TWI841568B - 可濕性農藥組成物 - Google Patents
可濕性農藥組成物 Download PDFInfo
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- TWI841568B TWI841568B TW108119777A TW108119777A TWI841568B TW I841568 B TWI841568 B TW I841568B TW 108119777 A TW108119777 A TW 108119777A TW 108119777 A TW108119777 A TW 108119777A TW I841568 B TWI841568 B TW I841568B
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- Taiwan
- Prior art keywords
- series
- active ingredient
- mass
- pesticide
- pesticide active
- Prior art date
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- 239000000575 pesticide Substances 0.000 title claims abstract description 135
- 239000000203 mixture Substances 0.000 title claims abstract description 96
- 239000004480 active ingredient Substances 0.000 claims abstract description 116
- 239000004094 surface-active agent Substances 0.000 claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 13
- 150000003839 salts Chemical class 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 6
- -1 polyoxyethylene Polymers 0.000 claims description 144
- 239000003795 chemical substances by application Substances 0.000 claims description 28
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 24
- 239000008101 lactose Substances 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 21
- 239000005909 Kieselgur Substances 0.000 claims description 19
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims description 16
- FHIVAFMUCKRCQO-UHFFFAOYSA-N diazinon Chemical compound CCOP(=S)(OCC)OC1=CC(C)=NC(C(C)C)=N1 FHIVAFMUCKRCQO-UHFFFAOYSA-N 0.000 claims description 13
- 235000002639 sodium chloride Nutrition 0.000 claims description 13
- 230000003115 biocidal effect Effects 0.000 claims description 12
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 12
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 12
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 12
- 238000001238 wet grinding Methods 0.000 claims description 12
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 11
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 150000001720 carbohydrates Chemical class 0.000 claims description 9
- 235000014633 carbohydrates Nutrition 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 239000010949 copper Substances 0.000 claims description 9
- 229940079593 drug Drugs 0.000 claims description 9
- 239000003814 drug Substances 0.000 claims description 9
- NYPJDWWKZLNGGM-UHFFFAOYSA-N fenvalerate Aalpha Natural products C=1C=C(Cl)C=CC=1C(C(C)C)C(=O)OC(C#N)C(C=1)=CC=CC=1OC1=CC=CC=C1 NYPJDWWKZLNGGM-UHFFFAOYSA-N 0.000 claims description 9
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 9
- 235000010755 mineral Nutrition 0.000 claims description 9
- 239000011707 mineral Substances 0.000 claims description 9
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims description 8
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims description 8
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 claims description 7
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 7
- 239000005946 Cypermethrin Substances 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 7
- 229960005424 cypermethrin Drugs 0.000 claims description 7
- KAATUXNTWXVJKI-UHFFFAOYSA-N cypermethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-UHFFFAOYSA-N 0.000 claims description 7
- 150000004676 glycans Chemical class 0.000 claims description 7
- 229920001282 polysaccharide Polymers 0.000 claims description 7
- 239000005017 polysaccharide Substances 0.000 claims description 7
- QWEWLLNSJDTOKH-UHFFFAOYSA-N 1,3-thiazole-2-carboxamide Chemical class NC(=O)C1=NC=CS1 QWEWLLNSJDTOKH-UHFFFAOYSA-N 0.000 claims description 6
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 claims description 6
- QMQZIXCNLUPEIN-UHFFFAOYSA-N 1h-imidazole-2-carbonitrile Chemical class N#CC1=NC=CN1 QMQZIXCNLUPEIN-UHFFFAOYSA-N 0.000 claims description 6
- BNYCHCAYYYRJSH-UHFFFAOYSA-N 1h-pyrazole-5-carboxamide Chemical class NC(=O)C1=CC=NN1 BNYCHCAYYYRJSH-UHFFFAOYSA-N 0.000 claims description 6
- LSBDFXRDZJMBSC-UHFFFAOYSA-N 2-phenylacetamide Chemical compound NC(=O)CC1=CC=CC=C1 LSBDFXRDZJMBSC-UHFFFAOYSA-N 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- VEMKTZHHVJILDY-UXHICEINSA-N bioresmethrin Chemical compound CC1(C)[C@H](C=C(C)C)[C@H]1C(=O)OCC1=COC(CC=2C=CC=CC=2)=C1 VEMKTZHHVJILDY-UXHICEINSA-N 0.000 claims description 6
- 150000004657 carbamic acid derivatives Chemical class 0.000 claims description 6
- 239000000969 carrier Substances 0.000 claims description 6
- ZXQYGBMAQZUVMI-UNOMPAQXSA-N cyhalothrin Chemical compound CC1(C)C(\C=C(/Cl)C(F)(F)F)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-UNOMPAQXSA-N 0.000 claims description 6
- LVQDKIWDGQRHTE-UHFFFAOYSA-N cyromazine Chemical compound NC1=NC(N)=NC(NC2CC2)=N1 LVQDKIWDGQRHTE-UHFFFAOYSA-N 0.000 claims description 6
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 6
- RONFGUROBZGJKP-UHFFFAOYSA-N iminoctadine Chemical compound NC(N)=NCCCCCCCCNCCCCCCCCN=C(N)N RONFGUROBZGJKP-UHFFFAOYSA-N 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 6
- IBBMAWULFFBRKK-UHFFFAOYSA-N picolinamide Chemical class NC(=O)C1=CC=CC=N1 IBBMAWULFFBRKK-UHFFFAOYSA-N 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 150000003230 pyrimidines Chemical class 0.000 claims description 6
- FBQQHUGEACOBDN-UHFFFAOYSA-N quinomethionate Chemical compound N1=C2SC(=O)SC2=NC2=CC(C)=CC=C21 FBQQHUGEACOBDN-UHFFFAOYSA-N 0.000 claims description 6
- XSCHRSMBECNVNS-UHFFFAOYSA-N quinoxaline Chemical compound N1=CC=NC2=CC=CC=C21 XSCHRSMBECNVNS-UHFFFAOYSA-N 0.000 claims description 6
- UCSJYZPVAKXKNQ-HZYVHMACSA-N streptomycin Chemical compound CN[C@H]1[C@H](O)[C@@H](O)[C@H](CO)O[C@H]1O[C@@H]1[C@](C=O)(O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](NC(N)=N)[C@H](O)[C@@H](NC(N)=N)[C@H](O)[C@H]1O UCSJYZPVAKXKNQ-HZYVHMACSA-N 0.000 claims description 6
- 239000011593 sulfur Substances 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- XLNZEKHULJKQBA-UHFFFAOYSA-N terbufos Chemical compound CCOP(=S)(OCC)SCSC(C)(C)C XLNZEKHULJKQBA-UHFFFAOYSA-N 0.000 claims description 6
- BAKXBZPQTXCKRR-UHFFFAOYSA-N thiodicarb Chemical compound CSC(C)=NOC(=O)NSNC(=O)ON=C(C)SC BAKXBZPQTXCKRR-UHFFFAOYSA-N 0.000 claims description 6
- DENPQNAWGQXKCU-UHFFFAOYSA-N thiophene-2-carboxamide Chemical class NC(=O)C1=CC=CS1 DENPQNAWGQXKCU-UHFFFAOYSA-N 0.000 claims description 6
- AIGRXSNSLVJMEA-UHFFFAOYSA-N EPN Chemical compound C=1C=CC=CC=1P(=S)(OCC)OC1=CC=C([N+]([O-])=O)C=C1 AIGRXSNSLVJMEA-UHFFFAOYSA-N 0.000 claims description 5
- 239000005906 Imidacloprid Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 5
- 229940056881 imidacloprid Drugs 0.000 claims description 5
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 claims description 5
- 239000002917 insecticide Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000001103 potassium chloride Substances 0.000 claims description 5
- 235000011164 potassium chloride Nutrition 0.000 claims description 5
- 239000005660 Abamectin Substances 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 229920001353 Dextrin Chemical class 0.000 claims description 4
- 239000004375 Dextrin Chemical class 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 229920000881 Modified starch Chemical class 0.000 claims description 4
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 4
- 239000012965 benzophenone Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Chemical class 0.000 claims description 4
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- 235000010980 cellulose Nutrition 0.000 claims description 4
- 235000019425 dextrin Nutrition 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 229920000609 methyl cellulose Polymers 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 239000001923 methylcellulose Substances 0.000 claims description 4
- 235000010981 methylcellulose Nutrition 0.000 claims description 4
- 235000019426 modified starch Nutrition 0.000 claims description 4
- ZCVAOQKBXKSDMS-PVAVHDDUSA-N (+)-trans-(S)-allethrin Chemical compound CC1(C)[C@H](C=C(C)C)[C@H]1C(=O)O[C@@H]1C(C)=C(CC=C)C(=O)C1 ZCVAOQKBXKSDMS-PVAVHDDUSA-N 0.000 claims description 3
- JWZZKOKVBUJMES-UHFFFAOYSA-N (+-)-Isoprenaline Chemical compound CC(C)NCC(O)C1=CC=C(O)C(O)=C1 JWZZKOKVBUJMES-UHFFFAOYSA-N 0.000 claims description 3
- FJDPATXIBIBRIM-QFMSAKRMSA-N (1R)-trans-cyphenothrin Chemical compound CC1(C)[C@H](C=C(C)C)[C@H]1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 FJDPATXIBIBRIM-QFMSAKRMSA-N 0.000 claims description 3
- XERJKGMBORTKEO-VZUCSPMQSA-N (1e)-2-(ethylcarbamoylamino)-n-methoxy-2-oxoethanimidoyl cyanide Chemical compound CCNC(=O)NC(=O)C(\C#N)=N\OC XERJKGMBORTKEO-VZUCSPMQSA-N 0.000 claims description 3
- SAPGTCDSBGMXCD-UHFFFAOYSA-N (2-chlorophenyl)-(4-fluorophenyl)-pyrimidin-5-ylmethanol Chemical compound C=1N=CN=CC=1C(C=1C(=CC=CC=1)Cl)(O)C1=CC=C(F)C=C1 SAPGTCDSBGMXCD-UHFFFAOYSA-N 0.000 claims description 3
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- CXNPLSGKWMLZPZ-GIFSMMMISA-N (2r,3r,6s)-3-[[(3s)-3-amino-5-[carbamimidoyl(methyl)amino]pentanoyl]amino]-6-(4-amino-2-oxopyrimidin-1-yl)-3,6-dihydro-2h-pyran-2-carboxylic acid Chemical compound O1[C@@H](C(O)=O)[C@H](NC(=O)C[C@@H](N)CCN(C)C(N)=N)C=C[C@H]1N1C(=O)N=C(N)C=C1 CXNPLSGKWMLZPZ-GIFSMMMISA-N 0.000 claims description 3
- DBTMGCOVALSLOR-DEVYUCJPSA-N (2s,3r,4s,5r,6r)-4-[(2s,3r,4s,5r,6r)-3,5-dihydroxy-6-(hydroxymethyl)-4-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]oxy-6-(hydroxymethyl)oxane-2,3,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](CO)O[C@H](O)[C@@H]2O)O)O[C@H](CO)[C@H]1O DBTMGCOVALSLOR-DEVYUCJPSA-N 0.000 claims description 3
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- WCXDHFDTOYPNIE-RIYZIHGNSA-N (E)-acetamiprid Chemical compound N#C/N=C(\C)N(C)CC1=CC=C(Cl)N=C1 WCXDHFDTOYPNIE-RIYZIHGNSA-N 0.000 claims description 3
- PGOOBECODWQEAB-UHFFFAOYSA-N (E)-clothianidin Chemical compound [O-][N+](=O)\N=C(/NC)NCC1=CN=C(Cl)S1 PGOOBECODWQEAB-UHFFFAOYSA-N 0.000 claims description 3
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- IQVNEKKDSLOHHK-FNCQTZNRSA-N (E,E)-hydramethylnon Chemical compound N1CC(C)(C)CNC1=NN=C(/C=C/C=1C=CC(=CC=1)C(F)(F)F)\C=C\C1=CC=C(C(F)(F)F)C=C1 IQVNEKKDSLOHHK-FNCQTZNRSA-N 0.000 claims description 3
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- IAKOZHOLGAGEJT-UHFFFAOYSA-N 1,1,1-trichloro-2,2-bis(p-methoxyphenyl)-Ethane Chemical compound C1=CC(OC)=CC=C1C(C(Cl)(Cl)Cl)C1=CC=C(OC)C=C1 IAKOZHOLGAGEJT-UHFFFAOYSA-N 0.000 claims description 3
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- CSNIZNHTOVFARY-UHFFFAOYSA-N 1,2-benzothiazole Chemical class C1=CC=C2C=NSC2=C1 CSNIZNHTOVFARY-UHFFFAOYSA-N 0.000 claims description 3
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- JWUCHKBSVLQQCO-UHFFFAOYSA-N 1-(2-fluorophenyl)-1-(4-fluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethanol Chemical compound C=1C=C(F)C=CC=1C(C=1C(=CC=CC=1)F)(O)CN1C=NC=N1 JWUCHKBSVLQQCO-UHFFFAOYSA-N 0.000 claims description 3
- IHGSAQHSAGRWNI-UHFFFAOYSA-N 1-(4-bromophenyl)-2,2,2-trifluoroethanone Chemical compound FC(F)(F)C(=O)C1=CC=C(Br)C=C1 IHGSAQHSAGRWNI-UHFFFAOYSA-N 0.000 claims description 3
- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 claims description 3
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- LQDARGUHUSPFNL-UHFFFAOYSA-N 1-[2-(2,4-dichlorophenyl)-3-(1,1,2,2-tetrafluoroethoxy)propyl]1,2,4-triazole Chemical compound C=1C=C(Cl)C=C(Cl)C=1C(COC(F)(F)C(F)F)CN1C=NC=N1 LQDARGUHUSPFNL-UHFFFAOYSA-N 0.000 claims description 3
- WKBPZYKAUNRMKP-UHFFFAOYSA-N 1-[2-(2,4-dichlorophenyl)pentyl]1,2,4-triazole Chemical compound C=1C=C(Cl)C=C(Cl)C=1C(CCC)CN1C=NC=N1 WKBPZYKAUNRMKP-UHFFFAOYSA-N 0.000 claims description 3
- PZBPKYOVPCNPJY-UHFFFAOYSA-N 1-[2-(allyloxy)-2-(2,4-dichlorophenyl)ethyl]imidazole Chemical compound ClC1=CC(Cl)=CC=C1C(OCC=C)CN1C=NC=C1 PZBPKYOVPCNPJY-UHFFFAOYSA-N 0.000 claims description 3
- MGNFYQILYYYUBS-UHFFFAOYSA-N 1-[3-(4-tert-butylphenyl)-2-methylpropyl]piperidine Chemical compound C=1C=C(C(C)(C)C)C=CC=1CC(C)CN1CCCCC1 MGNFYQILYYYUBS-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本發明揭示一種在30℃下為固體的可濕性農藥組成物,其係包含下述式(I)所示之化合物或其農藝/園藝上可容許之酸加成鹽的農藥活性成分(A)、1種以上之添加劑及1種以上之界面活性劑而成。此可濕性農藥組成物其製劑物理性及保存穩定性優異;
Description
本專利申請案係主張先前於日本所申請之專利申請案日本特願2018-110567號(申請日:2018年6月8日)之優先權。此先前專利申請案的全部揭示內容係因引用而成為本說明書的一部分。
本發明係有關於一種農藥組成物,更詳而言之係有關於一種可濕性農藥組成物。
現今為了防治作物之有害生物,而使用各式各樣的農藥。其中,水性懸浮狀農藥組成物(以下亦稱「流動性製劑」)為水基農藥製劑,基於顧及噴灑者及環境的觀點,近年來,其作為安全的農藥製劑之利用價值愈來愈高。
然而,在流動性製劑中,由於活性成分的結晶係懸浮於水中,隨活性成分的不同,有些在保存中會發生水解,或少量的活性成分溶解而再度結晶化,而發生活性成分的結晶生長。在製劑中一旦活性成分進行結晶生長,則會導致防治效果變差,而且亦有可能因物理化學特性變差而導致結硬塊或噴灑時堵塞於噴嘴,因此,就流動
性製劑而言重要的是將結晶生長抑制於容許範圍內。再者,當組成物中之活性成分的結晶粒徑會影響對對象害蟲之效果時,若因結晶生長而導致粒徑增大,則有效果顯著變差之虞,因此,宜長期持續抑制組成物中之活性成分的結晶生長。
專利文獻1及專利文獻2中揭示,包含屬喹啉化合物之一的2-乙基-3,7-二甲基-4-甲氧基羰氧基-6-(4-三氟對甲氧基苯氧基)-喹啉(俗名:氟奎因)作為活性成分的流動性製劑,隨組成物的配方或保存條件的不同,有時氟奎因的粒徑會增大,而無法充分發揮有效成分之效力,而為了解決此問題,作為抑制氟奎因的結晶生長之方法,藉由在組成物中摻混水溶解性纖維素衍生物或聚乙烯基酚,或在組成物中摻混特定的界面活性劑,可抑制結晶生長。
專利文獻3中記載,包含汰芬隆與各種殺生物化合物之組成物可擴大對待防治之有害生物的活性光譜,且亦可產生有效成分之相乘效果。然而,在實施例中,具體的有效成分僅限於汰芬隆與芬諾克或阿維菌素之組合,汰芬隆與所有的有效成分之組合是否有效仍不清楚。而且,在混合劑的乳劑或懸浮劑原液中,於長時間保存時有可能發生活性成分的相互溶解、再結晶、結晶生長、液相的分離、凝聚、結硬塊、有效成分的分解等問題。
專利文獻4中記載,在包含吡蟲啉與有機磷
系化合物之混合劑中,透過使用無晶形二氧化矽,可提供穩定性優良的混合劑。然而,此文獻中雖有針對含量的穩定性之記載,但無針對長期保存後之水合劑的製劑物理性的記載。而且,就此方法,其對特定的農藥活性成分雖屬有效,但對於所有的農藥活性成分是否有效亦仍舊不清楚。
專利文獻5中記載,若將鄰苯二甲醯胺化合物與數種活性物質混合,則可提升殺蟲活性及殺蟎活性,可獲得相乘效果。然而,實施例中僅有調成乳劑之記載,由於乳劑會於保存中析出有效成分,或者係使用有機溶劑,而有使植物發生藥害之虞;而且,由於其為可燃物,近年來就農藥製劑的趨勢而言係轉移至水系製劑,因此,隨有效成分的不同,其非屬最佳者。
[專利文獻1]日本特開2014-144944號公報
[專利文獻2]國際公開第2014/119620號
[專利文獻3]日本特開平9-136805號公報
[專利文獻4]日本特開平3-167107號公報
[專利文獻5]日本特表2006-503084號公報
氟奎因由於係低水溶解度之固體,為使其充分發揮活性成分之效力,則須將粒度減小至一定程度,從而,可藉由濕式粉碎而製造之流動性製劑係合適者,但因流動性製劑為水系製劑,而有氟奎因易因長期保存而受到水解的影響之虞。
再者,基於農業的節省勞力觀點,一般而言農藥製劑係以混合劑開發而於市場上販售;但隨活性成分性質的不同,有混合後之穩定性的問題,有時無法混合。尤其是液體製劑的混合係與各活性成分的製劑特性極為相關,而有可能引起活性成分的相互溶解、再結晶、結晶生長、凝聚、結硬塊、有效成分的分解等問題,使得有些活性成分無法混合。從而,如氟奎因般隨配方的不同而有可能引起結晶生長的物質,尤其有混合後之製劑的穩定性之顧慮。
本案發明人等發現,藉由將氟奎因作成如水合劑或顆粒水合劑的可濕性農藥製劑,可抑制長期保存後的外觀變化或結晶生長,而能夠維持良好的製劑物理性。再者,本案發明人等亦發現,藉由將氟奎因作成可濕性農藥製劑,可解決如上述之混合劑的問題,而能夠與不易在液體製劑中混合的其他活性成分混合。本發明係基於此等見解者。
亦即,本發明目的在於提供一種製劑物理性以及保存穩定性優良的可濕性農藥組成物。
本發明係包含以下發明。
[式中,R1表示COR4’或COOR5(於此,R4’及R5表示C1-4之烷基),R2表示C1-4烷基,R3表示C1-4烷基,X1及X2彼此獨立表示氫原子、或可經鹵素原子取代之C1-4之烷基;惟,X1及X2非同時表示氫原子,X3表示氫原子,W1、W2、及W3各自表示C-Y1、C-Y2、及C-Y3,Y1、Y2、Y3、Y4、及Y5彼此獨立表示氫原子、C1-8烷氧基(此C1-8烷氧基係經相同或相異的1個以上之鹵素原子、及/或由相同或相異的1個以上之鹵素原子取代之C1-4烷氧基所取代者)、或鹵素原子,惟,Y1、Y2、Y3、Y4、及Y5的至少1者係表示C1-8烷
氧基(此C1-8烷氧基係經相同或相異的1個以上之鹵素原子、及/或由相同或相異的1個以上之鹵素原子取代之C1-4烷氧基所取代者),或者,Y1、Y2、Y3、Y4、及Y5亦可相鄰的2個基一同表示由1個以上之鹵素原子取代的-O-(CH2)n-O-(此處n表示1或2),Z表示氧原子]。
(2)如前述(1)之可濕性農藥組成物,其係進一步包含1種以上的其他農藥活性成分(B)而成。
(3)如前述(1)或(2)之可濕性農藥組成物,其中前述農藥活性成分(A)係與界面活性劑共同經濕式粉碎而成的濕式粉碎物之形態,濕式粉碎時所得之懸浮液中的農藥活性成分(A)的體積中位直徑為0.1~5.0μm。
(4)如前述(2)之可濕性農藥組成物,其中前述農藥活性成分(A)及前述農藥活性成分(B)的混合物係與界面活性劑共同經濕式粉碎而成的濕式粉碎物之形態,濕式粉碎時所得之懸浮液中的農藥活性成分(A)及前述農藥活性成分(B)的體積中位直徑為0.1~5.0μm。
(5)如前述(1)~(4)中任一項之可濕性農藥組成物,其中前述農藥活性成分(A)為2-乙基-3,7-二甲基-4-甲氧基羰氧基-6-(4-三氟對甲氧基苯氧基)-喹啉(俗名:氟奎因)。
(6)如前述(1)~(5)中任一項之可濕性農藥組成物,其中前述農藥活性成分(B)為選自由殺蟲劑有效成分及殺菌
劑有效成分所成群組的至少1種成分。
(7)如前述(1)~(6)中任一項之可濕性農藥組成物,其中前述農藥活性成分(B)為選自由有機磷系、胺基甲酸酯系、擬除蟲菊酯系、新菸鹼系、菸鹼系、丁烯酸內酯系、環二烯有機氯系、苯二甲醯胺系、沙蠶毒素系、IGR系、吡咯系、巨環內酯系、保幼激素類似物系、苯甲醯脲系、多殺菌素系、喹唑啉系、苯基吡唑系、噁二嗪系、肼甲醯胺系、苯氧基苄基醯胺系、吡啶偶氮甲胺系、吡啶甲醯胺系、有機矽系、季酮酸系、β-酮腈衍生物系、膦系、METI劑系、BT劑系、銅劑系、硫劑系、多鹵代烷硫基系、碳酸氫鈉系、有機氯系、苯并咪唑系、二羧醯亞胺系、羧醯胺系、苯基醯胺系、烯醯嗎啉系、克絕系、氰基咪唑系、醯基丙胺酸系、噁唑烷酮系、丁內酯系、羥基-(2-胺基-)嘧啶系、異噁唑系、異噻唑酮系、羧酸系、多保淨系、N-苯基胺基甲酸酯系、苯甲醯胺系、噻唑甲醯胺系、苯基脲系、嘧啶胺系、吡唑甲醯胺系、苯基苯甲醯胺系、苯基氧代乙基噻吩醯胺系、吡啶基乙基苯甲醯胺系、呋喃甲醯胺系、噁草酮甲醯胺系、噻唑甲醯胺系、吡唑羧醯胺系、吡啶甲醯胺系、甲氧基丙烯酸酯系、甲氧基胺基甲酸酯系、羥亞胺基乙酸系、羥亞胺基乙醯胺系、噁唑烷二酮系、二氫二噁嗪系、咪唑啉酮系、苄基胺基甲酸酯系、氰基咪唑系、胺磺醯基三唑系、二硝基苯基巴豆酸系、2,6-二硝基苯胺系、三苯基錫系、噻吩羧醯胺系、噻吩甲醯胺系、噻唑并嘧啶胺系、苯胺嘧啶、異丙腎上腺素
抗生素系、六吡喃糖抗生素系、吡喃葡萄糖抗生素系、四環素抗生素系、烯丙氧基喹啉系、喹唑啉系、苯基吡咯系、二甲醯亞胺系、硫代磷酸酯系、二硫代烯烴系、芳烴系、1,2,4-噻二唑系、胺基甲酸酯系、多肽系、哌嗪系、嘧啶系、吡啶系、咪唑系、三唑系、三唑啉酮系、嗎啉系、哌啶系、螺環酮胺系、羥基苯胺系、胺基吡唑啉酮系、硫代胺基甲酸酯系、烯丙胺系、肽基嘧啶核苷系、肉桂酸醯胺系、纈胺酸醯胺胺基甲酸酯系、扁桃酸醯胺系、異苯并呋喃酮系、吡咯喹啉酮系、三唑并苯并噻唑系、環丙烷甲醯胺系、甲醯胺系、丙醯胺系、苯并噻二唑系、苯并異噻唑系、噻二唑甲醯胺系、多醣系、氰基乙醯胺肟系、乙基膦酸酯系、苯二甲酸系、苯并三嗪系、苯磺酸系、噠嗪酮系、硫胺甲酸酯系、苯乙醯胺系、二苯甲酮系、苯甲醯基吡啶系、胍系、氰基亞甲基噻唑烷系、嘧啶酮腙系、二硫代胺基甲酸酯系、鄰苯二甲醯亞胺系、氯腈系、磺胺系、三嗪系、醌系、喹喔啉系、馬來醯亞胺系及中離子系藥劑所成群組的至少1種藥劑。
(8)如前述(1)~(7)中任一項之可濕性農藥組成物,其中前述農藥活性成分(B)為選自由二嗪農(diazinon)、乙醯甲胺磷(acephate)、甲基吡啶磷(azamethyphos)、乙基谷硫磷(azinphos-ethyl)、甲基谷硫磷(azinphos-methyl)、硫線磷(cadusafos)、四氯乙磷(chlorethoxyphos)、毒蟲畏(clofenvinfos)、氯甲磷(chlormephos)、殺螟硫磷(fenitrothion)、異噁唑磷(isoxathion)、毒死蜱(chlorpyrifos)、甲基毒死蜱
(chlorpyrifos methyl)、蠅毒磷(coumaphos)、殺螟腈(cyanophos)、dimeton-S-methyl、敵敵畏(dichlorvos)、百治磷(dicrotophos)、樂果(dimethoate)、甲基毒蟲畏(dimethylvinphos)、乙基硫脲(ethyl thiometon)、EPN、乙硫磷(ethion)、滅線磷(etoprophos)、風扇滿(fanful)、苯線磷(fenamiphos)、倍硫磷(fenthione)、噻唑膦(fosthiazate)、庚蟲磷(heptenophos)、imiciaphos、異柳磷(isofenphos)、滅蚜磷(mecarbam)、甲胺磷(methamidophos)、殺撲磷(methidathion)、速滅磷(mevinphos)、久效磷(monocrotophos)、二溴磷(naled)、氧樂果(omethoate)、乙醯甲胺磷(oxydimethone methyl)、巴拉松(parathion)、甲基巴拉松(methyl parathion)、甲拌磷(phorate)、伏殺磷(phosalone)、亞胺硫磷(phosmet)、磷胺(phosphamidone)、肟(oxime)、甲基嘧啶磷(pirimiphos methyl)、丙溴磷(profenophos)、烯蟲磷(propetamphos)、丙硫磷(prothiophos)、吡唑硫磷(pyraclophos)、噠嗪硫磷(pyridaphenthion)、喹硫磷(quinalfos)、治螟磷(sulfotep)、丁基嘧啶磷(tebupirimfos)、雙硫磷(temefos)、特丁硫磷(terbufos)、殺蟲畏(tetrachlorvinphos)、甲基乙拌(thiomethone)、三唑磷(triazophos)、敵百蟲(trichlorofon)、蚜滅多(vamidothion)、丙硫磷(prothiophos)、馬拉硫磷(malathion)、PAP、DEP、EPN、滅多威(methomyl)、硫雙威(thiodicarb)、丙硫克百威(benflacarb)、丁硫克百威(carbosulfan)、棉鈴威(aranicalb)、氟丙菊酯(acrinathrin)、烯丙菊酯(arethrin)、聯苯菊酯(bifenthrin)、生物烯丙菊酯(bioallethrin)、生物苄呋菊酯
(bioresmethrin)、乙氰菊酯(cycloprothrin)、氟氯氰菊酯(cyfluthrin)、氯氟氰菊酯(cyhalothrin)、氯氰菊酯(cypermethrin)、苯醚氰菊酯(cyphenothrin)、溴氰菊酯(deltamethrin)、右旋烯炔菊酯(empenthrin)、高氰戊菊酯(esfenvalerate)、醚菊酯(etofenprox)、甲氰菊酯(fenpropatrin)、氰戊菊酯(fenvalerate)、氟氰戊菊酯(flucythrinate)、氟氯苯菊酯(flumethrin)、氟胺氰菊酯(fluvalinate)、菊酯(halfenprox)、炔咪菊酯(imiprothrin)、cadethrin、氯菊酯(permethrin)、苯醚菊酯(phenothrin)、炔丙菊酯(prarethrin)、氯氟氰菊酯(cyhalothrin)、七氟菊酯(tefluthrin)、似蟲菊(phthalthrin)、四溴菊酯(tralomethrin)、菊酯(transfluthrin)、DDT、甲氧滴滴梯(methoxychlor)、吡蟲啉(imidacloprid)、噻蟲嗪(thiamethoxam)、噻蟲胺(clothianidin)、啶蟲脒(acetamiprid)、烯啶蟲胺(nitenpyram)、噻蟲啉(thiacloprid)、呋蟲胺(dinotefuran)、硫酸菸鹼、氟啶蟲胺腈(sulfoxaflor)、氟吡呋喃酮(flupyradifurone)、烯蟲乙酯(hydroprene)、烯蟲炔酯(kinoprene)、烯蟲酯(methoprene)、吡丙醚(pyriproxyfen)、氯丹(chlordane)、硫丹(benzoepin)、氟蟲雙醯胺(flubendiamide)、氯蟲苯甲醯胺(chlorantraniliprole)、溴氰蟲醯胺(cyantraniliprole)、殺蟲環(thiocyclam)、殺螟丹(cartap)、殺蟲磺(bensultap)、殺蟲安(thiosultap)、環蟲醯肼(chromafenozide)、甲氧蟲醯肼(methoxyfenozide)、氯蟲醯肼(halofenozide)、蟲醯肼(tebufenozide)、氟啶脲(chlorfluazuron)、trigard、雙甲脒(amitraz)、滅蟻腙(hydramethylnon)、滅蟎醌(acequinosyl)、
嘧蟎酯(fluacripyrim)、喹蟎醚(fenazaquin)、唑蟎酯(fenpyroximate)、畢汰芬(pyrimidifen)、速蟎酮(pyridaben)、吡蟎胺(tebufenpyrad)、唑蟲醯胺(tolfenpyrad)、魚藤(derris)、溴蟲腈(chlorfenapyr)、DNOC、氟蟲胺(sulfuramide)、因滅汀(emamectin)、雷皮菌素(repimectin)、密滅汀(milbemectin)、阿維菌素(abamectin)、多殺菌素(spinosad)、賜諾特(spinetoram)、雙三氟蟲脲(bistrifluron)、除蟲脲(diflubenzuron)、氟環脲(flucycloxuron)、氟鈴脲(hexaflumuron)、虱蟎脲(lufenuron)、氟醯脲(novaluron)、雙苯氟脲(nobiflumuron)、多氟脲(teflubenzuron)、殺鈴脲(triflumuron)、噻嗪酮(buprofezin)、滅蠅胺(cyromazine)、氟蟲吡喹(pyrifluquinazone)、氟蟲腈(fipronil)、乙蟲腈(ethiprole)、苯氧威(fenoxycarb)、茚蟲威(indoxacarb)、氰氟蟲胺(metaflumizone)、螺蟎酯(spirodiclofen)、螺甲蟎酯(spiromesifen)、螺蟲乙酯(spirotetramat)、吡蚜酮(pimetrozin)、氟尼胺(flonicamid)、氯化苦(chloropicrin)、硫醯氟(sulfuryl fluoride)、四蟎嗪(clofentezine)、噻蟎酮(hexythiazox)、氟蟎嗪(diflovidazin)、乙蟎唑(etoxazole)、汰芬隆(diafenthiuron)、三唑錫(azocyclotin)、氫氧化三環己基錫、苯丁錫(fenbutatin oxide)、克蟎特(propargite)、四氯殺蟎碸(tetradifon)、氟矽菊酯(silafluofen)、磷化鋁、磷化鈣、磷化氫、磷化鋅、腈吡蟎酯(cyenopyrafen)、丁氟蟎酯(ciflumethophene)、印楝素(azadiractin)、苯甲醯氧酸鹽、聯苯肼酯(biphenazate)、溴蟎酯(bromopropyrate)、滅蟎猛(quinomethionate)、鋁氟化鈉、三氯殺蟎醇(dicofol)、
三氟甲吡醚(pyridalyl)、無機銅、有機銅、無機硫、聚胺基甲酸酯(polycarbamate)、苯霜靈(benalaxyl)、呋霜靈(fralaxyl)、甲霜靈(metalaxyl)、噁霜靈(oxadixyl)、呋醯胺(ofurace)、乙嘧酚磺酸酯(buprimate)、甲菌定(dimethirimol)、乙菌定(ethirimol)、羥基異噁唑、辛噻酮(octhilinone)、噁喹酸、苯菌靈(benomyl)、多菌靈四唑(carbendazole)、麥穗寧(fuberidazole)、噻菌靈(thiabendazole)、托布津(thiophanate)、甲基硫菌靈(thiophanate-methyl)、乙黴威(dietofencarb)、苯醯菌胺(zoxamide)、噻唑菌胺(etaboxam)、賓克隆(pencycuron)、氟吡菌胺(flupicolide)、二氟林(diflumetrim)、麥鏽靈(benodanil)、氟醯胺(flutolanil)、丙氧滅鏽胺(mepronil)、異丙噻菌胺(isofetamid)、氟吡菌醯胺(fluopirum)、甲呋醯胺(fenfuram)、萎鏽靈(carboxin)、氧化萎鏽靈(oxacarboxin)、賽氟滅(thifluzamide)、苯并烯氟菌胺(benzovindiflupyr)、溴氟唑菌(bixafen)、氟唑菌醯胺(fluxapyroxad)、福拉比(flametopyr)、異皮姆(isopyrazam)、氟唑菌苯胺(penflufen)、吡噻菌胺(penthiopyrade)、環丙吡菌胺(sedaxane)、白克列(boscalid)、嘧菌酯(azoxystrobin)、蜘蛛嘧菌酯(spiderxystrobin)、依諾肝素嘧菌酯(enoxastrobin)、fluphenoxystrobin、啶氧菌酯(picoxystrobin)、唑菌酯(pyraoxystrobin)、菌胺酯(pyraclostrobin)、pyramethostrobin、triclopyricarab、醚菌酯(kresoxim-methyl)、肟菌酯(trifloxystrobin)、醚菌胺(dimoxystrobin)、phenaminstrobin、苯氧菌胺(metominostrobin)、肟醚菌胺(orysastrobin)、噁
