548A (en) * | 2017-03-28 | 2017-08-18 | 黑龙江华夏统联农业技术开发有限公司 | A kind of anti-drift agent and the spray adjuvantses including it and its preparation method and application |
| CN107047548B (en) * | 2017-03-28 | 2020-11-13 | 黑龙江华夏统联农业技术开发有限公司 | Anti-drift agent, spraying aid comprising anti-drift agent, and preparation method and application of spraying aid |
| CN111264551A (en) * | 2020-03-30 | 2020-06-12 | 江西汇和化工有限公司 | Method for preparing prochloraz emulsifiable granules by novel feeding machine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102919231B (en) | 2015-06-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101999346B (en) | Emulsifiable granules containing ethofenprox composition and preparation method | |
| CN103125505B (en) | Dispersible oil suspending agent containing florasulam and MCPA-isooctyl | |
| CN103975917A (en) | Propanil Wwater dispersible granules | |
| CN102696630A (en) | Weeding composition and preparation thereof | |
| CN102919231B (en) | Emulsible granule containing spirodiclofen composition and preparation method thereof | |
| CN101856018B (en) | Etofenprox emulsified powder and manufacture method | |
| CN103053554B (en) | Wheat paddock weeding composition | |
| CN105494370A (en) | Pesticide composition prepared from aureonucleomycin and tetramycin | |
| CN105613556B (en) | A kind of dispersible oil-suspending agent of flucarbazone-sodium and mesosulfuron | |
| CN104522010A (en) | Synergistic acaricidal composition containing cyenopyrafen and bifenazate | |
| CN104542618A (en) | Synergetic acaricidal composition containing cyenopyrafen and etoxazole | |
| CN101911940A (en) | Germicide compounded from azoxystrobin, difenoconazole and cyproconazole and preparation method thereof | |
| CN102017960B (en) | Acaricidal composition containing etoxazole and pyridaben | |
| CN103493831B (en) | A kind of Pesticidal combination containing phonetic mite amine and tetronic acid insecticides | |
| CN102763664B (en) | Insecticide composite containing spirodiclofen and bifenazate | |
| CN102893993A (en) | Weeding suspending agent and preparation method thereof | |
| CN101380002A (en) | Insecticide and acaricide composition containing spirodiclofen | |
| CN106035376A (en) | Multifunctional suspended seed coating agent for wheat, and preparation method and application thereof | |
| CN101861868A (en) | Pesticide compound containing penoxsulam and quinclorac and application thereof | |
| CN101669479B (en) | Mite-killing combination | |
| CN102017969B (en) | Pesticide composition containing Bifenazate and Diafenthiuron | |
| CN103355328B (en) | Mite-killing composition containing C20H22Cl2O5 and etoxazole | |
| CN102696642B (en) | Acaricidal composition containing spirodiclofen and cyflumetofen | |
| CN103636614B (en) | Paddy field synergistic weeding composition containing oxadiargyl and mesotrione | |
| CN101317568A (en) | Tetonadiclofen water-dispersible granule and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |