AU2017100484B4 - Water soluble granule of MCPA salt and preparation method thereof - Google Patents
Water soluble granule of MCPA salt and preparation method thereof Download PDFInfo
- Publication number
- AU2017100484B4 AU2017100484B4 AU2017100484A AU2017100484A AU2017100484B4 AU 2017100484 B4 AU2017100484 B4 AU 2017100484B4 AU 2017100484 A AU2017100484 A AU 2017100484A AU 2017100484 A AU2017100484 A AU 2017100484A AU 2017100484 B4 AU2017100484 B4 AU 2017100484B4
- Authority
- AU
- Australia
- Prior art keywords
- mcpa
- salt
- water soluble
- soluble granule
- water
- 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.)
- Expired
Links
- 239000004549 water soluble granule Substances 0.000 title claims abstract description 63
- WHKUVVPPKQRRBV-UHFFFAOYSA-N Trasan Chemical class CC1=CC(Cl)=CC=C1OCC(O)=O WHKUVVPPKQRRBV-UHFFFAOYSA-N 0.000 title abstract description 67
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000002738 chelating agent Substances 0.000 claims abstract description 35
- 239000004094 surface-active agent Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000945 filler Substances 0.000 claims abstract description 25
- -1 alkyl glycoside Chemical class 0.000 claims description 32
- ORHJUFUQMQEFPQ-UHFFFAOYSA-M potassium;2-(4-chloro-2-methylphenoxy)acetate Chemical compound [K+].CC1=CC(Cl)=CC=C1OCC([O-])=O ORHJUFUQMQEFPQ-UHFFFAOYSA-M 0.000 claims description 29
- 239000008187 granular material Substances 0.000 claims description 21
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 15
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 14
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 14
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 14
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims description 14
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 12
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 10
- 229930006000 Sucrose Natural products 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000005720 sucrose Substances 0.000 claims description 10
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 9
- PKAUICCNAWQPAU-UHFFFAOYSA-N 2-(4-chloro-2-methylphenoxy)acetic acid;n-methylmethanamine Chemical compound CNC.CC1=CC(Cl)=CC=C1OCC(O)=O PKAUICCNAWQPAU-UHFFFAOYSA-N 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 239000004381 Choline salt Substances 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 235000019417 choline salt Nutrition 0.000 claims description 8
- 150000002191 fatty alcohols Chemical class 0.000 claims description 7
- 235000002639 sodium chloride Nutrition 0.000 claims description 7
- 229920005682 EO-PO block copolymer Polymers 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- STAPBGVGYWCRTF-UHFFFAOYSA-M sodium;2-(4-chloro-2-methylphenoxy)acetate Chemical compound [Na+].CC1=CC(Cl)=CC=C1OCC([O-])=O STAPBGVGYWCRTF-UHFFFAOYSA-M 0.000 claims description 6
- OXHMXYPUPTUWEZ-UHFFFAOYSA-N 1-[bis(2-hydroxypropyl)amino]propan-2-ol;2-(4-chloro-2-methylphenoxy)acetic acid Chemical compound CC(O)CN(CC(C)O)CC(C)O.CC1=CC(Cl)=CC=C1OCC(O)=O OXHMXYPUPTUWEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 5
- 239000000194 fatty acid Substances 0.000 claims description 5
- 229930195729 fatty acid Natural products 0.000 claims description 5
- 229930182470 glycoside Natural products 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 5
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 5
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 5
- 235000011151 potassium sulphates Nutrition 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 229920005646 polycarboxylate Polymers 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 2
- 235000013877 carbamide Nutrition 0.000 claims description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 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
- 238000001035 drying Methods 0.000 claims description 2
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical class CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 2
- 229960001484 edetic acid Drugs 0.000 claims 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 2
- 150000003248 quinolines Chemical class 0.000 claims 1
- 239000005574 MCPA Substances 0.000 abstract description 30
- 239000008233 hard water Substances 0.000 abstract description 12
- 239000002671 adjuvant Substances 0.000 abstract description 7
- 230000002085 persistent effect Effects 0.000 abstract description 6
- 239000000575 pesticide Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 description 22
- 238000004898 kneading Methods 0.000 description 16
- 238000012360 testing method Methods 0.000 description 12
- 241000196324 Embryophyta Species 0.000 description 6
- 238000009472 formulation Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 244000286177 Raphanus raphanistrum Species 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 239000003995 emulsifying agent Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 235000000245 Raphanus raphanistrum subsp raphanistrum Nutrition 0.000 description 3
- 235000011380 Raphanus sativus Nutrition 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 3
- 102000039446 nucleic acids Human genes 0.000 description 3
- 108020004707 nucleic acids Proteins 0.000 description 3
- 150000007523 nucleic acids Chemical class 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001243 protein synthesis Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 230000014616 translation Effects 0.000 description 3
- 239000004552 water soluble powder Substances 0.000 description 3
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- 241000209140 Triticum Species 0.000 description 2
- 235000021307 Triticum Nutrition 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004495 emulsifiable concentrate Substances 0.000 description 2
- 238000001668 nucleic acid synthesis Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 229940083575 sodium dodecyl sulfate Drugs 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- 235000019983 sodium metaphosphate Nutrition 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- 239000004557 technical material Substances 0.000 description 2
- QDGIAPPCJRFVEK-UHFFFAOYSA-N (1-methylpiperidin-4-yl) 2,2-bis(4-chlorophenoxy)acetate Chemical class C1CN(C)CCC1OC(=O)C(OC=1C=CC(Cl)=CC=1)OC1=CC=C(Cl)C=C1 QDGIAPPCJRFVEK-UHFFFAOYSA-N 0.000 description 1
- JKBWXPBNCSKXML-UHFFFAOYSA-N (4-chloro-2-methylphenyl) hydrogen carbonate Chemical compound CC1=CC(Cl)=CC=C1OC(O)=O JKBWXPBNCSKXML-UHFFFAOYSA-N 0.000 description 1
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 description 1
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 1
- PDIYKJRLQHHRAG-UHFFFAOYSA-N 6-methylheptyl 2-(4-chloro-2-methylphenoxy)acetate Chemical compound CC(C)CCCCCOC(=O)COC1=CC=C(Cl)C=C1C PDIYKJRLQHHRAG-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 241000722731 Carex Species 0.000 description 1
- 239000009261 D 400 Substances 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- 235000000241 Raphanus raphanistrum Nutrition 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 description 1
- 239000004227 calcium gluconate Substances 0.000 description 1
- 235000013927 calcium gluconate Nutrition 0.000 description 1
- 229960004494 calcium gluconate Drugs 0.000 description 1
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 230000032823 cell division Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- OPGYRRGJRBEUFK-UHFFFAOYSA-L disodium;diacetate Chemical compound [Na+].[Na+].CC([O-])=O.CC([O-])=O OPGYRRGJRBEUFK-UHFFFAOYSA-L 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 235000011118 potassium hydroxide Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017454 sodium diacetate Nutrition 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 210000000434 stratum corneum Anatomy 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 230000035899 viability Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/722—Ethers of polyoxyalkylene glycols having mixed oxyalkylene groups; Polyalkoxylated fatty alcohols or polyalkoxylated alkylaryl alcohols with mixed oxyalkylele groups
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/83—Mixtures of non-ionic with anionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/06—Phosphates, including polyphosphates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/122—Sulfur-containing, e.g. sulfates, sulfites or gypsum
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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Abstract
The present invention relates to the technical field of pesticides, and discloses a water soluble granule of 2-methyl-4-chlorophenoxy acetic acid (MCPA) salt and preparation method thereof. The water soluble granule of the present invention consists of the MCPA salt as well as a specific surfactant, a chelator and a filler. A water soluble granule of MCPA salt capable of achieving better storage stability, solubility and dissolving stability as well as persistent foamability in high concentration of hard water is prepared in the present invention by adjusting the adjuvant types of the water soluble granule of MCPA salt and using in combination with proper adjuvants. It is particularly suitable for countries and regions of higher water hardness.
Description
WATER SOLUBLE GRANULE OF MCPA SALT AND PREPARATION
METHOD THEREOF
Field of the invention
The present invention relates to the technical field of pesticides, and particularly to a water soluble granule of 2-methyl-4-chlorophenoxy acetic acid (MCPA) salt.
