CN114072226A - 一种获得高稳定性天然除虫菊酯微生物胶囊的方法和过程 - Google Patents
一种获得高稳定性天然除虫菊酯微生物胶囊的方法和过程 Download PDFInfo
- Publication number
- CN114072226A CN114072226A CN202080046321.9A CN202080046321A CN114072226A CN 114072226 A CN114072226 A CN 114072226A CN 202080046321 A CN202080046321 A CN 202080046321A CN 114072226 A CN114072226 A CN 114072226A
- Authority
- CN
- China
- Prior art keywords
- pyrethrin
- stage
- obtaining
- microbial capsules
- added
- 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.)
- Pending
Links
- HYJYGLGUBUDSLJ-UHFFFAOYSA-N pyrethrin Natural products CCC(=O)OC1CC(=C)C2CC3OC3(C)C2C2OC(=O)C(=C)C12 HYJYGLGUBUDSLJ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 39
- VQXSOUPNOZTNAI-UHFFFAOYSA-N Pyrethrin I Natural products CC(=CC1CC1C(=O)OC2CC(=O)C(=C2C)CC=C/C=C)C VQXSOUPNOZTNAI-UHFFFAOYSA-N 0.000 title claims abstract description 33
- VJFUPGQZSXIULQ-XIGJTORUSA-N pyrethrin II Chemical compound CC1(C)[C@H](/C=C(\C)C(=O)OC)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1 VJFUPGQZSXIULQ-XIGJTORUSA-N 0.000 title claims abstract description 33
- 239000002775 capsule Substances 0.000 title claims abstract description 31
- 230000000813 microbial effect Effects 0.000 title claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 239000002728 pyrethroid Substances 0.000 claims abstract description 15
- VXSIXFKKSNGRRO-MXOVTSAMSA-N [(1s)-2-methyl-4-oxo-3-[(2z)-penta-2,4-dienyl]cyclopent-2-en-1-yl] (1r,3r)-2,2-dimethyl-3-(2-methylprop-1-enyl)cyclopropane-1-carboxylate;[(1s)-2-methyl-4-oxo-3-[(2z)-penta-2,4-dienyl]cyclopent-2-en-1-yl] (1r,3r)-3-[(e)-3-methoxy-2-methyl-3-oxoprop-1-enyl Chemical class CC1(C)[C@H](C=C(C)C)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1.CC1(C)[C@H](/C=C(\C)C(=O)OC)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1 VXSIXFKKSNGRRO-MXOVTSAMSA-N 0.000 claims abstract description 11
- 229940070846 pyrethrins Drugs 0.000 claims abstract description 11
- 239000013543 active substance Substances 0.000 claims abstract description 5
- 239000003995 emulsifying agent Substances 0.000 claims description 20
- 125000004432 carbon atom Chemical group C* 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 10
- 239000008158 vegetable oil Substances 0.000 claims description 10
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 9
- 239000000194 fatty acid Substances 0.000 claims description 9
- 229930195729 fatty acid Natural products 0.000 claims description 9
- 150000004665 fatty acids Chemical class 0.000 claims description 9
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 9
- 239000000575 pesticide Substances 0.000 claims description 8
- 238000009472 formulation Methods 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 125000002091 cationic group Chemical group 0.000 claims description 6
- 241000607479 Yersinia pestis Species 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000012875 nonionic emulsifier Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 235000019198 oils Nutrition 0.000 claims description 4
- 235000010469 Glycine max Nutrition 0.000 claims description 3
- 244000068988 Glycine max Species 0.000 claims description 3
- 244000020551 Helianthus annuus Species 0.000 claims description 3
- 235000003222 Helianthus annuus Nutrition 0.000 claims description 3
- 240000008042 Zea mays Species 0.000 claims description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 230000002209 hydrophobic effect Effects 0.000 claims description 3
- 229940119170 jojoba wax Drugs 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 235000000832 Ayote Nutrition 0.000 claims description 2
- 240000004244 Cucurbita moschata Species 0.000 claims description 2
- 235000009854 Cucurbita moschata Nutrition 0.000 claims description 2
- 235000009804 Cucurbita pepo subsp pepo Nutrition 0.000 claims description 2
- 241001465754 Metazoa Species 0.000 claims description 2
- 244000025272 Persea americana Species 0.000 claims description 2
- 235000008673 Persea americana Nutrition 0.000 claims description 2
- 235000003434 Sesamum indicum Nutrition 0.000 claims description 2
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims description 2
- 239000002535 acidifier Substances 0.000 claims description 2
- 125000003342 alkenyl group Chemical group 0.000 claims description 2
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 239000003963 antioxidant agent Substances 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 claims description 2
- 238000004945 emulsification Methods 0.000 claims description 2
- 229940087559 grape seed Drugs 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 2
- 235000009973 maize Nutrition 0.000 claims description 2
- 235000015136 pumpkin Nutrition 0.000 claims description 2
- 239000012438 synthetic essential oil Substances 0.000 claims description 2
- 235000013311 vegetables Nutrition 0.000 claims description 2
- 239000010775 animal oil Substances 0.000 claims 2
- 240000009226 Corylus americana Species 0.000 claims 1
- 235000001543 Corylus americana Nutrition 0.000 claims 1
- 235000007466 Corylus avellana Nutrition 0.000 claims 1
- 244000000231 Sesamum indicum Species 0.000 claims 1
- 150000001450 anions Chemical group 0.000 claims 1
- 235000021323 fish oil Nutrition 0.000 claims 1
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims 1
- 230000000361 pesticidal effect Effects 0.000 claims 1
- 239000002917 insecticide Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000000749 insecticidal effect Effects 0.000 abstract description 4
- 235000007516 Chrysanthemum Nutrition 0.000 abstract description 2
- 230000001804 emulsifying effect Effects 0.000 abstract description 2
- 238000005538 encapsulation Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 241000723353 Chrysanthemum Species 0.000 abstract 1
- 230000000853 biopesticidal effect Effects 0.000 abstract 1
- 239000003094 microcapsule Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 238000011161 development Methods 0.000 description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- -1 alkylaryl ether sulfates Chemical class 0.000 description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 239000005642 Oleic acid Substances 0.000 description 3
- 240000004460 Tanacetum coccineum Species 0.000 description 3
- ROVGZAWFACYCSP-MQBLHHJJSA-N [2-methyl-4-oxo-3-[(2z)-penta-2,4-dienyl]cyclopent-2-en-1-yl] (1r,3r)-2,2-dimethyl-3-(2-methylprop-1-enyl)cyclopropane-1-carboxylate Chemical compound CC1(C)[C@H](C=C(C)C)[C@H]1C(=O)OC1C(C)=C(C\C=C/C=C)C(=O)C1 ROVGZAWFACYCSP-MQBLHHJJSA-N 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
- 150000002148 esters Chemical class 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 229940015367 pyrethrum Drugs 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 235000010384 tocopherol Nutrition 0.000 description 3
- 239000011732 tocopherol Substances 0.000 description 3
- 229930003799 tocopherol Natural products 0.000 description 3
- XMGQYMWWDOXHJM-JTQLQIEISA-N (+)-α-limonene Chemical compound CC(=C)[C@@H]1CCC(C)=CC1 XMGQYMWWDOXHJM-JTQLQIEISA-N 0.000 description 2
- YWWVWXASSLXJHU-AATRIKPKSA-N (9E)-tetradecenoic acid Chemical compound CCCC\C=C\CCCCCCCC(O)=O YWWVWXASSLXJHU-AATRIKPKSA-N 0.000 description 2
- NRVMCZSNPIHCNL-QSNNAOSGSA-N C\C=C1/C(O[C@@H]2O[C@H](CO)[C@@H](O)[C@H](O)[C@H]2O)OC=C2C1CC(=O)OCC1C(C)C(CC1C(C)CO)OC2=O Chemical compound C\C=C1/C(O[C@@H]2O[C@H](CO)[C@@H](O)[C@H](O)[C@H]2O)OC=C2C1CC(=O)OCC1C(C)C(CC1C(C)CO)OC2=O NRVMCZSNPIHCNL-QSNNAOSGSA-N 0.000 description 2
- 241000238631 Hexapoda Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 description 2
- VMORCWYWLVLMDG-YZGWKJHDSA-N Pyrethrin-II Natural products CC(=O)OC(=C[C@@H]1[C@H](C(=O)O[C@H]2CC(=O)C(=C2C)CC=CC=C)C1(C)C)C VMORCWYWLVLMDG-YZGWKJHDSA-N 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 150000008055 alkyl aryl sulfonates Chemical class 0.000 description 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 2
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 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 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- 239000000539 dimer Substances 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 239000004495 emulsifiable concentrate Substances 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- NRVMCZSNPIHCNL-UHFFFAOYSA-N jasminin Natural products O1C=C(C(OC2C(C)C(C(C2)C(C)CO)COC(=O)C2)=O)C2C(=CC)C1OC1OC(CO)C(O)C(O)C1O NRVMCZSNPIHCNL-UHFFFAOYSA-N 0.000 description 2
- KSMITTDZTTZFML-ZCFIWIBFSA-N jasminine Natural products O=C(OC)c1c2c([C@@H](C)NC(=O)C2)cnc1 KSMITTDZTTZFML-ZCFIWIBFSA-N 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 2
- 229960004488 linolenic acid Drugs 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- SECPZKHBENQXJG-FPLPWBNLSA-N palmitoleic acid Chemical compound CCCCCC\C=C/CCCCCCCC(O)=O SECPZKHBENQXJG-FPLPWBNLSA-N 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- ROVGZAWFACYCSP-VUMXUWRFSA-N pyrethrin I Chemical compound CC1(C)[C@H](C=C(C)C)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1 ROVGZAWFACYCSP-VUMXUWRFSA-N 0.000 description 2
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 2
- NPCOQXAVBJJZBQ-UHFFFAOYSA-N reduced coenzyme Q9 Natural products COC1=C(O)C(C)=C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)C(O)=C1OC NPCOQXAVBJJZBQ-UHFFFAOYSA-N 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- 229960001295 tocopherol Drugs 0.000 description 2
- 239000013638 trimer Substances 0.000 description 2
- VLPFTAMPNXLGLX-UHFFFAOYSA-N trioctanoin Chemical compound CCCCCCCC(=O)OCC(OC(=O)CCCCCCC)COC(=O)CCCCCCC VLPFTAMPNXLGLX-UHFFFAOYSA-N 0.000 description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 2
- BITHHVVYSMSWAG-KTKRTIGZSA-N (11Z)-icos-11-enoic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCC(O)=O BITHHVVYSMSWAG-KTKRTIGZSA-N 0.000 description 1
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- ATNNLHXCRAAGJS-QZQOTICOSA-N (e)-docos-2-enoic acid Chemical compound CCCCCCCCCCCCCCCCCCC\C=C\C(O)=O ATNNLHXCRAAGJS-QZQOTICOSA-N 0.000 description 1
- FRPZMMHWLSIFAZ-UHFFFAOYSA-N 10-undecenoic acid Chemical compound OC(=O)CCCCCCCCC=C FRPZMMHWLSIFAZ-UHFFFAOYSA-N 0.000 description 1
- YWWVWXASSLXJHU-UHFFFAOYSA-N 9E-tetradecenoic acid Natural products CCCCC=CCCCCCCCC(O)=O YWWVWXASSLXJHU-UHFFFAOYSA-N 0.000 description 1
- 240000006054 Agastache cana Species 0.000 description 1
- 241001124076 Aphididae Species 0.000 description 1
- 241000238421 Arthropoda Species 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 description 1
- 235000005747 Carum carvi Nutrition 0.000 description 1
- 240000000467 Carum carvi Species 0.000 description 1
- 240000003538 Chamaemelum nobile Species 0.000 description 1
- 235000007866 Chamaemelum nobile Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- 244000223760 Cinnamomum zeylanicum Species 0.000 description 1
- 244000183685 Citrus aurantium Species 0.000 description 1
- 235000007716 Citrus aurantium Nutrition 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- ACTIUHUUMQJHFO-UHFFFAOYSA-N Coenzym Q10 Natural products COC1=C(OC)C(=O)C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UHFFFAOYSA-N 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
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 241000208152 Geranium Species 0.000 description 1
- 235000019487 Hazelnut oil Nutrition 0.000 description 1
- 241000257303 Hymenoptera Species 0.000 description 1
- 235000010650 Hyssopus officinalis Nutrition 0.000 description 1
- 241000721662 Juniperus Species 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 244000165082 Lavanda vera Species 0.000 description 1
- 235000010663 Lavandula angustifolia Nutrition 0.000 description 1
- 235000004431 Linum usitatissimum Nutrition 0.000 description 1
- 240000006240 Linum usitatissimum Species 0.000 description 1
- 235000012854 Litsea cubeba Nutrition 0.000 description 1
- 240000002262 Litsea cubeba Species 0.000 description 1
- 235000007232 Matricaria chamomilla Nutrition 0.000 description 1
- 235000005135 Micromeria juliana Nutrition 0.000 description 1
- 244000179970 Monarda didyma Species 0.000 description 1
- 235000010672 Monarda didyma Nutrition 0.000 description 1
- 235000009421 Myristica fragrans Nutrition 0.000 description 1
- 244000270834 Myristica fragrans Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 244000178231 Rosmarinus officinalis Species 0.000 description 1
- 240000000513 Santalum album Species 0.000 description 1
- 235000008632 Santalum album Nutrition 0.000 description 1
- 235000007315 Satureja hortensis Nutrition 0.000 description 1
- 240000002114 Satureja hortensis Species 0.000 description 1
- 244000040738 Sesamum orientale Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 235000007769 Vetiveria zizanioides Nutrition 0.000 description 1
- 244000284012 Vetiveria zizanioides Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 229940100198 alkylating agent Drugs 0.000 description 1
- 239000002168 alkylating agent Substances 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 239000012874 anionic emulsifier Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 1
- KHAVLLBUVKBTBG-UHFFFAOYSA-N caproleic acid Natural products OC(=O)CCCCCCCC=C KHAVLLBUVKBTBG-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 235000017803 cinnamon Nutrition 0.000 description 1
- SECPZKHBENQXJG-UHFFFAOYSA-N cis-palmitoleic acid Natural products CCCCCCC=CCCCCCCCC(O)=O SECPZKHBENQXJG-UHFFFAOYSA-N 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- ACTIUHUUMQJHFO-UPTCCGCDSA-N coenzyme Q10 Chemical compound COC1=C(OC)C(=O)C(C\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UPTCCGCDSA-N 0.000 description 1
- 235000017471 coenzyme Q10 Nutrition 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- BITHHVVYSMSWAG-UHFFFAOYSA-N eicosenoic acid Natural products CCCCCCCCC=CCCCCCCCCCC(O)=O BITHHVVYSMSWAG-UHFFFAOYSA-N 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010642 eucalyptus oil Substances 0.000 description 1
- 229940044949 eucalyptus oil Drugs 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229940020356 folic acid and derivative as antianemic Drugs 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010468 hazelnut oil Substances 0.000 description 1
- 235000011167 hydrochloric acid Nutrition 0.000 description 1
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000001102 lavandula vera Substances 0.000 description 1
- 235000018219 lavender Nutrition 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 239000007908 nanoemulsion Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001702 nutmeg Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 229960002969 oleic acid Drugs 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 150000002889 oleic acids Chemical class 0.000 description 1
- RLBIQVVOMOPOHC-UHFFFAOYSA-N parathion-methyl Chemical compound COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C=C1 RLBIQVVOMOPOHC-UHFFFAOYSA-N 0.000 description 1
- 239000003090 pesticide formulation Substances 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 229940068968 polysorbate 80 Drugs 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000473 propyl gallate Substances 0.000 description 1
- 235000010388 propyl gallate Nutrition 0.000 description 1
- 229940075579 propyl gallate Drugs 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- WBHHMMIMDMUBKC-XLNAKTSKSA-N ricinelaidic acid Chemical compound CCCCCC[C@@H](O)C\C=C\CCCCCCCC(O)=O WBHHMMIMDMUBKC-XLNAKTSKSA-N 0.000 description 1
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 239000000541 tocopherol-rich extract Substances 0.000 description 1