唑菌酮(famoxadone)、氟嘧菌酯(fluoxastrobine)、咪唑菌酮(fenamidone)、吡菌苯威(pyribencarb)、氰霜唑(cyazofamid)、吲唑磺(amisulbrom)、樂殺蟎(binapacryl)、硝苯菌酯(meptyldinocap)、消蟎普(dinocup)、氟啶胺(furazinam)、嘧菌腙(ferrimzone)、有機錫、矽噻菌胺(silthiofam)、滅脫定(ametoctradin)、嘧菌環胺(cyprodinil)、嘧菌胺(mepanipyrim)、二甲嘧菌胺(pyrimethanyl)、滅瘟素S(blasticidin S)、春雷黴素(kasugamycin)、鏈黴素(streptomycin)、土黴素(oxytetracycline)、苯氧喹啉(quinoxifene)、丙氧喹啉(proquinazide)、拌種咯(fenpiclonil)、咯菌腈(fludioxonil)、乙菌利(chlozolinate)、異菌脲(iprodione)、腐黴利(procymidone)、乙烯菌核利(vinclozolin)、克瘟散(edifenphos)、異丙苯磷(iprobenfos)、定菌磷(pyrazophos)、稻瘟靈(isoprothiolane)、聯苯、地茂散(chloroneb)、二氯硝基苯(dichlorane)、五氯硝基苯(quintozene)、四氯硝基苯(tecnazene)、甲基立枯磷(tolclofos-methyl)、氯唑靈(echlomezol)、克打淨(iodocarb)、霜黴威(propamocarb)、硫菌(prothiocarb)、枯草芽孢桿菌(bacillus subtilis)、嗪氨靈(trifolin)、啶斑肟(pyriphenox)、pyrixazole、芬路某(fanarimol)、氟苯嘧啶醇(nuarimol)、抑黴唑(imazalil)、噁咪唑(oxosconazole)、稻瘟酯(peflazoate)、咪鮮胺(prochloraz)、賽福座(triflumizole)、戊環唑(azaconazole)、雙苯三唑醇(vitertanol)、糠菌唑(broconazole)、環唑醇(cyproconazole)、醚唑(difenoconazole)、待克立(diniconazole)、氟環唑(epoxiconazole)、乙環唑(etaconazole)、腈苯唑(fenbuconazole)、氟喹唑
(fluquinonazole)、氟矽唑(flusilazole)、粉唑醇(flutriafol)、己唑醇(hexaconazole)、亞胺唑(imibenconazole)、種菌唑(ipconazole)、葉菌唑(metoconazole)、腈菌唑(microbutanyl)、戊菌唑(penconazole)、丙環唑(propiconazole)、矽氟唑(simeconazole)、戊唑醇(tebuconazole)、四氟醚唑(tetraconazole)、三唑酮(triadimefon)、三唑醇(triadimenol)、滅菌唑(triticonazole)、丙硫菌唑(prothioconazole)、殺螟丹(aldimorph)、十二環嗎啉(dodemorph)、丁苯嗎啉(fenpropimorph)、十三嗎啉(tridemorph)、苯鏽(fenpropidin)、粉病靈(piperalin)、螺環菌胺(spiroxamine)、環醯菌胺(fenhexamid)、胺苯吡菌酮(fenpyrazamine)、稗草畏(pyributicarb)、萘替芬(naftifine)、特比萘芬(terbinafine)、有效黴素(validamycin)、多氧黴素(polyoxin)、烯醯嗎啉(dimethomorph)、氟嗎啉(flumorph)、丁吡嗎啉(pyrimorph)、苯噻菌胺(benthiavalicarb)、異丙菌胺(iprovalicarb)、霜霉滅(valifenalate)、雙炔醯菌(mandipropamide)、四氯苯酞(fushalide)、咯喹酮(piroquilone)、三環唑(tricyclazole)、環丙醯菌胺(carpropamide)、雙氯氰菌胺(diclocimet)、氰菌胺(phenoxanyl)、噻二唑素S-甲基(acibenzolar S-methyl)、噻菌靈(probenazole)、噻醯菌胺(tiazinyl)、異噻菌胺(isothianyl)、昆布多醣(laminarin)、霜脲氰(cymoxanil)、三乙膦酸(phosethyl)、葉枯酞(tecloftalam)、菌嗪(triazoxide)、磺菌胺(flusulfamide)、噠菌酮(diclomezin)、磺菌威(metasulfocarb)、環氟菌胺(cyfluphenamide)、苯菌酮
(metrafenone)、pyriofenone、胍(guanidine)、氟噻菌淨(flutianil)、嘧菌腙(ferimsone)、福美鐵(ferbam)、代森錳鋅(manzeb)、代森錳(maneb)、代森聯(methineum)、丙森鋅(propineb)、福美雙(thiuram)、代森鋅(dineb)、克菌丹(captan)、敵菌丹(difoltan)、滅菌丹(folpet)、TPN、抑菌(diclofluanide)、甲苯氟磺胺(trifluanide)、雙胍鹽(guazatine)、雙胍辛胺(iminoctadine)、三嗪(triazine)、二噻酮(dithianone)、滅蟎猛(quinomethionate)、氟亞胺(fluoroimide)、三氟苯嘧啶(triflumezopyrim)及dicloromezotiaz所成群組的至少1種藥劑。
(9)如前述(1)~(8)中任一項之可濕性農藥組成物,其中添加劑為選自由醣類、黏合劑、無機鹽、及礦物質粉末載體所成群組的1種或2種以上之材料。
(10)如前述(1)~(9)中任一項之可濕性農藥組成物,其中醣類係選自由乳糖、糊精、澱粉衍生物及纖維素衍生物所成群組。
(11)如前述(1)~(10)中任一項之可濕性農藥組成物,其中黏合劑係選自由聚乙烯吡咯啶酮、聚乙烯醇、甲基纖維素及羧甲基纖維素所成群組。
(12)如前述(1)~(11)中任一項之可濕性農藥組成物,其中無機鹽為選自由磷酸二氫鉀、氯化鈉、氯化鉀及硫酸銨所成群組的1種或2種以上之無機鹽。
(13)如前述(1)~(12)中任一項之可濕性農藥組成物,其中礦物質粉末載體為選自由白土、矽藻土及火山灰土所
成群組的1種或2種以上之載體。
(14)如前述(1)~(13)中任一項之可濕性農藥組成物,其中界面活性劑係選自由聚氧乙烯烷基醚硫酸鹽、聚氧乙烯醚磷酸鹽、聚氧乙烯化蓖麻油、烷基萘磺酸甲醛縮合物、二辛基磺基琥珀酸鹽及聚羧酸所成群組。
(15)一種製造如前述(1)~(14)中任一項之可濕性農藥組成物的方法,其係包含將農藥活性成分(A)與界面活性劑共同進行濕式粉碎之步驟而成,藉由濕式粉碎所得之懸浮液中的農藥活性成分(A)的體積中位直徑為0.1~5.0μm。
(16)一種製造如前述(2)及(4)~(14)中任一項之可濕性農藥組成物的方法,其係包含將農藥活性成分(A)及農藥活性成分(B)的混合物,與界面活性劑共同進行濕式粉碎之步驟而成,藉由濕式粉碎所得之懸浮液中的農藥活性成分(A)及前述農藥活性成分(B)的體積中位直徑為0.1~5.0μm。
(17)如前述(15)或(16)之方法,其中前述農藥活性成分(A)為2-乙基-3,7-二甲基-4-甲氧基羰氧基-6-(4-三氟對甲氧基苯氧基)-喹啉(俗名:氟奎因)。
本發明之可濕性農藥組成物具有在保存中物理化學性質不會發生變化,保存穩定性優良且防治效果不會變差等特徵,可滿足效果的穩定化與施用時的作業性改善此兩者。再者,根據本發明,亦可達到活性成分的高濃度化及包裝成本降低、穩定性的提升等。
[式中,R1表示COR4’或COOR5(於此,R4’及R5表示C1-4之烷基),R2表示C1-4烷基,R3表示C1-4烷基,X1及X2彼此獨立表示氫原子、或可經鹵素原子取代之C1-4之烷基;惟,X1及X2非同時表示氫原子,X3表示氫原子,W1、W2、及W3各自表示C-Y1、C-Y2、及C-Y3,Y1、Y2、Y3、Y4、及Y5彼此獨立表示氫原子、C1-8烷氧基(此C1-8烷氧基係經相同或相異的1個以上之鹵素原子、及/或由相同或相異的1個以上之鹵素原子取代之C1-4烷氧基所取
代者)、或鹵素原子,惟,Y1、Y2、Y3、Y4、及Y5的至少1者係表示C1-8烷氧基(此C1-8烷氧基係經相同或相異的1個以上之鹵素原子、及/或由相同或相異的1個以上之鹵素原子取代之C1-4烷氧基所取代者),或者,Y1、Y2、Y3、Y4、及Y5亦可相鄰的2個基一同表示由1個以上之鹵素原子取代的-O-(CH2)n-O-(此處n表示1或2),Z表示氧原子]。
農藥活性成分(A)為通式(I)所示之化合物,可為包含於通式(I)的1種化合物,亦可為包含於通式(I)的2種以上之化合物的混合物。根據本發明較佳實施形態,農藥活性成分(A)係採2-乙基-3,7-二甲基-4-甲氧基羰氧基-6-(4-三氟對甲氧基苯氧基)-喹啉(俗名:氟奎因)。
本發明之可濕性農藥組成物亦可進一步包含1種以上之其他農藥活性成分(B)。農藥活性成分(B)不特別限定,可舉出例如殺蟲劑有效成分及殺菌劑有效成分,此等可單獨或以2種以上之組合使用。作為農藥活性成分(B),具體而言可舉出對鱗翅目害蟲、雙翅目害蟲、半翅目害蟲、蟎目害蟲、纓翅目害蟲、鞘翅目害蟲、膜翅目害蟲、直翅目害蟲、小桿圓蟲目害蟲、病毒所引起之病害、細菌所引起之病害及絲狀菌所引起之病害的任一種具有防治效果者。
根據本發明較佳實施形態,農藥活性成分
(B)係採選自由有機磷系、胺基甲酸酯系、擬除蟲菊酯系、新菸鹼系、菸鹼系、丁烯酸內酯系、環二烯有機氯系、苯二甲醯胺系、沙蠶毒素系、IGR系、吡咯系、巨環內酯系、保幼激素類似物系、苯甲醯脲系、多殺菌素系、喹唑啉系、苯基吡唑系、噁二嗪系、肼甲醯胺系、苯氧基苄基醯胺系、吡啶偶氮甲胺系、吡啶甲醯胺系、有機矽系、季酮酸系、β-酮腈衍生物系、膦系、METI劑系、BT劑系、銅劑系、硫劑系、多鹵代烷硫基系、碳酸氫鈉系、有機氯系、苯并咪唑系、二羧醯亞胺系、羧醯胺系、苯基醯胺系、烯醯嗎啉系、克絕系、氰基咪唑系、醯基丙胺酸系、噁唑烷酮系、丁內酯系、羥基-(2-胺基-)嘧啶系、異噁唑系、異噻唑酮系、羧酸系、多保淨系、N-苯基胺基甲酸酯系、苯甲醯胺系、噻唑甲醯胺系、苯基脲系、嘧啶胺系、吡唑甲醯胺系、苯基苯甲醯胺系、苯基氧代乙基噻吩醯胺系、吡啶基乙基苯甲醯胺系、呋喃甲醯胺系、噁草酮甲醯胺系、噻唑甲醯胺系、吡唑羧醯胺系、吡啶甲醯胺系、甲氧基丙烯酸酯系、甲氧基胺基甲酸酯系、羥亞胺基乙酸系、羥亞胺基乙醯胺系、噁唑烷二酮系、二氫二噁嗪系、咪唑啉酮系、苄基胺基甲酸酯系、氰基咪唑系、胺磺醯基三唑系、二硝基苯基巴豆酸系、2,6-二硝基苯胺系、三苯基錫系、噻吩羧醯胺系、噻吩甲醯胺系、噻唑并嘧啶胺系、苯胺嘧啶、異丙腎上腺素抗生素系、六吡喃糖抗生素系、吡喃葡萄糖抗生素系、四環素抗生素系、烯丙氧基喹啉系、喹唑啉系、苯基吡咯系、二甲醯亞胺系、硫代磷
酸酯系、二硫代烯烴系、芳烴系、1,2,4-噻二唑系、胺基甲酸酯系、多肽系、哌嗪系、嘧啶系、吡啶系、咪唑系、三唑系、三唑啉酮系、嗎啉系、哌啶系、螺環酮胺系、羥基苯胺系、胺基吡唑啉酮系、硫代胺基甲酸酯系、烯丙胺系、肽基嘧啶核苷系、肉桂酸醯胺系、纈胺酸醯胺胺基甲酸酯系、扁桃酸醯胺系、異苯并呋喃酮系、吡咯喹啉酮系、三唑并苯并噻唑系、環丙烷甲醯胺系、甲醯胺系、丙醯胺系、苯并噻二唑系、苯并異噻唑系、噻二唑甲醯胺系、多醣系、氰基乙醯胺肟系、乙基膦酸酯系、苯二甲酸系、苯并三嗪系、苯磺酸系、噠嗪酮系、硫胺甲酸酯系、苯乙醯胺系、二苯甲酮系、苯甲醯基吡啶系、胍系、氰基亞甲基噻唑烷系、嘧啶酮腙系、二硫代胺基甲酸酯系、鄰苯二甲醯亞胺系、氯腈系、磺胺系、三嗪系、醌系、喹喔啉系、馬來醯亞胺系及中離子系藥劑所成群組的至少1種藥劑。
根據本發明其他較佳實施形態,農藥活性成分(B)係採選自由二嗪農(diazinon)、乙醯甲胺磷(acephate)、甲基吡啶磷(azamethyphos)、乙基谷硫磷(azinphos-ethyl)、甲基谷硫磷(azinphos-methyl)、硫線磷(cadusafos)、四氯乙磷(chlorethoxyphos)、毒蟲畏(clofenvinfos)、氯甲磷(chlormephos)、殺螟硫磷(fenitrothion)、異噁唑磷(isoxathion)、毒死蜱(chlorpyrifos)、甲基毒死蜱(chlorpyrifos methyl)、蠅毒磷(coumaphos)、殺螟腈(cyanophos)、dimeton-S-methyl、敵敵畏(dichlorvos)、百治磷(dicrotophos)、
樂果(dimethoate)、甲基毒蟲畏(dimethylvinphos)、乙基硫脲(ethyl thiometon)、EPN、乙硫磷(ethion)、滅線磷(etoprophos)、風扇滿(fanful)、苯線磷(fenamiphos)、倍硫磷(fenthione)、噻唑膦(fosthiazate)、庚蟲磷(heptenophos)、imiciaphos、異柳磷(isofenphos)、滅蚜磷(mecarbam)、甲胺磷(methamidophos)、殺撲磷(methidathion)、速滅磷(mevinphos)、久效磷(monocrotophos)、二溴磷(naled)、氧樂果(omethoate)、乙醯甲胺磷(oxydimethone methyl)、巴拉松(parathion)、甲基巴拉松(methyl parathion)、甲拌磷(phorate)、伏殺磷(phosalone)、亞胺硫磷(phosmet)、磷胺(phosphamidone)、肟(oxime)、甲基嘧啶磷(pirimiphos methyl)、丙溴磷(profenophos)、烯蟲磷(propetamphos)、丙硫磷(prothiophos)、吡唑硫磷(pyraclophos)、噠嗪硫磷(pyridaphenthion)、喹硫磷(quinalfos)、治螟磷(sulfotep)、丁基嘧啶磷(tebupirimfos)、雙硫磷(temefos)、特丁硫磷(terbufos)、殺蟲畏(tetrachlorvinphos)、甲基乙拌(thiomethone)、三唑磷(triazophos)、敵百蟲(trichlorofon)、蚜滅多(vamidothion)、丙硫磷(prothiophos)、馬拉硫磷(malathion)、PAP、DEP、EPN、滅多威(methomyl)、硫雙威(thiodicarb)、丙硫克百威(benflacarb)、丁硫克百威(carbosulfan)、棉鈴威(aranicalb)、氟丙菊酯(acrinathrin)、烯丙菊酯(arethrin)、聯苯菊酯(bifenthrin)、生物烯丙菊酯(bioallethrin)、生物苄呋菊酯(bioresmethrin)、乙氰菊酯(cycloprothrin)、氟氯氰菊酯(cyfluthrin)、氯氟氰菊酯(cyhalothrin)、氯氰菊酯