Background of the invention 2-methyl-4-chlorophenoxy acetic acid (MCPA) is a selective herbicide of 2-methyl-4-chlorophenoxy carboxylic acid category, has strong systemic conductivity, and is mainly used in post-emergence stem and leaf treatment. It passes through the stratum corneum and plasma membrane, and is ultimately transported to various parts and produces various impacts on nucleic acid and protein synthesis at different sites: inhibiting nucleic acid metabolism and protein synthesis at the top of the plant, such that the growing points stop growing, the young leaves cannot spread out, till the photosynthesis cannot normally proceed; increasing nucleic acid and protein synthesis when the reagent is transported to the bottom of the plant, which promotes abnormal cell division, root tip enlargement and loss of the ability to obsorb nutrients, causing stem twisted and deformed, sieve tube plugged, phloem destructed, transportation of organics disrupted, thereby undermining the normal viability of the plant, eventually leading to death of the plant. For years, MCPA is widely used on wheat fields, corn fields, paddy fields, city lawns and hemp crops for the controlling of annual or perennial broadleaf weeds and part of sedges; it can also be used as rice root removal agent, which can improve the efficacy of evulsing. When used in soil treatment, it also has some controlling effect on the buds of annual grasses and perennial weeds propagated by seed. It is widely used because of its advantages of low cost, rapid onset, no residue and safety to the afterculture crops, etc.
Pure product of MCPA is non-volatile colorless crystal, and its industrial product is a yellow to white solid powder. Its solubility at 25 °C in water is about 300 mg, and it is easily dissolved in organic solvents. In practical application, MCPA is typically required to be prepared as water-soluble salts or oil-soluble esters such as MCPA dimethylamine salt, MCPA isooctyl ester, MCPA sodium, MCPA thioethyl ester, MCPA ethyl ihioester, MCPA isopropylamine salt, MCPA ethyl butyrate, etc., as solubility of MCPA is extremely low in water. Currently, the main preparations of MCPA include aqueous solution, water-soluble powder and emulsifiable concentrate. Wherein, the effective content of the aqueous solution is 13% with the rest ingredients to be primarily water, and such a preparation increases transportation cost with low active ingredient but high dosage, and is unbeneficial to environment protection with a waste of resources. The water-soluble powder consists mainly of 56% of sodium salts. Although a solid formulation, there are safety risks for producers and users as it is a powdery material and thus easy to form dusts. The emulsifiable concentrate contains plenty of organic solvents and thus belongs to environmental-harmful preparation which would significantly damage the environment, wherein great safety risks for producers and users are presented by some of the solvents.
Water soluble granule (SG or WSG) rapidly disintegrates into water with high solubility to form a stable solution in the case of reasonable formula. Therefore, the utilization rate of the active ingredient is also higher. The requirements for the formulation and the preparation process of water soluble granules are higher, and the selection of adjuvants should be adapted to the main agents, otherwise the good solubility cannot be obtained by a WSG prepared with unsuitable adjuvant selection, leading to a long disintegration time and low suspension rate of the prepared waler soluble granule. A water soluble granule of MCPA salt and the preparation method thereof were disclosed in China patent CN104705301A, which is prepared from MCPA salt, a specific surfactant and a water-soluble filler to improve the suspension rate and decrease disintegration time and foamability. However, after testing research, it is found that the beneficial effects of the product in various aspects are suitable only for countries and regions of less higher water hardness, while employment of the above described water soluble granules in countries with commonly high concentration of hard water such as Australia still exhibits phenomena of unsatisfactory product qualities, such as poor stability for storage, weak solubility and dissolving stability, and persistent lower foamability, such that the efficacy of MCPA cannot be fully achieved.
Summary of the invention
In view of this, the object of the present invention is to provide a water soluble granule of MCPA salt and the preparation method thereof, such that the water soluble granule of MCPA salt has better storage stability, solubility and dissolving stability as well as persistent foamability in high concentration of hard water.
To achieve the object above, the present invention provides the following technical solution: A water soluble granule of MCPA salt, characterized in that it consists of the MCPA salt, a surfactant, a chelator and a filler.
The surfactant is one selected from the group consisting of alkylphenol polyoxyethylene polyoxypropylene ether, lauryl alcohol polyoxyethylene ether, fatly amine polyoxyethylene ether, allcylnaphthalenesulfonate, fatty alcohol polyoxyethylene ether alkylnaphthalenesulfonic acid formaldehyde condensate, dodecylsulfate; or both ethylene oxide-propylene oxide block copolymer and alkyl glycoside; or both polycarboxylate and polyethylene glycol; or both melhyloxirane and polyoxyethylene fatty acid ester.
The chelator is one or more selected from the group consisting of ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, tetrasodium ethylenediaminetetraacetate and sodium tripolyphosphate.
Aiming at the defect of the existing water soluble granule of MCPA salt in not suitable for high concentration of hard water, the adjuvant types are adjusted, the chelator is added and the specific combination of surfactant and chelator is defined in the present invention. On this basis, the problem of poor product performance of water soluble granule of MCPA salt in high concentration of hard water is solved.