- 235000019149 tocopherols Nutrition 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229940040064 ubiquinol Drugs 0.000 description 1
- QNTNKSLOFHEFPK-UPTCCGCDSA-N ubiquinol-10 Chemical compound COC1=C(O)C(C)=C(C\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CCC=C(C)C)C(O)=C1OC QNTNKSLOFHEFPK-UPTCCGCDSA-N 0.000 description 1
- 229940035936 ubiquinone Drugs 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- DTOSIQBPPRVQHS-UHFFFAOYSA-N α-Linolenic acid Chemical compound CCC=CCC=CCC=CCCCCCCCC(O)=O DTOSIQBPPRVQHS-UHFFFAOYSA-N 0.000 description 1
- QUEDXNHFTDJVIY-UHFFFAOYSA-N γ-tocopherol Chemical class OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P7/00—Arthropodicides
- A01P7/04—Insecticides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
本发明描述了一种方法，用于获得作为活性物质的一种或多种除虫菊酯的微生物胶囊，属于生物农药生产技术领域。天然除虫菊酯是从菊属植物的花中提取的广谱杀虫剂，易被空气和光分解。本发明增加了除虫菊酯的稳定性，相比现有技术的其他解决方案，能够更长时间有效。方法和过程包括以下步骤：准备油阶段的第一步、乳化混合物的第二步和包封的第三步。结果是尺寸在0.5至5微米之间的除虫菊酯微生物胶囊的产品，具有更高的稳定性。该过程不会降低除虫菊酯的杀虫能力。
Description
技术领域
本发明属于化学工业领域应用领域，致力于纳米生物农药的生产，具体涉及除虫菊酯纳米乳剂的生产方法。
背景技术
随着社会的发展和农业面积的扩大，产生了对新型、更高效以及安全的杀虫剂的需求。一些高效的化学制剂迅速出现，但在分析作物时出现了大量残留。然而，随着近年来环保意识和认证的发展以及生物技术的进步，杀虫剂生产商开始采取安全、高效、循环经济和人性化的准则，从而实现了无毒、生态和零残留产品。生物农药已成为农化行业的优先生产线。
天然除虫菊酯作为杀虫剂的使用有着悠久的历史，可用于防治影响人类和作物的害虫。天然除虫菊酯是从除虫菊(pyretheum)花朵(除虫菊(Chrysanthemumcinerariaefolium))中提取的杀虫剂，易被光、空气、水和微生物降解。除虫菊酯对破坏作物的昆虫有剧毒，但对温血动物是安全的、无污染、且不留残留物。
为防治害虫，除虫菊酯通常以固体、油、可湿性粉剂和可乳化浓缩物的形式存在。在除虫菊油和浓缩乳液的情况下，其通常与物质和植物衍生物混合，这些是水和环境的污染物。除虫菊酯的包封不仅考虑需要较低剂量的除虫菊酯，而且还保护环境、降低生产成本、增加杀虫剂与其他供应物或其他杀虫剂接触的有效性并阻止活性物质的难闻气味。含有拟除虫菊酯、植物油、溶剂和乳化表面活性剂体系的杀虫剂组合物是已知的(EP 567,368)。同样，含有拟除虫菊酯、可含有植物油的赋形剂、表面活性剂体系和可选的溶剂和稳定剂的可乳化浓缩物是已知的(GB 2,058,569)。含有拟除虫菊酯、植物油和表面活性剂体系的组合物也是已知的，例如由非离子和阴离子表面活性剂的混合物组成(US 4,617,3318)，例如含有拟除虫菊酯、植物油或其他酯的组合物，例如有机溶剂(ES 2,144,618)。然而，这些文件中没有一个声称、提及或能从描述中删去拟除虫菊酯微胶囊。
关于获得微胶囊的过程，从20世纪70年代初至今，微胶囊技术已开始应用于农药剂型加工。但是，具有微胶囊活性物质的产品数量相当有限。1976年，美国Pennwalt公司推出了第一款微胶囊杀虫剂：甲基对硫磷，其可显著降低产品的毒性并延长其作用时间。Pennwalt公司还通过复杂且高成本的过程包封了来自Pennwalt公司的除虫菊酯ES8506420。此后，在微胶囊开发领域进行了不同的调查，特别是在农业领域，至今有200多家农化公司在微胶囊的开发和应用方面具有研究项目。因此，农药微胶囊的发展已有40多年的历史，但与医药行业的发展相比，这是相当缓慢的。因此，市场上基于农药微胶囊的产品种类还很少。
目前的农药微胶囊方法主要包括：聚合、内聚分离阶段和溶剂蒸发。这些方法不仅复杂而且成本高。还大量使用有机溶剂，造成污染。
尽管存在所有这些现有的替代方案，仍然需要提供一种获得除虫菊酯微生物胶囊的过程，该过程不会影响杀虫能力，从而可以用于害虫防治。
发明内容
本发明通过以下方式进行设计，以提供根据本发明的第一方面的，一种获得作为活性物质的一种或多种除虫菊酯的微生物胶囊的过程，该过程包括三个步骤：
1.油制备阶段，由浓度介于48％-80％之间的作为活性物质的一种或多种除虫菊酯以1:20的比例溶解在一种或多种植物油中，可选地进行搅拌，可选地可以加入溶剂，溶剂可以是脂肪酸、醇、精油或它们的混合物，然后对混合物进行搅拌。
2.乳化阶段，其中加入乳化剂和可选的稳定剂和/或防腐剂，同时进行搅拌。此外，可以加入具有抗氧化性能的共配制剂、防腐剂和/或消泡剂。
3.获得微生物胶囊的阶段，其中通过混合过程，优选使用混合器，例如具有桨式搅拌器的混合器，结果是获得介于4-25％p/v，优选4-8％w/v之间，且尺寸在0.5至5微米之间的除虫菊酯微生物胶囊，具有更高的稳定性。
本发明中，除虫菊酯微胶囊是指：具有外膜的微米颗粒，其中含有作为活性物质的除虫菊酯。
在阶段(1)中，加入一种或多种植物油，它们选自由向日葵、玉米、大豆、鳄梨、荷荷巴油、南瓜、葡萄籽、芝麻、榛子油、甘油三己辛酸酯或分子式为R9COOR10的植物油组成的组，其中R9表示包含7至29个碳原子的高级脂肪酸的部分，R10表示包含3至30个碳原子的直链或支链烃链，特别是烷基或烯基、十一烯酸、肉豆蔻油酸、棕榈油酸，油酸、亚油酸、亚麻酸、蓖麻油酸、二十碳烯酸或二十二碳烯酸(存在于松树、玉米、向日葵、大豆、葡萄干种子、亚麻或荷荷巴油中)。作为脂肪酸的优选示例，可以提及包含不饱和分子的脂肪酸，例如油酸类型，其通过双键缩合反应低聚。该反应产生基本上包括二聚体和三聚体的混合物。脂肪酸的二聚体和三聚体是指2或3个相同或不同单体的低聚物。有利地，这些饱和或不饱和的脂肪酸包括12至100个碳原子，更有利地包含24至90个。
在阶段(1)中，以60-150RPM进行搅拌。
在阶段(1)中，温度为20℃至40℃，优选在25℃-35℃之间。
在阶段(1)中，可以加入选自不饱和脂肪酸及其衍生物的溶剂：亚油酸、亚麻酸、油酸、叶酸及其衍生物、泛醌和泛醇及其衍生物、生育酚及其衍生物。
在阶段(1)中，可加入溶剂，溶剂选自乙醇、异丙醇等低级醇；甘油、丙二醇、二丙二醇、山梨糖醇等多元醇；
在阶段(1)中，可以加入选自天然或合成精油的溶解剂，例如桉树油、薰衣草油、薰衣草、香根草、山苍子、柠檬、檀香、迷迭香、洋甘菊、香薄荷、肉豆蔻、肉桂、牛膝草、香菜、橙子、天竺葵、杜松和佛手柑。
在阶段(2)中，加入非离子乳化剂，其以组合物的10至50％重量，优选地，相对于组合物总重量的15至30％重量的比例出现。
非离子乳化剂应理解为是指两性的、阴离子的，优选阳离子的。两性或两性乳化剂应理解为那些表面活性剂化合物，其除了含有8至18个碳原子的烷基或酰基外，分子中还含有至少一个游离氨基和至少一个-COOH或-SO3H基团，适合形成内盐。合适的两性表面活性剂的示例是N-烷基甘氨酸、N-烷基丙酸、N-烷基氨基丁酸、N-烷基亚氨基二丙酸、N-羟乙基-N-烷基酰胺丙基甘氨酸、N-烷基牛磺酸、N-烷基肌氨酸、2-烷基氨基丙酸和烷基氨基乙酸，在每种情况下在烷基中具有约8至18个碳原子。阴离子乳化剂应理解为具有负电荷的那些乳化剂，阴离子表面活性剂的示例是，例如链长为8至18个C原子的烷基硫酸盐、疏水部分中具有8至18个C原子的烷基或烷基芳基醚硫酸盐和最多40个环氧乙烷或环氧丙烷单元、具有8至18个碳原子的烷基或烷基芳基磺酸盐、磺基琥珀酸与一元醇或烷基酚的酯和半酯、烷基或烷基芳基磺酸盐、羟基链烷醇硫酸盐、具有8至24个碳原子的饱和和不饱和链的脂肪酸及其氧化烯化酯，以及聚乙氧基化链烷醇的硫酸盐和磷酸盐。阳离子乳化剂应理解为在水溶液中含有正电荷的那些乳化剂、胺类以及季铵化合物。阳离子乳化剂的示例是具有7至25个碳原子的烷基胺，具有7至25个碳原子的N，N-二甲基-N-(羟烷基)铵盐，与烷基化剂季铵化的单-和二-(具有7至25个碳原子)-烷基二甲基铵盐，诸如酯化的季单-、二-或三链烷醇胺等的酯季铵盐，其与具有8至22个碳原子的羧酸酯化，以及诸如通式I或II的1-烷基咪唑啉盐等的咪唑啉季铵盐。