(cypermethrin)、苯醚氰菊酯(cyphenothrin)、溴氰菊酯(deltamethrin)、右旋烯炔菊酯(empenthrin)、高氰戊菊酯(esfenvalerate)、醚菊酯(etofenprox)、甲氰菊酯(fenpropatrin)、氰戊菊酯(fenvalerate)、氟氰戊菊酯(flucythrinate)、氟氯苯菊酯(flumethrin)、氟胺氰菊酯(fluvalinate)、菊酯(halfenprox)、炔咪菊酯(imiprothrin)、cadethrin、氯菊酯(permethrin)、苯醚菊酯(phenothrin)、炔丙菊酯(prarethrin)、氯氟氰菊酯(cyhalothrin)、七氟菊酯(tefluthrin)、似蟲菊(phthalthrin)、四溴菊酯(tralomethrin)、菊酯(transfluthrin)、DDT、甲氧滴滴梯(methoxychlor)、吡蟲啉(imidacloprid)、噻蟲嗪(thiamethoxam)、噻蟲胺(clothianidin)、啶蟲脒(acetamiprid)、烯啶蟲胺(nitenpyram)、噻蟲啉(thiacloprid)、呋蟲胺(dinotefuran)、硫酸菸鹼、氟啶蟲胺腈(sulfoxaflor)、氟吡呋喃酮(flupyradifurone)、烯蟲乙酯(hydroprene)、烯蟲炔酯(kinoprene)、烯蟲酯(methoprene)、吡丙醚(pyriproxyfen)、氯丹(chlordane)、硫丹(benzoepin)、氟蟲雙醯胺(flubendiamide)、氯蟲苯甲醯胺(chlorantraniliprole)、溴氰蟲醯胺(cyantraniliprole)、殺蟲環(thiocyclam)、殺螟丹(cartap)、殺蟲磺(bensultap)、殺蟲安(thiosultap)、環蟲醯肼(chromafenozide)、甲氧蟲醯肼(methoxyfenozide)、氯蟲醯肼(halofenozide)、蟲醯肼(tebufenozide)、氟啶脲(chlorfluazuron)、trigard、雙甲脒(amitraz)、滅蟻腙(hydramethylnon)、滅蟎醌(acequinosyl)、嘧蟎酯(fluacripyrim)、喹蟎醚(fenazaquin)、唑蟎酯
(fenpyroximate)、畢汰芬(pyrimidifen)、速蟎酮(pyridaben)、吡蟎胺(tebufenpyrad)、唑蟲醯胺(tolfenpyrad)、魚藤(derris)、溴蟲腈(chlorfenapyr)、DNOC、氟蟲胺(sulfuramide)、因滅汀(emamectin)、雷皮菌素(repimectin)、密滅汀(milbemectin)、阿維菌素(abamectin)、多殺菌素(spinosad)、賜諾特(spinetoram)、雙三氟蟲脲(bistrifluron)、除蟲脲(diflubenzuron)、氟環脲(flucycloxuron)、氟鈴脲(hexaflumuron)、虱蟎脲(lufenuron)、氟醯脲(novaluron)、雙苯氟脲(nobiflumuron)、多氟脲(teflubenzuron)、殺鈴脲(triflumuron)、噻嗪酮(buprofezin)、滅蠅胺(cyromazine)、氟蟲吡喹(pyrifluquinazone)、氟蟲腈(fipronil)、乙蟲腈(ethiprole)、苯氧威(fenoxycarb)、茚蟲威(indoxacarb)、氰氟蟲胺(metaflumizone)、螺蟎酯(spirodiclofen)、螺甲蟎酯(spiromesifen)、螺蟲乙酯(spirotetramat)、吡蚜酮(pimetrozin)、氟尼胺(flonicamid)、氯化苦(chloropicrin)、硫醯氟(sulfuryl fluoride)、四蟎嗪(clofentezine)、噻蟎酮(hexythiazox)、氟蟎嗪(diflovidazin)、乙蟎唑(etoxazole)、汰芬隆(diafenthiuron)、三唑錫(azocyclotin)、氫氧化三環己基錫、苯丁錫(fenbutatin oxide)、克蟎特(propargite)、四氯殺蟎碸(tetradifon)、氟矽菊酯(silafluofen)、磷化鋁、磷化鈣、磷化氫、磷化鋅、腈吡蟎酯(cyenopyrafen)、丁氟蟎酯(ciflumethophene)、印楝素(azadiractin)、苯甲醯氧酸鹽、聯苯肼酯(biphenazate)、溴蟎酯(bromopropyrate)、滅蟎猛(quinomethionate)、鋁氟化鈉、
三氯殺蟎醇(dicofol)、三氟甲吡醚(pyridalyl)、無機銅、有機銅、無機硫、聚胺基甲酸酯(polycarbamate)、苯霜靈(benalaxyl)、呋霜靈(fralaxyl)、甲霜靈(metalaxyl)、噁霜靈(oxadixyl)、呋醯胺(ofurace)、乙嘧酚磺酸酯(buprimate)、甲菌定(dimethirimol)、乙菌定(ethirimol)、羥基異噁唑、辛噻酮(octhilinone)、噁喹酸、苯菌靈(benomyl)、多菌靈四唑(carbendazole)、麥穗寧(fuberidazole)、噻菌靈(thiabendazole)、托布津(thiophanate)、甲基硫菌靈(thiophanate-methyl)、乙黴威(dietofencarb)、苯醯菌胺(zoxamide)、噻唑菌胺(etaboxam)、賓克隆(pencycuron)、氟吡菌胺(flupicolide)、二氟林(diflumetrim)、麥鏽靈(benodanil)、氟醯胺(flutolanil)、丙氧滅鏽胺(mepronil)、異丙噻菌胺(isofetamid)、氟吡菌醯胺(fluopirum)、甲呋醯胺(fenfuram)、萎鏽靈(carboxin)、氧化萎鏽靈(oxacarboxin)、賽氟滅(thifluzamide)、苯并烯氟菌胺(benzovindiflupyr)、溴氟唑菌(bixafen)、氟唑菌醯胺(fluxapyroxad)、福拉比(flametopyr)、異皮姆(isopyrazam)、氟唑菌苯胺(penflufen)、吡噻菌胺(penthiopyrade)、環丙吡菌胺(sedaxane)、白克列(boscalid)、嘧菌酯(azoxystrobin)、蜘蛛嘧菌酯(spiderxystrobin)、依諾肝素嘧菌酯(enoxastrobin)、fluphenoxystrobin、啶氧菌酯(picoxystrobin)、唑菌酯(pyraoxystrobin)、菌胺酯(pyraclostrobin)、pyramethostrobin、triclopyricarab、醚菌酯(kresoxim-methyl)、肟菌酯(trifloxystrobin)、醚菌胺(dimoxystrobin)、phenaminstrobin、苯氧菌胺(metominostrobin)、肟醚菌胺(orysastrobin)、噁唑
菌酮(famoxadone)、氟嘧菌酯(fluoxastrobine)、咪唑菌酮(fenamidone)、吡菌苯威(pyribencarb)、氰霜唑(cyazofamid)、吲唑磺(amisulbrom)、樂殺蟎(binapacryl)、硝苯菌酯(meptyldinocap)、消蟎普(dinocup)、氟啶胺(furazinam)、嘧菌腙(ferrimzone)、有機錫、矽噻菌胺(silthiofam)、滅脫定(ametoctradin)、嘧菌環胺(cyprodinil)、嘧菌胺(mepanipyrim)、二甲嘧菌胺(pyrimethanyl)、滅瘟素S(blasticidin S)、春雷黴素(kasugamycin)、鏈黴素(streptomycin)、土黴素(oxytetracycline)、苯氧喹啉(quinoxifene)、丙氧喹啉(proquinazide)、拌種咯(fenpiclonil)、咯菌腈(fludioxonil)、乙菌利(chlozolinate)、異菌脲(iprodione)、腐黴利(procymidone)、乙烯菌核利(vinclozolin)、克瘟散(edifenphos)、異丙苯磷(iprobenfos)、定菌磷(pyrazophos)、稻瘟靈(isoprothiolane)、聯苯、地茂散(chloroneb)、二氯硝基苯(dichlorane)、五氯硝基苯(quintozene)、四氯硝基苯(tecnazene)、甲基立枯磷(tolclofos-methyl)、氯唑靈(echlomezol)、克打淨(iodocarb)、霜黴威(propamocarb)、硫菌(prothiocarb)、枯草芽孢桿菌(bacillus subtilis)、嗪氨靈(trifolin)、啶斑肟(pyriphenox)、pyrixazole、芬路某(fanarimol)、氟苯嘧啶醇(nuarimol)、抑黴唑(imazalil)、噁咪唑(oxosconazole)、稻瘟酯(peflazoate)、咪鮮胺(prochloraz)、賽福座(triflumizole)、戊環唑(azaconazole)、雙苯三唑醇(vitertanol)、糠菌唑(broconazole)、環唑醇(cyproconazole)、醚唑(difenoconazole)、待克立(diniconazole)、氟環唑(epoxiconazole)、乙環唑
(etaconazole)、腈苯唑(fenbuconazole)、氟喹唑(fluquinonazole)、氟矽唑(flusilazole)、粉唑醇(flutriafol)、己唑醇(hexaconazole)、亞胺唑(imibenconazole)、種菌唑(ipconazole)、葉菌唑(metoconazole)、腈菌唑(microbutanyl)、戊菌唑(penconazole)、丙環唑(propiconazole)、矽氟唑(simeconazole)、戊唑醇(tebuconazole)、四氟醚唑(tetraconazole)、三唑酮(triadimefon)、三唑醇(triadimenol)、滅菌唑(triticonazole)、丙硫菌唑(prothioconazole)、殺螟丹(aldimorph)、十二環嗎啉(dodemorph)、丁苯嗎啉(fenpropimorph)、十三嗎啉(tridemorph)、苯鏽(fenpropidin)、粉病靈(piperalin)、螺環菌胺(spiroxamine)、環醯菌胺(fenhexamid)、胺苯吡菌酮(fenpyrazamine)、稗草畏(pyributicarb)、萘替芬(naftifine)、特比萘芬(terbinafine)、有效黴素(validamycin)、多氧黴素(polyoxin)、烯醯嗎啉(dimethomorph)、氟嗎啉(flumorph)、丁吡嗎啉(pyrimorph)、苯噻菌胺(benthiavalicarb)、異丙菌胺(iprovalicarb)、霜霉滅(valifenalate)、雙炔醯菌(mandipropamide)、四氯苯酞(fushalide)、咯喹酮(piroquilone)、三環唑(tricyclazole)、環丙醯菌胺(carpropamide)、雙氯氰菌胺(diclocimet)、氰菌胺(phenoxanyl)、噻二唑素S-甲基(acibenzolar S-methyl)、噻菌靈(probenazole)、噻醯菌胺(tiazinyl)、異噻菌胺(isothianyl)、昆布多醣(laminarin)、霜脲氰(cymoxanil)、三乙膦酸(phosethyl)、葉枯酞(tecloftalam)、菌嗪(triazoxide)、磺菌胺(flusulfamide)、噠菌酮(diclomezin)、磺菌威(metasulfocarb)、環氟菌胺(cyfluphenamide)、苯菌酮(metrafenone)、pyriofenone、
胍(guanidine)、氟噻菌淨(flutianil)、嘧菌腙(ferimsone)、福美鐵(ferbam)、代森錳鋅(manzeb)、代森錳(maneb)、代森聯(methineum)、丙森鋅(propineb)、福美雙(thiuram)、代森鋅(dineb)、克菌丹(captan)、敵菌丹(difoltan)、滅菌丹(folpet)、TPN、抑菌(diclofluanide)、甲苯氟磺胺(trifluanide)、雙胍鹽(guazatine)、雙胍辛胺(iminoctadine)、三嗪(triazine)、二噻酮(dithianone)、滅蟎猛(quinomethionate)、氟亞胺(fluoroimide)、三氟苯嘧啶(triflumezopyrim)及dicloromezotiaz所成群組的至少1種藥劑。
可使用於本發明之添加劑不特別限定,可舉出例如醣類、黏合劑、無機鹽、礦物質粉末載體等,此等可單獨或以2種以上之組合使用。
可使用於本發明之醣類不特別限定,可舉出乳糖、果糖、葡萄糖、麥芽糖、澱粉、糊精、蔗糖、海藻糖、纖維素類等,此等可單獨或以2種以上之組合使用。醣類較佳為乳糖及糊精。就此等的用量,相對於本發明之可濕性農藥組成物100質量份較佳為0.1~50質量份的範圍,更佳為5~25質量份的範圍。特佳之具體的醣類可舉出例如Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)、Pineflow((商品名)、澱粉衍生物、松谷化學工業(股)製)等。根據本發明較佳實施形態,本發明之可濕性農藥組成物係採包含醣類者。
可使用於本發明之黏合劑不特別限定,可舉出聚乙烯醇、聚乙烯吡咯啶酮、甲基纖維素、羧甲基纖維
素、木質素鹽等,此等可單獨或以2種以上之組合使用。黏合劑較佳為聚乙烯吡咯啶酮及聚乙烯醇。就此等的用量,相對於本發明之可濕性農藥組成物100質量份較佳為0.1~20質量份的範圍,更佳為1~10質量份的範圍。特佳之具體的黏合劑可舉出例如CREEJUS K-30((商品名)、聚乙烯吡咯啶酮、第一工業製藥(股)公司製)、KURARAY POVAL((商品名)、聚乙烯醇、KURARAY(股)公司製)、Metolose MCE-4((商品名)、甲基纖維素、信越化學工業(股)公司製)、CELLOGEN 7A((商品名)、羧甲基纖維素鈉、(股)公司製)等。
可使用於本發明之無機鹽不特別限定,可舉出磷酸二氫鉀、氯化鉀、氯化鈉、硫酸銨、碳酸鈉、硫酸鈉等,此等可單獨或以2種以上之組合使用。無機鹽較佳為磷酸二氫鉀及氯化鉀。就此等的用量,相對於本發明之可濕性農藥組成物100質量份較佳為0.1~20質量份的範圍,更佳為1~10質量份的範圍。
可使用於本發明之礦物質粉末載體不特別限定,可舉出矽藻土、酸性白土、火山灰土、滑石、黏土、碳酸鈣、膨潤土、鎂鋁海泡石、海泡石、沸石、矽酸鈣等,此等可單獨或以2種以上之組合使用。礦物質粉末載體較佳為矽藻土、酸性白土及火山灰土。就此等的用量,相對於本發明之可濕性農藥組成物100質量份較佳為0~70質量份的範圍,更佳為0~50質量份的範圍。特佳之具體的礦物質粉末載體可舉出例如MAARLITE 735C((商品