Preferably, the surfactant and chelator are used in one of the following combinations: (1) alkylnaphthalenesulfonate and disodium ethylenediaminetetraacetate; (2) ethylene oxide-propylene oxide block copolymer, alkyl glycoside and ethylenediamine tetraacetic acid; (3) melhyloxirane, polyoxyethylene fatty acid ester and tetrasodium ethylenediaminetetraacetate; (4) alkylphenol polyoxyethylene polyoxypropylene ether and ethylenediamine tetraacetic acid; ' (5) lauryl alcohol polyoxyethylene ether and tetrasodium ethylenediaminetetraacetate; (6) fatty alcohol polyoxyethylene ether and sodium tripolyphosphate; (7) fatty alcohol polyoxyethylene ether alkylnaphthalenesulfonic acid formaldehyde condensate and tetrasodium ethylenediaminetetraacetate; (8) sodium dodecylsulfate and sodium tripolyphosphate; (9) polycarboxylate, polyethylene glycols and sodium tripolyphosphate.
Preferably, by weight percentage, the water soluble granule comprises 10%-90% of the MCPA salt, l%-20% of the surfactant, 1%-10% of the chelator and the balance of the filler; more preferably, 30%-90% of the MCPA salt, 1%-10% of the surfactant, l%-6% of the chelator and the balance of the filler; further preferably, 50%-90% of the MCPA salt, l%-5% of the surfactant, 1.5% of the chelator and the balance of the filler; most preferably, 90% of the MCPA salt, 2% of the surfactant, 1.5% of the chelator and the balance of the filler.
In some particular embodiments of the present invention, the weight percentage of each component can be chosen as follows: (1) 90% of the MCPA salt, 2% of the surfactant, 1.5% of the chelator and the balance of the filler; (2) 80% of the MCPA salt, 2% of the surfactant, 1.5% of the chelator and the balance of the filler; (3) 50% of the MCPA salt, 10% of the surfactant, 6% of the chelator and the balance of the filler; (4) 30% of the MCPA salt, 2% of the surfactant, 1.5% of the chelator and the balance of the filler; (5) 10% of the MCPA salt, 2% of the surfactant, 1.5% of the chelator and the balance of the filler; (6) 50% of the MCPA salt, 2% of the surfactant, 1.5% of the chelator and the balance of the filler; (7) 90% of the MCPA salt, 3.5% of the surfactant, 0.5% of the chelator and the balance of the filler; (8) 70% of the MCPA salt, 9.5% of the surfactant, 3.5% of the chelator and the balance of the filler; (9) 40% of the MCPA salt, 12% of the surfactant, 4% of the chelator and the balance of the filler; (10) 10% of the MCPA salt, 20% of the surfactant, 6% of the chelator and the balance of the filler; (11) 60% of the MCPA salt, 12% of the surfactant, 3% of the chelator and the balance of the filler; (12) 40% of the MCPA salt, 15% of the surfactant, 5% of the chelator and the balance of a filler; (13) 20% of the MCPA salt, 20% of the surfactant, 6% of the chelator and the balance of the filler;
Preferably, the alkylnaphthalenesulfonate is Morwel EFW which can be purchased from AkzoNobel; the ethylene oxide-propylene oxide block copolymer is PE6200 which can be purchased from BASF; the polyoxyethylene fatty acid ester is selected from A (OEO) series of emulsifier, and the A (OEO) series of emulsifier is preferably A-105 emulsifier, all of which are commercially available; the polycarboxylate preferably is TERSPERSE-2700, which can be purchased from Hunstman.
Preferably, the MCPA salt of the present invention is MCPA potassium salt, MCPA sodium salt, MCPA dimethylamine salt, MCPA amine salt, MCPA isopropylammonium salt, MCPA choline salt or MCPA triisopropanolamine salt. Each of the MCPA salt can be purchased or self-made, and the process for self-making can refer to the following process:
Mixing MCPA with alkaline substance for 10-15 min, adding 12-16% of water, and reacting for 50-70 min at a condition of 45-55 °C to obtain the MCPA salt. Wherein, the alkaline substance can be selected from the group consisting of sodium hydroxide, potassium carbonate, potassium hydroxide, potassium bicarbonate, ammonium bicarbonate, ammonia water, isopropyl amine, sodium carbonate, sodium bicarbonate, dimethylamine, triisopropanolamine and choline based on the required type of MCPA salt. The molar ratio of the MCPA salt acid to the alkaline substance is 1:(1-1.1), preferably 1:1.04.