在阶段(2)中，使用的阳离子乳化剂是季铵化合物，观察到它增加了根据所述过程得到的产品的杀虫能力。
在阶段(2)中，可选地，可以加入第二乳化剂，当使用乳化剂组合时，有利的是使用相对疏水的乳化剂与相对亲水的试剂的组合，或者组合使用阴离子乳化剂与非离子试剂。
在阶段(2)中，通常可以以相对于组合物总重量的10至50％重量，优选15至30％重量的比例，向组合物中加入第二乳化剂。
在阶段(2)中，另外，可以加入共配制剂，其可以选自抗氧化剂例如生育酚和没食子酸丙酯、硝基氧化物、BHT-丁基羟基甲苯、BHA-丁基羟基茴香醚和/或酸化剂，例如，柠檬酸、乳酸和苹果酸、盐酸、酒石酸、磷酸、乳酸、磺酸和/或消泡剂；包含14-24个碳原子的至少一种硅基或氟基脂肪酸。
在阶段(2)中，温度在10-45℃之间，优选在25-35℃之间。
在阶段(3)中，以60-300RPM进行搅拌1至36小时，优选1至4小时。该阶段在密度为0.910-0.980g/cm3和pH值在5-10之间，优选在6.5-8.5之间的受控条件下工作。所述过程的最终结果是获得尺寸在0.5-5μm之间、具有规则形态和光滑表面的除虫菊酯微生物胶囊。
另一方面，本发明涉及本发明的微生物胶囊作为杀虫剂的用途。更具体地，本发明涉及本发明的微胶囊用于防治节肢动物害虫用途，节肢动物例如为昆虫，优选蚜虫和蚂蚁。通过此过程获得的杀虫产品的有效性可持续长达2年。
附图说明
为了补充所做出的描述并帮助更好地理解本发明的特征，附上一组附图作为所述描述的组成部分，其中出于说明性和非限制性的目的，表示以下内容：
图1示出了在正常条件下和14天后在同一化合物中应用MT 46.3方法所得组合物的色谱图。
图2示出了除虫菊酯微生物胶囊的照片，其中观察落射荧光显微镜(Axioplan，ZEISS)。将样品滴放置在具有20×物镜的载玻片(20×40×0.25mm)上。
图3示出了除虫菊酯微生物胶囊的照片，其中标明了它们的大小和单分散性：
1.长度5.14μm
2.长度4.42μm
3.长度5.48μm
4.长度5.14μm
具体实施方式
本发明将通过发明人进行的试验说明如下，这些试验表明了本发明过程的有效性：
实施例1
将73g菊花精制提取物EDEOIL
混合作为60％(w/w)的除虫菊酯来源；除虫菊酯I、瓜菊酯I、茉莉宁I、除虫菊酯II、瓜菊酯II和茉莉宁II，除虫菊酯I和除虫菊酯II的比例为1.85，其中557g的大豆油含有50％的亚油酸和25％的油酸，还含有月桂酸、肉豆蔻酸、棕榈酸、硬脂酸和亚麻酸，在HI
中25℃温度下以60rpm的转速进行搅拌，并加入1g富含生育酚E306的提取物，继续搅拌20分钟，然后不停搅拌，加入158g的99.5％丙二醇和185g的97％聚山梨醇酯80
然后加入15g浓度为94％的D-柠檬烯(苦橙)和8g植物甘油E-422，作为共制剂，从而提高制剂的张力活性。以120rpm转速搅拌约2小时，观察微生物胶囊的外观(图2)，然后根据(图3)测量微胶囊及其形状。
实施例2
为了确定通过如实施例1中所述的本发明过程获得的产物的稳定性，方法MT 46.3(J.Zhang等人，色谱法杂志A辑(J.of Chromatography A.)1218(2011)6621-6629，DeanBan等人，非洲生物技术期刊(Afr.J.of Biotechnology)，卷9(18)，第2702-2708页，2010年5月3日)通过热刺激使制剂老化并模拟包封和储存的产品(图1)。通过测试的制剂被认为至少可以使用2年。
表I
54℃下储存稳定性
Claims (29)
1.一种获得除虫菊酯微生物胶囊的过程，包括以下几个步骤：(1)油阶段，由浓度介于(48％-80％)之间的作为活性物质的一种或多种除虫菊酯以1:20的比例溶解在一种或多种植物油中的溶液组成；(2)乳化阶段，其中加入乳化剂；(3)获得微生物胶囊阶段，其中通过受控制的混合过程，获得4-25％w/v的除虫菊酯微生物胶囊。
2.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(1)中，动物油或植物油选自由向日葵、玉米、大豆、鳄梨、荷荷巴油、南瓜、葡萄籽、芝麻、榛子、鱼油、甘油三己辛酸酯或分子式为R9COOR10的植物油或动物油组成的组，其中R9表示包括7至29个碳原子的高级脂肪酸的部分，R10表示包含3至30个碳原子的直链或支链烃链，特别是烷基或烯基。
3.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(1)中，以60-150RPM进行搅拌。
4.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(1)中，温度为20℃至40℃。
5.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(1)中，可以加入溶剂，例如脂肪酸及其衍生物。
6.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(1)中，可以加入溶剂，例如低级醇。
7.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(1)中，可以加入溶剂，例如天然或合成精油。
8.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(1)中，可以加入溶剂，其可以是权利要求5、6和/或7的混合物。
9.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(2)中，加入非离子乳化剂，其相对于组合物的总重量以组合物的10至50％重量的比例出现。
10.在权利要求9中，加入的所述非离子乳化剂是两性或两性类型的。
11.在权利要求9中，加入的所述非离子乳化剂是阴离子型的。
12.在权利要求9中，加入的所述非离子乳化剂是阳离子型的。
13.在权利要求9中，第二相对疏水的乳化剂可以与相对亲水的试剂组合加入。
14.在权利要求13中，所述乳化剂是与非离子试剂组合的阴离子。
15.在权利要求13中，所述乳化剂通常以介于10至50％重量范围之间的比例存在于组合物中。
16.在权利要求9中，还可以加入共配制剂。
17.在权利要求16中，所述共配制剂可以是抗氧化剂。
18.在权利要求16中，所述共配制剂可以是酸化剂。
19.在权利要求16中，所述共配制剂可以是消泡剂。
20.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(2)中，温度在10℃-45℃之间。
21.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(3)中，以60-300RPM进行搅拌1至36小时。
22.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(3)中，以0.910g/cm3至0.980g/cm3之间的密度生产所述除虫菊酯微生物胶囊。
23.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(3)中，所述过程在5-10之间的pH下进行。
24.根据权利要求1所述的获得除虫菊酯微生物胶囊的过程，其特征在于在阶段(3)中，生产尺寸在0.5μ至5μ之间的微生物胶囊。
25.根据权利要求1所述的过程得到的包封产品的用途为防治害虫。
26.根据权利要求25所述的用途，其中它是杀虫剂。
27.根据权利要求26所述的用途，其中它是拟除虫菊酯。
28.根据权利要求25所述的用途，具有至少2年的最佳功效持久性。
29.根据权利要求25所述的用途，其中在阶段(2)中加入的乳化剂是增加杀虫能力的阳离子乳化剂。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ES201930434A ES2794124B8 (es) | 2019-05-17 | 2019-05-17 | Método y procedimiento de obtención de microbiocápsulas de piretrinas naturales con alta estabilidad |
| ESP201930434 | 2019-05-17 | ||
| PCT/ES2020/000026 WO2020234492A2 (es) | 2019-05-17 | 2020-05-18 | Método y procedimiento de obtención de microbiocápsulas de piretrinas naturales con alta estabilidad |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114072226A true CN114072226A (zh) | 2022-02-18 |
Family
ID=73197495