名)、白土、丸中白土(股)公司製)、Radiolite F((商品名)、矽藻土、昭和化學工業(股)公司製)、Radiolite #200((商品名)、矽藻土、昭和化學工業(股)公司製)、TOPCO-PERLITE((商品名)、火山灰土、昭和化學工業(股)公司製)等。
本發明中所使用之界面活性劑不特別限定,較佳為聚氧乙烯烷基醚硫酸鹽、聚氧乙烯化蓖麻油、聚氧乙烯三苯乙烯醚磷酸鹽、烷基萘磺酸甲醛縮合物、二辛基磺基琥珀酸鹽、聚羧酸等,可單獨或混合2種以上使用,混合時的比例亦可自由選擇。本發明之可濕性農藥組成物中的界面活性劑的含量不特別限定,相對於本發明之可濕性農藥組成物100質量份較佳為0.1~20質量份的範圍,特佳為1.0~10.0質量份的範圍。特佳之具體的界面活性劑可舉出例如SOLPOL 7868((商品名)、東邦化學工業(股))Morwet D-425 Powder((商品名)、LION AKZO(股))、New Cargen WG-5((商品名)、竹本油脂(股))、SOLPOL 5050((商品名)、東邦化學工業(股))等。
於本發明一實施形態中,農藥有效成分與其他成分的摻混比例,例如相對於農藥有效成分與其他成分的合計100質量份,係採農藥有效成分(A)為1~30質量份,較佳為5~20質量份;農藥活性成分(B)為0~50質量份,較佳為0~25質量份;其他成分為20~99質量份,較佳為55~95質量份的比例。
本發明之可濕性農藥組成物例如可藉由包含
將農藥活性成分(A)、或農藥活性成分(A)與農藥活性成分(B)的混合物,與界面活性劑共同進行濕式粉碎之步驟的方法來製造。更具體而言,例如可藉由在溶有界面活性劑的水中添加農藥活性成分(A)、或農藥活性成分(A)與農藥活性成分(B)之組合並加以混合,再以批次式珠磨機或者DYNO-MILL等濕式粉碎機微粒化處理成期望的粒徑而得到漿液,並對此漿液添加添加劑或添加劑與農藥活性成分(B)之組合並加以混合,而製造本發明之可濕性農藥組成物。其後,若要將劑型製成水合劑,藉由進行乾燥、乾式粉碎並篩分成所需粒度等,或者藉由在造粒後並加以乾燥後進行粉碎,可予以製劑化。若要將劑型製成顆粒水合劑,則藉由視需求進行加水捏合,並以造粒機造粒成直徑0.5~1.0mm的粒狀物後加以乾燥,再篩分成所需粒度的方法,或者同樣地對經微粒子化的漿液添加混合添加劑及農藥活性成分(A)或者農藥活性成分(B),並使用噴霧乾燥機等進行噴霧乾燥的方法,可予以製劑化。
本發明之製法中的濕式粉碎之方法不特別限定,可應用周知作為一般的濕式粉碎法之方法。此種方法可舉出例如將農藥活性成分(A)、或農藥活性成分(A)與農藥活性成分(B)之組合與水及界面活性劑共同進行粉碎的方法。一般而言,濕式粉碎漿液的農藥活性成分係經粉碎成0.5~5μm左右。
濕式粉碎漿液中亦可視需求適宜摻混增黏劑、防凍劑、防腐劑、消泡劑、結晶生長抑制劑等周知之
添加劑。增黏劑可舉出黃原膠、刺槐豆膠等天然多醣類、鎂鋁矽酸鹽等膨潤土類、羧甲基纖維素等半合成多醣類。防凍劑可舉出尿素、或丙二醇、乙二醇等二醇類。防腐劑可舉出1,2-苯并異噻唑啉-3-酮、2-甲基-異噻唑啉-3-酮等。消泡劑可舉出聚矽氧系乳液等。
作為本發明中可使用之粉碎機,就乾式粉碎,可舉出磨咖啡機、錘磨機、Neamill、針磨機、PowerMill、噴射磨機等,可根據待粉碎物質的性質與目的來選擇使用何種粉碎機。就濕式粉碎,可舉出批次式珠磨機、DYNO-MILL等粉碎機;使用之珠粒可舉出玻璃珠、氧化鋯珠等。就珠粒粒徑,較佳使用0.3~1.0mm的範圍者,更佳使用0.5~0.7mm的範圍者。透過使用小粒徑珠粒,可調製小體積中位直徑的粉碎液。
根據本發明較佳實施形態,在本發明之可濕性農藥組成物中,農藥活性成分(A)、或農藥活性成分(A)與農藥活性成分(B)的混合物係與界面活性劑共同經濕式粉碎而成的濕式粉碎物之形態,濕式粉碎時所得之懸浮液中的農藥活性成分(A)、或農藥活性成分(A)及農藥活性成分(B)的體積中位直徑為0.1~5.0μm。具有此種體積中位直徑的農藥活性成分,在增強有害生物的防治效果上為較佳者。
本發明中所稱「體積中位直徑」,係表示根據體積基準的平均粒徑,意指將其集體的全部體積設為100%而求出累積曲線時,達該累積曲線的50%之點的粒
徑。本發明之可濕性農藥組成物中的農藥活性成分粒子的體積中位直徑可使用市售之雷射繞射式粒度分布測定裝置,例如SALD2200(島津製作所(股)製)等測定體積中位直徑的大小及其分布狀態而求得。
本發明之製法中,要將農藥活性成分粒子調整成目標體積中位直徑,界面活性劑的種類及濃度,以及使活性成分分散之粉碎條件(珠粒粒徑、粉碎機種、攪拌速度、送液速度等)係發揮重要的作用。由於活性成分的粒徑係大致由粉碎條件及製作分散系統的步驟來決定,因此,重要的是在此步驟中配合活性成分的粒子設計來選擇界面活性劑及粉碎方法。
本發明之製法中,農藥活性成分或添加劑的混合可藉由物理混合來進行,於混合步驟中宜進行機械式攪拌及混合,藉由固定條件可達均勻混合。攪拌可使用葉片、螺旋槳、渦輪等;混合則可使用捏合機、帶式混合機、V型混合機、雙錐式混合機、SPARTAN混合機、葉片混料機、轉鼓混合機等。
本發明之製法中的造粒方法不特別限定,可使用擠出造粒法、攪拌造粒法、轉動造粒法、加壓式造粒法、流動層造粒法等標準方法,其中較佳藉由擠出造粒法來進行。擠出造粒法係將前述混合物進行混練,使混合物通過既定大小的貫孔而將粒子成型,並視需求將粒子切成既定的大小再加以乾燥、篩分的方法。造粒機可使用薄金屬製多孔板、Multigran(DALTON(股)公司製)、Basketreuser
(DALTON(股)公司製)等,貫孔的直徑為0.1mm~2mm左右,較佳為0.3mm~1mm。
本發明之製法中的乾燥方法不特別限定,若為20g以下的少量較佳為恆溫槽,若為20g以上則較佳為流動層乾燥機等。乾燥溫度較佳為40℃~60℃,乾燥時間較佳為15分鐘~2小時左右。
本發明之可濕性農藥組成物其崩解性及分散性優良,經長期間保存後仍具有良好的製劑物理性。根據本發明之製造方法,可在將以氟奎因為首的活性成分的體積中位直徑維持於小粒徑的狀態下轉換成顆粒水合劑;而且,可達到迄此在液體製劑中可能因混合而發生之活性成分的溶解或分解、再結晶、結晶生長、凝聚、結硬塊等由穩定性與物理化學性方面而言不易混合之農藥活性成分的混合。由此而言,本發明係極為有用。
以下,根據實施例對本發明更詳細地加以說明,惟本發明不受此等實施例所限定。
實施例及比較例之製劑中的農藥活性成分粒子的體積中位直徑係使用以下分析儀器及分析條件來測定。
分析機器:雷射繞射式粒度分布測定裝置SALD-2200、(島津製作所(股)製);
測定方式:雷射繞射及雷射散射法;測定範圍:0.03~1000μm;光源:半導體雷射(波長680nm、輸出功率3mW);試樣槽:流式處理槽方式;試樣槽材質:石英玻璃製;軟體:WingSALD-2200;分析試料:就體積中位直徑測定方法,流動性劑係取500mg分散於50mL的水中,以粒度分布位測定機對分散液進行測定。若為顆粒水合劑時係取200mg分散於10mL的水,為了去除載體等的粗大粒子,使載體自然沉降或以離心分離等使其沉降後,以粒度分布測定機對上澄液進行測定。
在容量100mL的燒瓶中,將SOLPOL 5050((商品名)、二辛基磺基琥珀酸鈉、東邦化學工業(股)製)0.5質量份、SOLPOL 7868((商品名)、聚氧乙烯烷基醚硫酸鹽、東邦化學工業(股)製)3質量份、Morwet D-425 Powder((商品名)、烷基萘磺酸甲醛縮合物、LION AKZO(股)製)3質量份、ANTIFOAM E-20((商品名)、聚矽氧系消泡劑、花王(股)製)0.25質量份、及氟奎因原體(99.0%)10質量份添加於15.2質量份的水中並加以混合攪拌。將所得混合物以批次式珠磨機進行濕式粉碎,調製成氟奎因的粉碎液(A)。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為
1.0μm。
在容量100mL的燒瓶中,將SOLPOL 5050((商品名)、二辛基磺基琥珀酸鈉、東邦化學工業(股)製)0.5質量份、SOLPOL 7868((商品名)、聚氧乙烯烷基醚硫酸鹽、東邦化學工業(股)製)3質量份、Morwet D-425 Powder((商品名)、烷基萘磺酸甲醛縮合物、LION AKZO(股)製)3質量份、ANTIFOAM E-20((商品名)、聚矽氧系消泡劑、花王(股)製)0.25質量份、氟奎因原體(99.0%)10.5質量份、及吡蟲啉原體(98.7%)10.4質量份添加於42.5質量份的水中並加以混合攪拌。將所得混合物以批次式珠磨機進行濕式粉碎,調製成氟奎因及吡蟲啉混合粉碎液(B)。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為1.4μm。
將丙二醇28.6質量份、LOADPOL 23((商品名)、黃原膠、SOLBAY日華(股)製)0.6質量份、Kinipia F((商品名)、膨潤土、KUNIMINE工業(股)製)1質量份、PROXEL GXL(S)((商品名)、殺菌劑、Lonza(股)製)0.9質量份、及水53.6質量份混合,調製成增黏劑液。
對將Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)6質量份、New Cargen WG-5((商品名)、聚羧酸鈉、竹本油脂(股)製)1質量份、Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)2質量份、及磷酸二氫鉀(和光純藥試劑)1質量份混合並以磨咖啡機粉碎的混合物適宜添加前述氟奎因粉碎液(A)4質量份及水並進行捏合,使其通過0.5mm多孔板而造粒成柱狀。將所得柱狀顆粒在50℃恆溫槽中乾燥2小時後,使其通過孔徑1mm的篩進行整粒,而得到10%氟奎因顆粒水合劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為1.0μm。
到實施例1中添加4質量份的粉碎液(A)前全以同樣方式調製並進行捏合後在50℃恆溫槽中乾燥2小時,再度以磨咖啡機粉碎,而得到10%氟奎因水合劑。
除將實施例1之Radiolite F改為MAARLITE 735C((商品名)、酸性白土、丸中白土(股)製)以外係全以同樣方式製造,而得到10%氟奎因顆粒水合劑。
除將實施例1之Radiolite F改為TOPCO-PERLITE((商
品名)、發泡波來鐵、昭和化學工業(股)製)以外係全以同樣方式製造,而得到10%氟奎因顆粒水合劑。
除將實施例1之磷酸二氫鉀(和光純藥試劑)1質量份改為氯化鉀(和光純藥試劑)1質量份以外係全以同樣方式製造,而得到10%氟奎因顆粒水合劑。
除將實施例1之Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)6質量份改為4質量份、Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)2質量份改為1質量份、New Cargen WG-5((商品名)、聚羧酸鈉、竹本油脂(股)製)1質量份改為0.5質量份、磷酸二氫鉀(和光純藥試劑)1質量份改為0.5質量份以外係全以同樣方式製造,而得到15%氟奎因顆粒水合劑。
對將Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)29質量份、New Cargen WG-5((商品名)、聚羧酸鈉、竹本油脂(股)製)2.5質量份、Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)5質量份、磷酸二氫鉀(和光純藥試劑)1質量份、及CREEJUS K-30((商品名)、聚乙烯吡咯啶酮、第一工業製藥(股)製)1質量
份混合並以錘磨機粉碎的混合物添加前述氟奎因粉碎液(A)30質量份並進行捏合,在50℃恆溫槽中乾燥2小時後,對所得粉體進一步添加氟奎因粉碎液(A)10質量份並進行捏合,再適宜加水後,以Multigran MG-55(商品名、造粒機、DALTON(股)製)使其通過篩網Φ0.5mm而造粒成柱狀顆粒。將所得柱狀顆粒,使用流動層乾燥機以50℃乾燥30分鐘後,使其通過孔徑1mm的篩進行整粒,而得到20%氟奎因顆粒水合劑。
除將實施例7之CREEJUS K-30((商品名)、聚乙烯吡咯啶酮、第一工業製藥(股)製)1質量份改為Pineflow((商品名)、澱粉衍生物、松谷化學工業(股)製)1質量份以外係全以同樣方式製造,而得到20%氟奎因顆粒水合劑。
對將Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)5.6質量份、吡蟲啉1.2質量份(純度98.7%)、New Cargen WG-5((商品名)、聚羧酸鈉、竹本油脂(股)製)1質量份、Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)2質量份、及CREEJUS K-30((商品名)、聚乙烯吡咯啶酮、第一工業製藥(股)製)0.2質量份混合並以磨咖啡機粉碎的混合物適宜添加前述氟奎因粉碎液(A)4質量份及水並進行捏合,使其通過0.5mm多孔板而造粒成
柱狀。將所得柱狀顆粒在50℃恆溫槽中乾燥2小時後,使其通過孔徑1mm的篩進行整粒,而得到10%氟奎因及10%吡蟲啉的混合顆粒水合劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為1.3μm。
到實施例9中添加氟奎因粉碎液(A)前全以同樣方式調製,在50℃恆溫槽中乾燥2小時後以磨咖啡機粉碎,而得到10%氟奎因及10%吡蟲啉的混合水合劑。
對將Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)4.4質量份、New Cargen WG-5((商品名)、聚羧酸鈉、竹本油脂(股)製)1質量份、Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)2質量份、磷酸二氫鉀(和光純藥試劑)0.5質量份、及CREEJUS K-30((商品名)、聚乙烯吡咯啶酮、第一工業製藥(股)製)0.2質量份混合並以磨咖啡機粉碎的混合物適宜添加前述粉碎液(B)8質量份及水並進行捏合,使其通過0.5mm多孔板而造粒成柱狀。將所得柱狀顆粒在50℃恆溫槽中乾燥2小時後,使其通過孔徑1mm的篩進行整粒,而得到8%氟奎因及8%吡蟲啉的混合顆粒水合劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為1.5μm。
到實施例11中添加粉碎液(B)前全以同樣方式調製,在50℃恆溫槽中乾燥2小時後以磨咖啡機粉碎,而得到8%氟奎因及8%吡蟲啉的混合水合劑。
對將Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)3.7質量份、New Cargen WG-5((商品名)、聚羧酸鈉、竹本油脂(股)製)1.5質量份、Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)3質量份、磷酸二氫鉀(和光純藥試劑)1質量份、CREEJUS K-30((商品名)、聚乙烯吡咯啶酮、第一工業製藥(股)製)0.2質量份、及可芬諾原體(純度95.0%)0.6質量份混合並以磨咖啡機粉碎的混合物適宜添加前述粉碎液(A)4質量份及水並進行捏合,使其通過0.5mm多孔板而造粒成柱狀。將所得柱狀顆粒在50℃恆溫槽中乾燥2小時後,使其通過孔徑1mm的篩進行整粒,而得到10%氟奎因及5%可芬諾的混合顆粒水合劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為1.0μm。