Preferably, the filler is one or more selected from the group consisting of ammonium sulfate, diammonium hydrogen phosphate, sodium sulfate, sodium chloride, urea, potassium nitrate, ammonium nitrate, ammonium chloride, dipolassium hydrogen phosphate, sucrose, potassium sulfate and sodium tripolyphosphate.
Meanwhile, the present invention also provides a method for preparing the water soluble granule of MCPA salt: homogeneously mixing the MCPA salt with the surfactant, the chelator and the filler, and then adding water and mixing, extruding, granulating, and dring to obtain the water soluble granule.
Preferably, the drying is carried out under a condition of 50-75 °C.
The water soluble granule of MCPA salt of the present invention is compared with the products of Example 13-Example 47 in the prior patent CN104705301A in storage stability, solubility and dissolving stability as well as persistent foamability in high concentration of hard water. The results show that the water soluble granule of MCPA salt is significantly superior to the products of the prior patent.
Meanwhile, the present invention selects a chelator different from those employed in the present invention, and various types of surfactant for contrast test. The results show that, the excellent product performance can be exhibited in circumstance of high concentration of hard water only on the premise of the combination of the surfactant and chelator selected by the present invention.
It can be known from the above technical solution that, a water soluble granule of MCPA salt capable of achieving better storage stability, solubility and dissolving stability as well as persistent foamability in high concentration of hard water is prepared in the present invention by adjusting the adjuvant types of the water soluble granule of MCPA salt and using in combination with proper adjuvants. It is particularly suitable for countries and regions of higher water hardness.
Detailed description of the invention
The example of the present invention discloses a water soluble granule of MCPA salt and the preparation method thereof. Those skilled in the art can use the content herein for reference to achieve by appropriately improving the process parameters. It should be particular noted that all the similar substitutions and modifications will be apparent to those skilled in the art, and they are all considered to fall within the scope of the present invention. The water soluble granule of MCPA salt and the preparation method thereof have been described through preferred examples, and for an ordinary skilled in the art, modifications or proper alternations and combinations can be made to the product and method described in the present invention without departing from the content, spirit and scope of the present invention, to achieve and apply the technology of the present invention.
Each of the mass percentage of the water soluble granule is the percentage of the amount of each component in the total feeding. While in the purchased or self-made MCPA salt, the purity is generally not 100%, and the amount of MFC A salt in tire total feeding refers to an impurity-containing MPCA salt, while the mass percentage of MCPA salt is the percentage of pure MCPA salt amount in the total feeding.
The water soluble granule of MCPA salt and the preparation method thereof provided by the present invention are further illustrated below.
Example 1: Preparation of MCPA salt 421.1 g of MCPA technical material (purity of 95%) together with an alkaline substance (purity of higher than 99%) were put into a 1 L kneader equipped with a heating device and mixed for 10 min-15 min under a condition of normal temperature and pressure. 12-16% of water was added and heated up to 45°C-55°C to react for 50 min-70 min to obtain the MCPA salt. Wherein the reaction conditions for each MCPA salt is shown in Table 1.
Table 1. Preparation conditions for MCPA salt
Example 2: Water soluble granule of 90% MCPA potassium salt 93.75 g of MCPA potassium salt (purity of 96%), 2 g of Morwet EFW (AkzoNobel, alkylnaphthalenesulfonate), 1.5 g of disodium EDTA and 2.75 g of sucrose were weighed and mixed, then 3% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA potassium salt in 90% mass fraction, yield 99.7%.
Example 3: Water soluble granule of 80% MCPA potassium salt 83.3 g of MCPA potassium salt (purity of 96%), 2 g of Morwet EFW (AkzoNobel, alkylnaphthalenesulfonate), 1.5 g of disodium EDTA and 13.2 g of sucrose were weighed and mixed, then 3% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA potassium salt in 80% mass fraction, yield 99.5%.
Example 4: Water soluble granule of 50% MCPA potassium salt 52.1 g of MCPA potassium salt (purity of 96%), 2 g of Morwet EFW (AkzoNobel, alkylnaphthalenesulfonate), 1.5 g of disodium EDTA and 44.4 g of sucrose were weighed and mixed, then 2.5% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA potassium salt in 50% mass fraction, yield 99.3%.