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202080046321.9A Pending CN114072226A (zh) | 2019-05-17 | 2020-05-18 | 一种获得高稳定性天然除虫菊酯微生物胶囊的方法和过程 |
Country Status (10)
| Country | Link |
|---|---|
| US (1) | US20220225619A1 (zh) |
| EP (1) | EP3970847A4 (zh) |
| CN (1) | CN114072226A (zh) |
| BR (1) | BR112021023036A2 (zh) |
| CL (1) | CL2021003028A1 (zh) |
| ES (1) | ES2794124B8 (zh) |
| MA (1) | MA55980A (zh) |
| MX (1) | MX2021014011A (zh) |
| PE (1) | PE20220385A1 (zh) |
| WO (1) | WO2020234492A2 (zh) |
Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2058569A (en) * | 1979-09-12 | 1981-04-15 | Montedison Spa | Liquid insecticide compositions containing synthetic pyrethroids |
| WO1992022206A1 (en) * | 1991-06-12 | 1992-12-23 | Mitsui Toatsu Chemicals, Incorporated | Insecticidal composition and production thereof |
| US5700473A (en) * | 1995-08-24 | 1997-12-23 | W. Neudorff Gmbh Kg | Triglyceride enhanced pyrethrin-based arthropodicidal composition |
| KR20060071380A (ko) * | 2006-06-02 | 2006-06-26 | 김규석 | 식물 추출물을 이용한 생물 농약으로써의 천연 살충제 |
| CN100998331A (zh) * | 2006-01-10 | 2007-07-18 | 潘贞德 | 以除虫菊酯为原料的一组微乳剂杀虫剂 |
| CN101406177A (zh) * | 2008-11-24 | 2009-04-15 | 上海龙蟒生物科技有限公司 | 杀虫剂组合物浓缩液及其使用方法 |
| WO2010044832A2 (en) * | 2008-10-17 | 2010-04-22 | Appleton Papers Inc. | An agriculture actives delivery composition comprising boron and persulfate ion-crosslinked polyvinyl alcohol mocrocapsules and metod of use thereof |
| CN102845456A (zh) * | 2012-10-11 | 2013-01-02 | 聊城大学 | 一种氯氰菊酯乳油杀虫剂 |
| CN103004858A (zh) * | 2012-11-28 | 2013-04-03 | 李建中 | 一种含有甲胺基阿维菌素和拟除虫菊酯化合物的杀虫组合物 |
| ES2444991A1 (es) * | 2012-08-27 | 2014-02-27 | Seipasa S.A. | Un insecticida ecológico, procedimiento de producción del insecticida y utilización del mismo |
| CA2937809A1 (en) * | 2014-02-19 | 2015-08-27 | Fmc Corporation | High-load pyrethroid encapsulated seed treatment formulations |
| CN105409944A (zh) * | 2015-12-31 | 2016-03-23 | 周德志 | 除虫菊酯微胶囊的制备方法 |
| JP5938762B1 (ja) * | 2015-09-01 | 2016-06-22 | 日揮株式会社 | マイクロカプセル製剤及びその製造方法 |
| CN106508895A (zh) * | 2016-09-05 | 2017-03-22 | 广东康绿宝科技实业有限公司 | 一种安全型杀虫释放控制组合 |
| CN108887291A (zh) * | 2018-06-21 | 2018-11-27 | 同济大学 | 一种天然除虫菊酯微胶囊及其制备方法 |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4617318A (en) | 1981-09-25 | 1986-10-14 | American Cyanamid Company | Non-irritating pyrethroid formulations in vegetable oils and tall oils |
| ES535633A0 (es) | 1984-09-04 | 1985-08-01 | Pennwalt Corp | Un procedimiento de microencapsular piretrinas existentes en la naturaleza |
| FR2689729B1 (fr) | 1992-04-09 | 1994-06-03 | Roussel Uclaf | Nouvelles compositions pesticides renfermant un pyrethrinouide. |
| FR2721800B1 (fr) | 1994-07-01 | 1997-12-26 | Roussel Uclaf | Nouveaux concentres emulsionnables renfermant un u plussieurs pesticides |
| CN102239890B (zh) * | 2011-08-04 | 2013-08-07 | 华南农业大学 | 一种用于防治螺旋粉虱的微胶囊悬浮剂及其制备方法 |
| CN103039463B (zh) * | 2012-12-31 | 2014-04-23 | 深圳市华农生物工程有限公司 | 一种鱼藤酮微乳剂及其制备方法 |
| CN108041082A (zh) * | 2017-12-26 | 2018-05-18 | 同济大学 | 一种除虫菊酯的脲醛树脂-光稳定剂复合壁材微胶囊剂及其制备方法和应用 |
| CN108739872A (zh) * | 2018-06-21 | 2018-11-06 | 同济大学 | 一种天然除虫菊酯微胶囊及其制备方法 |
-
2019
- 2019-05-17 ES ES201930434A patent/ES2794124B8/es active Active
-
2020
- 2020-05-18 MA MA055980A patent/MA55980A/fr unknown
- 2020-05-18 EP EP20809227.0A patent/EP3970847A4/en active Pending
- 2020-05-18 MX MX2021014011A patent/MX2021014011A/es unknown
- 2020-05-18 PE PE2021001905A patent/PE20220385A1/es unknown
- 2020-05-18 WO PCT/ES2020/000026 patent/WO2020234492A2/es active Application Filing
- 2020-05-18 BR BR112021023036A patent/BR112021023036A2/pt unknown
- 2020-05-18 CN CN202080046321.9A patent/CN114072226A/zh active Pending
- 2020-05-18 US US17/611,865 patent/US20220225619A1/en active Pending
-
2021
- 2021-11-16 CL CL2021003028A patent/CL2021003028A1/es unknown
Patent Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2058569A (en) * | 1979-09-12 | 1981-04-15 | Montedison Spa | Liquid insecticide compositions containing synthetic pyrethroids |