到實施例13中添加粉碎液(A)前全以同樣方式調製,在50℃恆溫槽中乾燥2小時後以磨咖啡機粉碎,而得到10%氟奎因及5%可芬諾的混合水合劑。
對將Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)6質量份、New Cargen WG-5((商品名)、聚羧酸鈉、竹本油脂(股)製)1.0質量份、Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)2質量份、及CREEJUS K-30((商品名)、聚乙烯吡咯啶酮、第一工業製藥(股)製)0.2質量份混合並以磨咖啡機粉碎的混合物適宜添加前述粉碎液(A)2質量份與Shotgun((商品名)、二嗪農EW製劑、日本化藥(股)製)3質量份的混合液及水並進行捏合,使其通過0.5mm多孔板而造粒成柱狀。將所得柱狀顆粒在50℃恆溫槽中乾燥2小時後,使其通過孔徑1mm的篩進行整粒,而得到5%氟奎因及10%二嗪農的混合顆粒水合劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為2.9μm。
到實施例15中添加粉碎液(A)與Shotgun前全以同樣方式調製,在50℃恆溫槽中乾燥2小時後以磨咖啡機粉碎,而得到5%氟奎因及10%二嗪農的混合水合劑。
除將實施例15之Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)6質量份改為4.6質量份、Shotgun((商品
名)、二嗪農EW製劑、日本化藥(股)製)3質量份改為二嗪農原體(純度95.4%)3.2質量份以外係全以同樣方式調製,而得到5%氟奎因及25%二嗪農的混合顆粒水合劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為3.1μm。
到實施例17中添加粉碎液(A)及二嗪農原體前全以同樣方式調製,在50℃恆溫槽中乾燥2小時後以磨咖啡機粉碎,而得到5%氟奎因及25%二嗪農的混合水合劑。
除將實施例15之Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)6質量份改為5.8質量份、Shotgun((商品名)、二嗪農EW製劑、日本化藥(股)製)3質量份改為Bellkute Flowable((商品名)、雙胍辛胺烷苯磺酸鹽(顯示值30%)、日本曹達(股)製)4質量份以外係全以同樣方式調製,而得到5%氟奎因及10%雙胍辛胺烷苯磺酸鹽的混合顆粒水合劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為1.7μm。
到實施例19中添加粉碎液(A)及Bellkute Flowable前全以同樣方式調製,在50℃恆溫槽中乾燥2小時後以磨咖啡
機粉碎,而得到5%氟奎因及10%雙胍辛胺烷苯磺酸鹽的混合水合劑。
除將實施例15之Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)6質量份改為5.8質量份、Shotgun((商品名)、二嗪農EW製劑、日本化藥(股)製)3質量份改為Labin Flowable((商品名)、硫雙威(顯示值33.5%)、Bayer CropScience(股)製)4質量份以外係全以同樣方式調製,而得到5%氟奎因及11%硫雙威的混合顆粒水合劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為1.5μm。
到實施例21中添加粉碎液(A)及Labin Flowable前全以同樣方式調製,在50℃恆溫槽中乾燥2小時後以磨咖啡機粉碎,而得到5%氟奎因及11%硫雙威的混合水合劑。
在容量1L的燒瓶中,將SOLPOL 5050((商品名)、二辛基磺基琥珀酸鈉、東邦化學工業(股)製)5質量份、SOLPOL 7868((商品名)、聚氧乙烯烷基醚硫酸鹽、東邦化學工業(股)製)30質量份、Morwet D-425 Powder((商品名)、烷基萘磺酸甲醛縮合物、LION AKZO(股)製)30質量份、ANTIFOAM E-20((商品名)、聚矽氧系消泡劑、花王(股)
製)2.5質量份、及氟奎因原體(99.0%)100質量份添加於152質量份的水中並加以混合攪拌。將所得混合物以批次式珠磨機進行濕式粉碎,調製成氟奎因的粉碎液。對此粉碎液100質量份添加混合水101.3質量份、及增黏劑液84.7質量份,而得到10%氟奎因的流動性製劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為0.8μm。
對粉碎液(B)70.4質量份添加混合增黏劑液29.6質量份,而得到10%氟奎因及10%吡蟲啉的混合流動性製劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為1.4μm。
在容量100mL的燒瓶中,將SOLPOL 5050((商品名)、二辛基磺基琥珀酸鈉、東邦化學工業(股)製)0.5質量份、SOLPOL 7868((商品名)、聚氧乙烯烷基醚硫酸鹽、東邦化學工業(股)製)3質量份、Morwet D-425 Powder((商品名)、烷基萘磺酸甲醛縮合物、LION AKZO(股)製)3質量份、ANTIFOAM E-20((商品名)、聚矽氧系消泡劑、花王(股)製)0.25質量份、氟奎因原體(99.0%)10.5質量份、及殺蟲環原體(87.0%)29.0質量份添加於24.2質量份的水中並加以混合攪拌。將所得混合物以批次式珠磨機進行濕式粉碎,調製成氟奎因及殺蟲環的混合粉碎液。對所得粉碎液
70.4質量份添加混合增黏劑液29.6質量份,而得到10%氟奎因及25%殺蟲環的混合流動性製劑。以雷射繞射式粒度分布測定機測定粒度的結果,體積中位直徑為2.5μm。
如表1所示,將比較例1中所得之氟奎因10%流動性製劑與一般的市售劑以重量比1:1混合,而得到氟奎因混合流動性製劑。又,調製之混合流動性製劑的粒度係以雷射繞射式粒度分布測定機測定。
除將實施例1之WG-5((商品名)、聚羧酸鈉、竹本油脂(股)製)1質量份改為1.5質量份、Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)2質量份改為0質量份、Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)6質量份改為無水硫酸鈉(和光純藥試劑)2.5質量
份、磷酸二氫鉀(和光純藥試劑)1質量份改為磷酸氫二鈉(和光純藥試劑)5質量份、粉碎液(A)4質量份改為8.2質量份以外係全以同樣方式製造,而得到19%氟奎因顆粒水合劑。
除將實施例1之Radiolite F((商品名)、矽藻土、昭和化學工業(股)製)6質量份改為無水硫酸鈉(和光純藥試劑)2.2質量份、Hilmar 5030 Extra Fine Grind Lactose((商品名)、乳糖、Hilmar(股)製)2質量份改為0質量份、磷酸二氫鉀(和光純藥試劑)1質量份改為磷酸氫二鈉(和光純藥試劑)4質量份、粉碎液(A)4質量份改為8.2質量份,並進一步添加SAN X P252((商品名)、木質素、日本製紙工業(股)製)1.3質量份以外係全以同樣方式製造,而得到20%氟奎因顆粒水合劑。
對將水合劑用黏土6質量份、Carplex #80((商品名)、白碳、Evonik Japan(股)製)2質量份及SAN X P-252((商品名)、木質素鹽、日本製紙(股)製)2質量份混合並以磨咖啡機粉碎的混合物適宜添加前述粉碎液(A)4質量份及水並進行捏合,使其通過0.5mm多孔板而造粒成柱狀。將所得柱狀顆粒在50℃恆溫槽中乾燥2小時後,使其通過孔徑1mm的篩進行整粒,而得到10%氟奎因顆粒水合劑。
除將試驗區35之水合劑用黏土6質量份改為4.7質量份,並進一步重新添加吡蟲啉原體(純度98.7%)1.3質量份以外係全以同樣方式製造,而得到10%氟奎因及10%吡蟲啉的混合顆粒水合劑。
將實施例1、7、9、11、13、15、17、19、21、23及25以及比較例1~32中所製造之製劑封入於容積10mL有蓋玻璃瓶,在54℃的恆溫槽中保存14日。將保存後的製劑放置於室溫下數日,依目視確認外觀的變化。此外,就一部分的試樣,係以結晶生長率來評定體積中位直徑的變化。
就體積中位直徑測定方法,比較例之流動性劑係取500mg分散於50mL的水中,以粒度分布位測定機對分散液進行測定。實施例之顆粒水合劑係取200mg分散於10mL的水中,為了去除載體等的粗大粒子而使載體自然沉降30~60分鐘後,以粒度分布測定機對上澄液進行測定。
將結果示於以下表2。
由表2可知,就實施例之製劑,54℃下2週後之製劑仍為固體而外觀無變化,且結晶生長率的變化亦較小,故體積中位直徑亦呈穩定。相對於此,比較例之流動性劑,在大部分的製劑中外觀有分離或固化等變化,且在數個製劑中確認體積中位直徑大幅增大。就此種變化的原因,研判係氟奎因與混合對象之活性成分的相容性,或製劑配方中的界面活性劑等原料產生交互作用,而於製劑系統內發生活性成分的溶解或析出等現象,而導致製劑物理性惡化。
就實施例1、3~9、11、13、15、17、19及21以及試驗區33~36之顆粒水合劑,係分別封入於容積10mL有蓋玻璃瓶,在54℃的恆溫槽中保存14日。對容積250mL的有栓量筒加入硬度3度的水250mL,並添加製劑250mg,評定加入水後粒子落下而崩解的情形(崩解性),同時,自投入水中1分鐘後起以每1分鐘30次之速度倒轉,測定完全達到分散前的倒轉次數。將結果示於表3。
由表3可知,就實施例之製劑,保存於54℃後之製劑其崩解性及分散性亦優良,投入水中後迅速開始崩解,以較少的倒轉次數即達到均勻的分散狀態。相對於此,試驗區33~36之顆粒水合劑則非屬崩解性良好者,保存於54℃後之製劑,倒轉10次仍未完成分散。研判這是因為,由於原料使用氟奎因等活性成分的粉碎液,將試驗區33~36所使用之原料與粉碎液混合時,粉碎液中的細微粒子均勻地分布於粉體原料中,於擠出造粒、乾燥後製劑變硬,而導致崩解性顯著變差。基於實施例與試驗區33~36之構成上的差異,研判顆粒水合劑係以含有醣類為宜。再者,研判顆粒水合劑宜含有白土、矽藻土或火山灰土作為礦物質粉末載體。
Claims (10)
- 一種在30℃下為固體的可濕性農藥組成物,其係包含2-乙基-3,7-二甲基-4-甲氧基羰氧基-6-(4-三氟對甲氧基苯氧基)-喹啉之農藥活性成分(A)、1種以上之添加劑及1種以上之界面活性劑而成,前述農藥活性成分(A)係與界面活性劑共同進行濕式粉碎而成的濕式粉碎物之形態,濕式粉碎時所得之懸浮液中的農藥活性成分(A)的體積中位直徑為0.1~5.0μm,前述添加劑包含醣類及礦物質粉末載體,前述醣類係選自由乳糖、糊精、澱粉衍生物及纖維素衍生物所成群組,前述礦物質粉末載體為選自由白土、矽藻土及火山灰土所成群組的1種或2種以上之載體,前述界面活性劑係選自由聚氧乙烯烷基醚硫酸鹽、聚氧乙烯醚磷酸鹽、聚氧乙烯化蓖麻油、烷基萘磺酸甲醛縮合物、二辛基磺基琥珀酸鹽及聚羧酸所成群組。
- 如請求項1之可濕性農藥組成物,其係進一步包含1種以上的其他農藥活性成分(B)而成,前述農藥活性成分(A)及前述農藥活性成分(B)的混合物係與界面活性劑共同進行濕式粉碎而成的濕式粉碎物之形態,濕式粉碎時所得之懸浮液中的農藥活性成分(A)及前述農藥活性成分(B)的體積中位直徑為0.1~5.0μm。
- 如請求項2之可濕性農藥組成物,其中前述農藥活性成分(B)為選自由殺蟲劑有效成分及殺菌劑有效成分所成群組的至少1種成分。
- 如請求項2之可濕性農藥組成物,其中前述農藥活性成分(B)為選自由有機磷系、胺基甲酸酯系、擬除蟲菊酯系、新菸鹼系、菸鹼系、丁烯酸內酯系、環二烯有機氯系、苯二甲醯胺系、沙蠶毒素系、IGR系、吡咯系、巨環內酯系、保幼激素類似物系、苯甲醯脲系、多殺菌素系、喹唑啉系、苯基吡唑系、噁二嗪系、肼甲醯胺系、苯氧基苄基醯胺系、吡啶偶氮甲胺系、吡啶甲醯胺系、有機矽系、季酮酸系、β-酮腈衍生物系、膦系、METI劑系、BT劑系、銅劑系、硫劑系、多鹵代烷硫基系、碳酸氫鈉系、有機氯系、苯并咪唑系、二羧醯亞胺系、羧醯胺系、苯基醯胺系、烯醯嗎啉系、克絕系、氰基咪唑系、醯基丙胺酸系、噁唑烷酮系、丁內酯系、羥基-(2-胺基-)嘧啶系、異噁唑系、異噻唑酮系、羧酸系、多保淨系、N-苯基胺基甲酸酯系、苯甲醯胺系、噻唑甲醯胺系、苯基脲系、嘧啶胺系、吡唑甲醯胺系、苯基苯甲醯胺系、苯基氧代乙基噻吩醯胺系、吡啶基乙基苯甲醯胺系、呋喃甲醯胺系、噁草酮甲醯胺系、噻唑甲醯胺系、吡唑羧醯胺系、吡啶甲醯胺系、甲氧基丙烯酸酯系、甲氧基胺基甲酸酯系、羥亞胺基乙酸系、羥亞胺基乙醯胺系、噁唑烷二酮系、二氫二噁嗪 系、咪唑啉酮系、苄基胺基甲酸酯系、氰基咪唑系、胺磺醯基三唑系、二硝基苯基巴豆酸系、2,6-二硝基苯胺系、三苯基錫系、噻吩羧醯胺系、噻吩甲醯胺系、噻唑并嘧啶胺系、苯胺嘧啶、異丙腎上腺素抗生素系、六吡喃糖抗生素系、吡喃葡萄糖抗生素系、四環素抗生素系、烯丙氧基喹啉系、喹唑啉系、苯基吡咯系、二甲醯亞胺系、硫代磷酸酯系、二硫代烯烴系、芳烴系、1,2,4-噻二唑系、胺基甲酸酯系、多肽系、哌嗪系、嘧啶系、吡啶系、咪唑系、三唑系、三唑啉酮系、嗎啉系、哌啶系、螺環酮胺系、羥基苯胺系、胺基吡唑啉酮系、硫代胺基甲酸酯系、烯丙胺系、肽基嘧啶核苷系、肉桂酸醯胺系、纈胺酸醯胺胺基甲酸酯系、扁桃酸醯胺系、異苯并呋喃酮系、吡咯喹啉酮系、三唑并苯并噻唑系、環丙烷甲醯胺系、甲醯胺系、丙醯胺系、苯并噻二唑系、苯并異噻唑系、噻二唑甲醯胺系、多醣系、氰基乙醯胺肟系、乙基膦酸酯系、苯二甲酸系、苯并三嗪系、苯磺酸系、噠嗪酮系、硫胺甲酸酯系、苯乙醯胺系、二苯甲酮系、苯甲醯基吡啶系、胍系、氰基亞甲基噻唑烷系、嘧啶酮腙系、二硫代胺基甲酸酯系、鄰苯二甲醯亞胺系、氯腈系、磺胺系、三嗪系、醌系、喹喔啉系、馬來醯亞胺系及中離子系藥劑所成群組的至少1種藥劑。
- 如請求項2之可濕性農藥組成物,其中前述農藥活性成分(B)為選自由二嗪農(diazinon)、乙醯甲胺磷 (acephate)、甲基吡啶磷(azamethyphos)、乙基谷硫磷(azinphos-ethyl)、甲基谷硫磷(azinphos-methyl)、硫線磷(cadusafos)、四氯乙磷(chlorethoxyphos)、毒蟲畏(clofenvinfos)、氯甲磷(chlormephos)、殺螟硫磷(fenitrothion)、異噁唑磷(isoxathion)、毒死蜱(chlorpyrifos)、甲基毒死蜱(chlorpyrifos methyl)、蠅毒磷(coumaphos)、殺螟腈(cyanophos)、dimeton-S-methyl、敵敵畏(dichlorvos)、百治磷(dicrotophos)、樂果(dimethoate)、甲基毒蟲畏(dimethylvinphos)、乙基硫脲(ethyl thiometon)、EPN、乙硫磷(ethion)、滅線磷(etoprophos)、風扇滿(fanful)、苯線磷(fenamiphos)、倍硫磷(fenthione)、噻唑膦(fosthiazate)、庚蟲磷(heptenophos)、imiciaphos、異柳磷(isofenphos)、滅蚜磷(mecarbam)、甲胺磷(methamidophos)、殺撲磷(methidathion)、速滅磷(mevinphos)、久效磷(monocrotophos)、二溴磷(naled)、氧樂果(omethoate)、乙醯甲胺磷(oxydimethone methyl)、巴拉松(parathion)、甲基巴拉松(methyl parathion)、甲拌磷(phorate)、伏殺磷(phosalone)、亞胺硫磷(phosmet)、磷胺(phosphamidone)、肟(oxime)、甲基嘧啶磷(pirimiphos methyl)、丙溴磷(profenophos)、烯蟲磷(propetamphos)、丙硫磷(prothiophos)、吡唑硫磷(pyraclophos)、噠嗪硫磷(pyridaphenthion)、喹硫磷(quinalfos)、治螟磷(sulfotep)、丁基嘧啶磷(tebupirimfos)、雙硫磷(temefos)、特丁硫磷(terbufos)、殺蟲畏(tetrachlorvinphos)、甲基乙拌(thiomethone)、三唑磷(triazophos)、敵百蟲(trichlorofon)、蚜滅多(vamidothion)、 丙硫磷(prothiophos)、馬拉硫磷(malathion)、PAP、DEP、EPN、滅多威(methomyl)、硫雙威(thiodicarb)、丙硫克百威(benflacarb)、丁硫克百威(carbosulfan)、棉鈴威(aranicalb)、氟丙菊酯(acrinathrin)、烯丙菊酯(arethrin)、聯苯菊酯(bifenthrin)、生物烯丙菊酯(bioallethrin)、生物苄呋菊酯(bioresmethrin)、乙氰菊酯(cycloprothrin)、氟氯氰菊酯(cyfluthrin)、氯氟氰菊酯(cyhalothrin)、氯氰菊酯(cypermethrin)、苯醚氰菊酯(cyphenothrin)、溴氰菊酯(deltamethrin)、右旋烯炔菊酯(empenthrin)、高氰戊菊酯(esfenvalerate)、醚菊酯(etofenprox)、甲氰菊酯(fenpropatrin)、氰戊菊酯(fenvalerate)、氟氰戊菊酯(flucythrinate)、氟氯苯菊酯(flumethrin)、氟胺氰菊酯(fluvalinate)、菊酯(halfenprox)、炔咪菊酯(imiprothrin)、cadethrin、氯菊酯(permethrin)、苯醚菊酯(phenothrin)、炔丙菊酯(prarethrin)、氯氟氰菊酯(cyhalothrin)、七氟菊酯(tefluthrin)、似蟲菊(phthalthrin)、四溴菊酯(tralomethrin)、菊酯(transfluthrin)、DDT、甲氧滴滴梯(methoxychlor)、吡蟲啉(imidacloprid)、噻蟲嗪(thiamethoxam)、噻蟲胺(clothianidin)、啶蟲脒(acetamiprid)、烯啶蟲胺(nitenpyram)、噻蟲啉(thiacloprid)、呋蟲胺(dinotefuran)、硫酸菸鹼、氟啶蟲胺腈(sulfoxaflor)、氟吡呋喃酮(flupyradifurone)、烯蟲乙酯(hydroprene)、烯蟲炔酯(kinoprene)、烯蟲酯(methoprene)、吡丙醚(pyriproxyfen)、氯丹(chlordane)、硫丹(benzoepin)、氟蟲雙醯胺(flubendiamide)、氯蟲苯甲醯胺(chlorantraniliprole)、溴氰蟲醯胺(cyantraniliprole)、 殺蟲環(thiocyclam)、殺螟丹(cartap)、殺蟲磺(bensultap)、殺蟲安(thiosultap)、環蟲醯肼(chromafenozide)、甲氧蟲醯肼(methoxyfenozide)、氯蟲醯肼(halofenozide)、蟲醯肼(tebufenozide)、氟啶脲(chlorfluazuron)、trigard、雙甲脒(amitraz)、滅蟻腙(hydramethylnon)、滅蟎醌(acequinosyl)、嘧蟎酯(fluacripyrim)、喹蟎醚(fenazaquin)、唑蟎酯(fenpyroximate)、畢汰芬(pyrimidifen)、速蟎酮(pyridaben)、吡蟎胺(tebufenpyrad)、唑蟲醯胺(tolfenpyrad)、魚藤(derris)、溴蟲腈(chlorfenapyr)、DNOC、氟蟲胺(sulfuramide)、因滅汀(emamectin)、雷皮菌素(repimectin)、密滅汀(milbemectin)、阿維菌素(abamectin)、多殺菌素(spinosad)、賜諾特(spinetoram)、雙三氟蟲脲(bistrifluron)、除蟲脲(diflubenzuron)、氟環脲(flucycloxuron)、氟鈴脲(hexaflumuron)、虱蟎脲(lufenuron)、氟醯脲(novaluron)、雙苯氟脲(nobiflumuron)、多氟脲(teflubenzuron)、殺鈴脲(triflumuron)、噻嗪酮(buprofezin)、滅蠅胺(cyromazine)、氟蟲吡喹(pyrifluquinazone)、氟蟲腈(fipronil)、乙蟲腈(ethiprole)、苯氧威(fenoxycarb)、茚蟲威(indoxacarb)、氰氟蟲胺(metaflumizone)、螺蟎酯(spirodiclofen)、螺甲蟎酯(spiromesifen)、螺蟲乙酯(spirotetramat)、吡蚜酮(pimetrozin)、氟尼胺(flonicamid)、氯化苦(chloropicrin)、硫醯氟(sulfuryl fluoride)、四蟎嗪(clofentezine)、噻蟎酮(hexythiazox)、氟蟎嗪(diflovidazin)、乙蟎唑(etoxazole)、汰芬隆(diafenthiuron)、三唑錫(azocyclotin)、氫氧化三環己基 錫、苯丁錫(fenbutatin oxide)、克蟎特(propargite)、四氯殺蟎碸(tetradifon)、氟矽菊酯(silafluofen)、磷化鋁、磷化鈣、磷化氫、磷化鋅、腈吡蟎酯(cyenopyrafen)、丁氟蟎酯(ciflumethophene)、印楝素(azadiractin)、苯甲醯氧酸鹽、聯苯肼酯(biphenazate)、溴蟎酯(bromopropyrate)、滅蟎猛(quinomethionate)、鋁氟化鈉、三氯殺蟎醇(dicofol)、三氟甲吡醚(pyridalyl)、無機銅、有機銅、無機硫、聚胺基甲酸酯(polycarbamate)、苯霜靈(benalaxyl)、呋霜靈(fralaxyl)、甲霜靈(metalaxyl)、噁霜靈(oxadixyl)、呋醯胺(ofurace)、乙嘧酚磺酸酯(buprimate)、甲菌定(dimethirimol)、乙菌定(ethirimol)、羥基異噁唑、辛噻酮(octhilinone)、噁喹酸、苯菌靈(benomyl)、多菌靈四唑(carbendazole)、麥穗寧(fuberidazole)、噻菌靈(thiabendazole)、托布津(thiophanate)、甲基硫菌靈(thiophanate-methyl)、乙黴威(dietofencarb)、苯醯菌胺(zoxamide)、噻唑菌胺(etaboxam)、賓克隆(pencycuron)、氟吡菌胺(flupicolide)、二氟林(diflumetrim)、麥鏽靈(benodanil)、氟醯胺(flutolanil)、丙氧滅鏽胺(mepronil)、異丙噻菌胺(isofetamid)、氟吡菌醯胺(fluopirum)、甲呋醯胺(fenfuram)、萎鏽靈(carboxin)、氧化萎鏽靈(oxacarboxin)、賽氟滅(thifluzamide)、苯并烯氟菌胺(benzovindiflupyr)、溴氟唑菌(bixafen)、氟唑菌醯胺(fluxapyroxad)、福拉比(flametopyr)、異皮姆(isopyrazam)、氟唑菌苯胺(penflufen)、吡噻菌胺(penthiopyrade)、環丙吡菌胺(sedaxane)、白克列(boscalid)、嘧菌酯 (azoxystrobin)、蜘蛛嘧菌酯(spiderxystrobin)、依諾肝素嘧菌酯(enoxastrobin)、fluphenoxystrobin、啶氧菌酯(picoxystrobin)、唑菌酯(pyraoxystrobin)、菌胺酯(pyraclostrobin)、pyramethostrobin、triclopyricarab、醚菌酯(kresoxim-methyl)、肟菌酯(trifloxystrobin)、醚菌胺(dimoxystrobin)、phenaminstrobin、苯氧菌胺(metominostrobin)、肟醚菌胺(orysastrobin)、噁唑菌酮(famoxadone)、氟嘧菌酯(fluoxastrobine)、咪唑菌酮(fenamidone)、吡菌苯威(pyribencarb)、氰霜唑(cyazofamid)、吲唑磺(amisulbrom)、樂殺蟎(binapacryl)、硝苯菌酯(meptyldinocap)、消蟎普(dinocup)、氟啶胺(furazinam)、嘧菌腙(ferrimzone)、有機錫、矽噻菌胺(silthiofam)、滅脫定(ametoctradin)、嘧菌環胺(cyprodinil)、嘧菌胺(mepanipyrim)、二甲嘧菌胺(pyrimethanyl)、滅瘟素S(blasticidin S)、春雷黴素(kasugamycin)、鏈黴素(streptomycin)、土黴素(oxytetracycline)、苯氧喹啉(quinoxifene)、丙氧喹啉(proquinazide)、拌種咯(fenpiclonil)、咯菌腈(fludioxonil)、乙菌利(chlozolinate)、異菌脲(iprodione)、腐黴利(procymidone)、乙烯菌核利(vinclozolin)、克瘟散(edifenphos)、異丙苯磷(iprobenfos)、定菌磷(pyrazophos)、稻瘟靈(isoprothiolane)、聯苯、地茂散(chloroneb)、二氯硝基苯(dichlorane)、五氯硝基苯(quintozene)、四氯硝基苯(tecnazene)、甲基立枯磷(tolclofos-methyl)、氯唑靈(echlomezol)、克打淨(iodocarb)、霜黴威(propamocarb)、硫菌(prothiocarb)、枯草芽孢桿菌(bacillus subtilis)、嗪氨 靈(trifolin)、啶斑肟(pyriphenox)、pyrixazole、芬路某(fanarimol)、氟苯嘧啶醇(nuarimol)、抑黴唑(imazalil)、噁咪唑(oxosconazole)、稻瘟酯(peflazoate)、咪鮮胺(prochloraz)、賽福座(triflumizole)、戊環唑(azaconazole)、雙苯三唑醇(vitertanol)、糠菌唑(broconazole)、環唑醇(cyproconazole)、醚唑(difenoconazole)、待克立(diniconazole)、氟環唑(epoxiconazole)、乙環唑(etaconazole)、腈苯唑(fenbuconazole)、氟喹唑(fluquinonazole)、氟矽唑(flusilazole)、粉唑醇(flutriafol)、己唑醇(hexaconazole)、亞胺唑(imibenconazole)、種菌唑(ipconazole)、葉菌唑(metoconazole)、腈菌唑(microbutanyl)、戊菌唑(penconazole)、丙環唑(propiconazole)、矽氟唑(simeconazole)、戊唑醇(tebuconazole)、四氟醚唑(tetraconazole)、三唑酮(triadimefon)、三唑醇(triadimenol)、滅菌唑(triticonazole)、丙硫菌唑(prothioconazole)、殺螟丹(aldimorph)、十二環嗎啉(dodemorph)、丁苯嗎啉(fenpropimorph)、十三嗎啉(tridemorph)、苯鏽(fenpropidin)、粉病靈(piperalin)、螺環菌胺(spiroxamine)、環醯菌胺(fenhexamid)、胺苯吡菌酮(fenpyrazamine)、稗草畏(pyributicarb)、萘替芬(naftifine)、特比萘芬(terbinafine)、有效黴素(validamycin)、多氧黴素(polyoxin)、烯醯嗎啉(dimethomorph)、氟嗎啉(flumorph)、丁吡嗎啉(pyrimorph)、苯噻菌胺(benthiavalicarb)、異丙菌胺(iprovalicarb)、霜霉滅(valifenalate)、雙炔醯菌(mandipropamide)、四氯苯酞(fushalide)、咯喹酮(piroquilone)、三環唑(tricyclazole)、環丙醯菌胺(carpropamide)、雙氯氰 菌胺(diclocimet)、氰菌胺(phenoxanyl)、噻二唑素S-甲基(acibenzolar S-methyl)、噻菌靈(probenazole)、噻醯菌胺(tiazinyl)、異噻菌胺(isothianyl)、昆布多醣(laminarin)、霜脲氰(cymoxanil)、三乙膦酸(phosethyl)、葉枯酞(tecloftalam)、菌嗪(triazoxide)、磺菌胺(flusulfamide)、噠菌酮(diclomezin)、磺菌威(metasulfocarb)、環氟菌胺(cyfluphenamide)、苯菌酮(metrafenone)、pyriofenone、胍(guanidine)、氟噻菌淨(flutianil)、嘧菌腙(ferimsone)、福美鐵(ferbam)、代森錳鋅(manzeb)、代森錳(maneb)、代森聯(methineum)、丙森鋅(propineb)、福美雙(thiuram)、代森鋅(dineb)、克菌丹(captan)、敵菌丹(difoltan)、滅菌丹(folpet)、TPN、抑菌(diclofluanide)、甲苯氟磺胺(trifluanide)、雙胍鹽(guazatine)、雙胍辛胺(iminoctadine)、三嗪(triazine)、二噻酮(dithianone)、滅蟎猛(quinomethionate)、氟亞胺(fluoroimide)、三氟苯嘧啶(triflumezopyrim)及dicloromezotiaz所成群組的至少1種藥劑。
- 如請求項1或2之可濕性農藥組成物,其中添加劑進一步含有選自由黏合劑及無機鹽所成群組的1種或2種以上之材料。
- 如請求項6之可濕性農藥組成物,其中黏合劑係選自由聚乙烯吡咯啶酮、聚乙烯醇、甲基纖維素及羧甲基纖維素所成群組。
- 如請求項6之可濕性農藥組成物,其中無機鹽為選自由磷酸二氫鉀、氯化鈉、氯化鉀及硫酸銨所成群組的1種或2種以上之無機鹽。
- 一種製造如請求項1、6~8中任一項之可濕性農藥組成物的方法,其係包含將農藥活性成分(A)與界面活性劑共同進行濕式粉碎之步驟而成,藉由濕式粉碎所得之懸浮液中的農藥活性成分(A)的體積中位直徑為0.1~5.0μm。
- 一種製造如請求項2~8中任一項之可濕性農藥組成物的方法,其係包含將農藥活性成分(A)及農藥活性成分(B)的混合物,與界面活性劑共同進行濕式粉碎之步驟而成,藉由濕式粉碎所得之懸浮液中的農藥活性成分(A)及前述農藥活性成分(B)的體積中位直徑為0.1~5.0μm。
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