Example 5: Water soluble granule of 30% MCPA potassium sail 31.3 g of MCPA potassium salt (purity of 96%), 2 g of Morwet EFW (AkzoNobel, alkylnaphthalenesulfonate), 1,5 g of disodium EDTA and 65.2 g of sucrose were weighed and mixed, then 1.5% of water was added and the mixture was pul into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA potassium salt in 30% mass fraction, yield 99.1%.
Example 6: Water soluble granule of 10% MCPA potassium salt 110.4 g of MCPA potassium salt (purity of 96%), 2 g of Morwet EFW (AkzoNobel, alkylnaphthalenesulfonate), 1.5 g of disodium EDTA and 86.1 g of sucrose were weighed and mixed, then 1.5% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA potassium salt in 10% mass fraction, yield 99.0%.
Example 7: Water soluble granule of 90% MCPA dimethylamine salt 93.75 g of MCPA dimethylamine salt (purity of 96%), 2 g of Morwet EFW (AkzoNobel, alkylnaphthalenesulfonate), 2.75 g of disodium EDTA and 1.8 g of sucrose were weighed and mixed, then 4% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA dimethylamine salt in 90% mass fraction, yield 99.0%.
Example 8: Water soluble granule of 80% MCPA isopropylamine salt 83.3 g of MCPA isopropylamine salt (purity of 96%), 2 g of Morwet EFW (AkzoNobel, alkylnaphthalenesulfonate), 1.5 g of disodium EDTA and 13.2 g of sucrose were weighed and mixed, then 3.5% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA isopropylamine salt in 80% mass fraction, yield 98.7%.
Example 9: Water soluble granule of 50% MCPA choline salt 52.1 g of MCPA choline salt (purity of 96%), 2 g of Morwet EFW (AkzoNobel, alkylnaphthalenesulfonate), 1.5 g of disodium EDTA and 44.4 g of sucrose were weighed and mixed, then 4.5% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA choline salt in 50% mass fraction, yield 98.5%.
Example 10: Water soluble granule of 90% MCPA potassium salt 993.75 g of MCPA potassium salt (purity of 96%), 1.5 g of PE6200 (BASF, ethylene oxide-propylene oxide block copolymer), 2% of APG (alkyl glycoside), 0.5 g of EDTA and 2.25 g of ammonium sulfate were weighed and mixed, then 3.2% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA potassium salt in 90% mass fraction, yield 99.2%.
Example 11: Water soluble granule of 70% MCPA potassium salt 72.9 g of MCPA potassium salt (purity of 96%), 6.5 g of T-7200 (Hunstman, polycarboxylafe), 3 g of polyethylene glycol, 3.5g of sodium tripolyphosphate, 5 g of sodium chloride and 9.1 g of potassium nitrate were weighed and mixed, then 4,2% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA potassium salt in 70% mass fraction, yield 98.8%.
Example 12: Water soluble granule of 40% MCPA potassium salt 41.7 g of MCPA potassium salt (purity of 96%), 10 g of methyloxirane, 2 g of A-105 (emulsifier A(OEO) series), 4.0 g of tetrasodium EDTA, 20 g of ammonium nitrate and 22.3g dipotassium hydrogen phosphate were weighed and mixed, then 8.2% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA potassium salt in 40% mass fraction, yield 98.5%.
Example 13: Water soluble granule of 10% MCPA potassium salt 10.4g of MCPA potassium salt (purity of 96%), 20 g of allcylphenol polyoxyethylene polyoxypropylene ether, 6.0 g of EDTA, 40 g of ammonium chloride, and 23.6 g of diammonium hydrogen phosphate were weighed and mixed, then 10.0% of water was added and the mixture was put into a I L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA potassium salt in 10% mass fraction, yield 98.1%.
Example 14: Water soluble granule of 60% MCPA sodium salt 62.5g of MCPA sodium salt (purity of 96%), 12 g of lauryl alcohol polyoxyethylene ether, 3.0 g of tetrasodium EDTA, 20g of sodium chloride and 2.5 g of urea were weighed and mixed, then 5.0% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA sodium salt in 60% mass fraction, yield 98.3%.
Example 15: Water soluble granule of 50% MCPA ammonium salt 52.1 g of MCPA ammonium salt {purity of 96%), 10 g of fatty alcohol polyoxyethylene ether, 6.0 g of sodium tripolyphosphate and 31.9 g of sodium sulfate were weighed and mixed, then 6.0% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA ammonium salt in 50% mass fraction, yield 98.0%.
Example 16: Water soluble granule of 40% MCPA triisopropanolamine salt 41.7g of MCPA triisopropanolamine salt (purity of 96%), 15 g of fatty alcohol polyoxyethylene ether alkylnaphthalenesulfonic acid formaldehyde condensate, 5.0 g of tetrasodium EDTA, 30 g of potassium sulfate and 8.3 g of potassium sulfate were weighed and mixed, then 7.0% of water was added and the mixture was pul into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA triisopropanolamine salt in 40% mass fraction, yield 98.1%.
Example 17: Water soluble granule of 20% MCPA choline salt 20.8 g of MCPA choline salt (purity of 96%), 20 g of sodium dodecylsulfate, 6.0 g of sodium tripolyphosphate, 40 g of potassium sulfate and 13.2 g of ammonium chloride were weighed and mixed, then 9.0% of water was added and the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having MCPA choline salt in 20% mass fraction, yield 98.0%.
Example 18: Contrast test
Controls: 1. The products of Example 13-Example 47 in CN104705301A (hereinafter abbreviated as CN13-CN47); 2. Substitution of the chelators to the ones other than those used in the present invention based on the formulations of Example 2, Example 10, Example 11 and Example 15, with the same amount, respectively: Example 2: citric acid; Example 10: tartaric acid; Example 11: calcium gluconate; Example 15: sodium metaphosphate; (hereinafter abbreviated as controls 1-4); 3. Substitution of the alkylnaphthalenesulfonates to the ones other than Morwet EFW based on the formulation of Example 2, with the same amount, respectively: Tamol NN 8906 (BASF), Morwet D-400 (AkzoNobel), TP04 (CRODA); (hereinafter abbreviated as controls 5-7); 4. Addition of the chelators other than those used in the present invention based on the formulations of CN13-CN17, with the amount of 1.5%, respectively: CN13: tartaric acid; CN14: sodium gluconate; CN13: sodium diacetate; CN16: sorbitol; CN17: sodium metaphosphate; (hereinafter abbreviated as controls 8-12);
The performance index test was conducted on all of the products in the present invention and the above 4 types of controls in the same high concentration of hard water (3 times of D water, hardness of 1026 mg/L, pH=6.0-7.0, Ca3+:Mg3+=4:l). For the test, reference can be made to the methods provided in “Physical-Chemical method of Pesticide Technical Material and Formulalion-CIPAC Handbook”; and for the quality standard, reference can be made to “FAO Handbook of pesticide standard formulation and application” and “Standard preparation specifications for water soluble powder pesticide product”, as specifically shown in Table 2.
Table 2. Standard for test
The test results are shown in Table 3.
Table 3. Test results
It is clear from the results in Table 3 that the water soluble granules of MCPA salt according to the present invention meet all of the requirements of the three product performances, i.e. storage stability, solubility and dissolving stability as well as persistent foamability, and perform much better than that required by the standards under the circumstance of high concentration of hard water; wehreas, the prior patent products and the control products essentially do not meet the requirement of the standards, and also exhibit significant difference as compared to the performance of the present invention.
Meanwhile, the results of controls 1-4 illustrated that not all of the chelators could obtain the ideal product performance through combination with the other components of the present invention; the results of controls 5-7 illustrated that the better performance could be achieved only by the combinations of surfactants and chelators suitable to the present invention; the results of controls 8-12 illustrated that it is incapable of improving the product performance based on prior patent products even if some chelators beyond the defined range in the present invention are added.
Example 19: Efficacy test
The efficacy test of the example product of the present invention was earned out in New South Wales state, Australia (high concentration of hard water quality), with the crop to be wheat and the control target to be wild radish (Raphanus raphanistrum). The controlling was conducted since the wild radish was grown to 2 leaf stage, with a temperature of 11° C and a moisture of 79% on the administration day. The test field was acid lateritic soil with a pH of 5.4, and the dosage was 2175 a.i/ha. The results are shown in Table 4:
Table 4. Efficacy comparison (35 d after administration)
It can be known from the test of efficacy in Table 4 that the controlling efficacy of the water soluble granule of MCPA salt of the present invention on wild radish is obviously superior to that of the product of control patent under the circumstance of high concentration of hard water.
The above described illustrations are used only to understand the method and core concept of the present invention. It should be noted that, for an ordinary skilled in the art, some improvements and modifications can be made to the present invention without departing from the principles of the present invention. These improvements and modifications also fall within the protection scope of the present invention.
Claims (4)
1. A water soluble granule of 2-mcthyl-4-chlorophenoxy acetic acid (MCPA) salt, consisting of, by weight percentage, 50%-90% of the MCPA salt, l%-5% of a surfactant, 1.5% of a chelator and the balance of a filler; wherein, the surfactant is one selected from the group consisting of alkylphenol polyoxyethylene polyoxypropylene ether, Iauryl alcohol polyoxyethylene ether, fatty amine polyoxyethylene ether, alkylnaphthalenesulfonate, fatty alcohol polyoxyethylene ether alkylnaphthalenesulfonic acid formaldehyde condensate, dodecylsulfate; or both ethylene oxide-propylene oxide block copolymer and alkyl glycoside; or both polycarboxyl ate and polyethylene glycol; or both methyloxirane and polyoxyethylene fatty acid ester; the chelator is one or more selected from the group consisting of ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate and tetrasodium ethylenediaminetetraacetate;
2, The water soluble granule of MCPA salt according to claim 1, wherein the surfactant and chelator are used according to one of the following combinations: (1) alkylnaphthalenesulfonate and disodium ethylenediaminetetraacetate; (2) ethylene oxide-propylene oxide block copolymer, alkyl glycoside and ethyl enediamine tetraacetic acid; (3) methyloxirane, polyoxyethylene fatty acid ester and tetrasodium ethylenedi aminetetraacetate; (4) alkylphenol polyoxyethylene polyoxypropylene ether and ethylenediamine tetraacetic acid; (5) Iauryl alcohol polyoxyethylene ether and tetrasodium ethylenediaminetetraacetate; (6) fatty alcohol polyoxyethylene ether alkylnaphthalenesulfonic acid formaldehyde condensate and tetrasodium ethylenediaminetetraacetate.
3. The water soluble granule of MCPA salt according to claim 1, wherin the MCPA acid is MCPA potassium salt, MCPA sodium salt, MCPA dimethylamine salt, MCPA amine salt, MCPA isopropylammonium salt, MCPA choline salt or MCPA triisopropanolamine salt; the filler is one or more selected from the group consisting of ammonium sulfate, diammonium hydrogen phosphate, sodium sulfate, sodium chloride, urea, potassium nitrate, ammonium nitrate, ammonium chloride, dipotassium hydrogen phosphate, sucrose, potassium sulfate and sodium tripolyphosphate.
4. A method for preparing the water soluble granule of MCPA salt according to claim 1, comprising homogeneously mixing the MCPA salt with the surfactant, the chelator and the filler, and then adding water and mixing, extruding to granulate and drying, to obtain the water soluble granule of MCPA salt.
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AU2016101531A Ceased AU2016101531A4 (en) | 2016-08-03 | 2016-08-30 | Water soluble granule of MCPA salt and preparation method thereof |
AU2017100484A Expired AU2017100484B4 (en) | 2016-08-03 | 2017-05-04 | Water soluble granule of MCPA salt and preparation method thereof |
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AU (2) | AU2016101531A4 (en) |
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CN109096093A (en) * | 2018-09-14 | 2018-12-28 | 鹤壁市鹤农生物科技有限公司 | A kind of preparation method of 2-methyl-4-chlorophenoxyacetic acid sodium |
CN111440672A (en) * | 2020-03-06 | 2020-07-24 | 山东海天生物化工有限公司 | Oil stain cleaning agent and preparation method thereof |
CN114190378B (en) * | 2021-12-30 | 2023-08-18 | 四川国光农化股份有限公司 | Pesticide solid preparation for reducing decomposition rate of diethyl aminoethyl hexanoate |
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CN104705301A (en) * | 2015-04-07 | 2015-06-17 | 山东潍坊润丰化工股份有限公司 | 2-methyl-4-chlorophenoxyacetic acid salt water-soluble granular preparation and preparation method thereof |
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CN103843766A (en) * | 2012-11-30 | 2014-06-11 | 浙江新安化工集团股份有限公司 | 2-methyl-4-chloro-phenoxyacetic acid salt soluble granules (tablets) and preparation method thereof |
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CN104705301A (en) * | 2015-04-07 | 2015-06-17 | 山东潍坊润丰化工股份有限公司 | 2-methyl-4-chlorophenoxyacetic acid salt water-soluble granular preparation and preparation method thereof |
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CN107686777A (en) | 2018-02-13 |
AU2016101531A4 (en) | 2016-09-29 |
CN107686777B (en) | 2020-09-25 |
AU2017100484A4 (en) | 2017-06-01 |
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