| WO1992022206A1 (en) * | 1991-06-12 | 1992-12-23 | Mitsui Toatsu Chemicals, Incorporated | Insecticidal composition and production thereof |
| US5700473A (en) * | 1995-08-24 | 1997-12-23 | W. Neudorff Gmbh Kg | Triglyceride enhanced pyrethrin-based arthropodicidal composition |
| CN100998331A (zh) * | 2006-01-10 | 2007-07-18 | 潘贞德 | 以除虫菊酯为原料的一组微乳剂杀虫剂 |
| KR20060071380A (ko) * | 2006-06-02 | 2006-06-26 | 김규석 | 식물 추출물을 이용한 생물 농약으로써의 천연 살충제 |
| WO2010044832A2 (en) * | 2008-10-17 | 2010-04-22 | Appleton Papers Inc. | An agriculture actives delivery composition comprising boron and persulfate ion-crosslinked polyvinyl alcohol mocrocapsules and metod of use thereof |
| CN101406177A (zh) * | 2008-11-24 | 2009-04-15 | 上海龙蟒生物科技有限公司 | 杀虫剂组合物浓缩液及其使用方法 |
| ES2444991A1 (es) * | 2012-08-27 | 2014-02-27 | Seipasa S.A. | Un insecticida ecológico, procedimiento de producción del insecticida y utilización del mismo |
| CN102845456A (zh) * | 2012-10-11 | 2013-01-02 | 聊城大学 | 一种氯氰菊酯乳油杀虫剂 |
| CN103004858A (zh) * | 2012-11-28 | 2013-04-03 | 李建中 | 一种含有甲胺基阿维菌素和拟除虫菊酯化合物的杀虫组合物 |
| CA2937809A1 (en) * | 2014-02-19 | 2015-08-27 | Fmc Corporation | High-load pyrethroid encapsulated seed treatment formulations |
| JP5938762B1 (ja) * | 2015-09-01 | 2016-06-22 | 日揮株式会社 | マイクロカプセル製剤及びその製造方法 |
| CN105409944A (zh) * | 2015-12-31 | 2016-03-23 | 周德志 | 除虫菊酯微胶囊的制备方法 |
| CN106508895A (zh) * | 2016-09-05 | 2017-03-22 | 广东康绿宝科技实业有限公司 | 一种安全型杀虫释放控制组合 |
| CN108887291A (zh) * | 2018-06-21 | 2018-11-27 | 同济大学 | 一种天然除虫菊酯微胶囊及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP3970847A2 (en) | 2022-03-23 |
| EP3970847A4 (en) | 2023-02-08 |
| WO2020234492A3 (es) | 2021-01-14 |
| US20220225619A1 (en) | 2022-07-21 |
| PE20220385A1 (es) | 2022-03-18 |
| MX2021014011A (es) | 2022-02-11 |
| MA55980A (fr) | 2022-03-23 |
| WO2020234492A2 (es) | 2020-11-26 |
| ES2794124B2 (es) | 2021-09-14 |
| ES2794124A1 (es) | 2020-11-17 |
| ES2794124B8 (es) | 2021-10-07 |
| BR112021023036A2 (pt) | 2021-12-28 |
| CL2021003028A1 (es) | 2022-06-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| DE69219373T3 (de) | Biozide und agrochemische Suspensionen | |
| DE69728172T2 (de) | Mikroemulsion und verfahren | |
| JP2019011340A (ja) | 殺有害生物剤のスプレードリフトを制御するためのマイクロカプセル化油 | |
| WO2013054194A1 (en) | A formulated solvent composition for pesticide | |
| JPS6362481B2 (zh) | ||
| US6171608B1 (en) | Insecticide formulations | |
| US8808762B2 (en) | Cinnamaldehyde and diallyl disulfide formulations and methods of use | |
| KR950006927B1 (ko) | 수중유 유탁액 및 그것의 제조방법 | |
| CN102388912A (zh) | 一种噻唑膦水乳剂及其制备方法 | |
| EP1082007B1 (de) | Wässrige, agrochemische Wirkstoffe enthaltende Mittel | |
| CN114072226A (zh) | 一种获得高稳定性天然除虫菊酯微生物胶囊的方法和过程 | |
| WO2012057610A2 (en) | A potentiator for soluble liquid herbicide | |
| JP2016145177A (ja) | 農園芸用乳剤およびその調製方法 | |
| DE69720770T2 (de) | Verfahren zur Bekämpfung kriechender Insekten mittels Mikroemulsionen | |
| CN101611708A (zh) | 一种鱼藤酮微乳剂 | |
| Mohsin et al. | Influence of surfactant structure on physical stability and physicochemical properties of insecticide emulsions | |
| WO2014047021A1 (en) | Cinnamaldehyde and diallyl disulfide formulations and methods of use | |
| US20230354824A1 (en) | Minimum Risk Pesticide Formulations Containing Mineral Oil | |
| WO2016111661A1 (en) | Capsule formulation technique for insect growth regulator pyriproxyfen, a juvenile hormone analog | |
| US20240148005A1 (en) | Mineral Oil And Water-Based Pesticide Formulations | |
| US20230354825A1 (en) | Water-Based Pesticide Formulations For Yard Applications | |
| IT202100021710A1 (it) | Composizione concentrata emulsionabile comprendente carvacrolo e/o timolo. | |
| CN109221232A (zh) | 一种水基杀虫微乳剂及其制备方法 | |
| Libertyville et al. | Belkind et al.(43) Pub. Date: Jan. 17, 2013 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |