CN117617240A - Long-acting volatile electrothermal mosquito-repellent incense liquid and preparation method thereof - Google Patents
Long-acting volatile electrothermal mosquito-repellent incense liquid and preparation method thereof Download PDFInfo
- Publication number
- CN117617240A CN117617240A CN202210953603.8A CN202210953603A CN117617240A CN 117617240 A CN117617240 A CN 117617240A CN 202210953603 A CN202210953603 A CN 202210953603A CN 117617240 A CN117617240 A CN 117617240A
- Authority
- CN
- China
- Prior art keywords
- component
- repellent liquid
- cyano
- tetrafluorobenzyl
- vinyl
- 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
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- 239000007788 liquid Substances 0.000 title claims abstract description 77
- 239000000077 insect repellent Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- 238000005485 electric heating Methods 0.000 claims abstract description 16
- 230000005923 long-lasting effect Effects 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 59
- 239000000203 mixture Substances 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 25
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 22
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 22
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical group OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 claims description 16
- -1 ethyl ethoxy ester Chemical class 0.000 claims description 10
- 239000003759 ester based solvent Substances 0.000 claims description 8
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 6
- 229940093609 tricaprylin Drugs 0.000 claims description 6
- VLPFTAMPNXLGLX-UHFFFAOYSA-N trioctanoin Chemical compound CCCCCCCC(=O)OCC(OC(=O)CCCCCCC)COC(=O)CCCCCCC VLPFTAMPNXLGLX-UHFFFAOYSA-N 0.000 claims description 6
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 4
- 239000003755 preservative agent Substances 0.000 claims description 4
- 150000003627 tricarboxylic acid derivatives Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 125000000008 (C1-C10) alkyl group Chemical group 0.000 claims description 2
- ZZXUZKXVROWEIF-UHFFFAOYSA-N 1,2-butylene carbonate Chemical compound CCC1COC(=O)O1 ZZXUZKXVROWEIF-UHFFFAOYSA-N 0.000 claims description 2
- LAVARTIQQDZFNT-UHFFFAOYSA-N 1-(1-methoxypropan-2-yloxy)propan-2-yl acetate Chemical compound COCC(C)OCC(C)OC(C)=O LAVARTIQQDZFNT-UHFFFAOYSA-N 0.000 claims description 2
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 claims description 2
- AIAMDEVDYXNNEU-UHFFFAOYSA-N 6-methylheptyl propanoate Chemical compound CCC(=O)OCCCCCC(C)C AIAMDEVDYXNNEU-UHFFFAOYSA-N 0.000 claims description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- 239000004288 Sodium dehydroacetate Substances 0.000 claims description 2
- 239000005456 alcohol based solvent Substances 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 claims description 2
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 claims description 2
- KWKXNDCHNDYVRT-UHFFFAOYSA-N dodecylbenzene Chemical compound CCCCCCCCCCCCC1=CC=CC=C1 KWKXNDCHNDYVRT-UHFFFAOYSA-N 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- NZYMWGXNIUZYRC-UHFFFAOYSA-N hexadecyl 3,5-ditert-butyl-4-hydroxybenzoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NZYMWGXNIUZYRC-UHFFFAOYSA-N 0.000 claims description 2
- PKAHQJNJPDVTDP-UHFFFAOYSA-N methyl cyclopropanecarboxylate Chemical compound COC(=O)C1CC1 PKAHQJNJPDVTDP-UHFFFAOYSA-N 0.000 claims description 2
- 150000004702 methyl esters Chemical class 0.000 claims description 2
- 235000010241 potassium sorbate Nutrition 0.000 claims description 2
- 239000004302 potassium sorbate Substances 0.000 claims description 2
- 229940069338 potassium sorbate Drugs 0.000 claims description 2
- 230000002335 preservative effect Effects 0.000 claims description 2
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical group [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 2
- 235000010234 sodium benzoate Nutrition 0.000 claims description 2
- 239000004299 sodium benzoate Substances 0.000 claims description 2
- 229960003885 sodium benzoate Drugs 0.000 claims description 2
- 235000019259 sodium dehydroacetate Nutrition 0.000 claims description 2
- 229940079839 sodium dehydroacetate Drugs 0.000 claims description 2
- DSOWAKKSGYUMTF-GZOLSCHFSA-M sodium;(1e)-1-(6-methyl-2,4-dioxopyran-3-ylidene)ethanolate Chemical compound [Na+].C\C([O-])=C1/C(=O)OC(C)=CC1=O DSOWAKKSGYUMTF-GZOLSCHFSA-M 0.000 claims description 2
- WERKSKAQRVDLDW-ANOHMWSOSA-N [(2s,3r,4r,5r)-2,3,4,5,6-pentahydroxyhexyl] (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO WERKSKAQRVDLDW-ANOHMWSOSA-N 0.000 claims 1
- 239000012752 auxiliary agent Substances 0.000 claims 1
- 239000004480 active ingredient Substances 0.000 abstract description 2
- 231100000053 low toxicity Toxicity 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 21
- 238000009472 formulation Methods 0.000 description 20
- HBTAOSGHCXUEKI-UHFFFAOYSA-N 4-chloro-n,n-dimethyl-3-nitrobenzenesulfonamide Chemical compound CN(C)S(=O)(=O)C1=CC=C(Cl)C([N+]([O-])=O)=C1 HBTAOSGHCXUEKI-UHFFFAOYSA-N 0.000 description 13
- 229940031578 diisopropyl adipate Drugs 0.000 description 13
- 239000003814 drug Substances 0.000 description 10
- 229940079593 drug Drugs 0.000 description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- HIQIXEFWDLTDED-UHFFFAOYSA-N 4-hydroxy-1-piperidin-4-ylpyrrolidin-2-one Chemical compound O=C1CC(O)CN1C1CCNCC1 HIQIXEFWDLTDED-UHFFFAOYSA-N 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- MSQKMFXJFBXZNQ-UHFFFAOYSA-N dipropan-2-yl pentanedioate Chemical compound CC(C)OC(=O)CCCC(=O)OC(C)C MSQKMFXJFBXZNQ-UHFFFAOYSA-N 0.000 description 5
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002728 pyrethroid Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 241000255925 Diptera Species 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 2
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-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
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- 241000607479 Yersinia pestis Species 0.000 description 2
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 125000005908 glyceryl ester group Chemical group 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 239000002917 insecticide Substances 0.000 description 2
- KVSRWNPBUMDYOQ-UHFFFAOYSA-N methyl 3-formyl-2,2-dimethylcyclopropane-1-carboxylate Chemical compound COC(=O)C1C(C=O)C1(C)C KVSRWNPBUMDYOQ-UHFFFAOYSA-N 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- YCOZIPAWZNQLMR-UHFFFAOYSA-N pentadecane Chemical compound CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 description 2
- WLJVXDMOQOGPHL-UHFFFAOYSA-N phenylacetic acid Chemical compound OC(=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-UHFFFAOYSA-N 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- IIYFAKIEWZDVMP-UHFFFAOYSA-N tridecane Chemical compound CCCCCCCCCCCCC IIYFAKIEWZDVMP-UHFFFAOYSA-N 0.000 description 2
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
- AGWVQASYTKCTCC-UHFFFAOYSA-N (2,3,5,6-tetrafluorophenyl)methanol Chemical compound OCC1=C(F)C(F)=CC(F)=C1F AGWVQASYTKCTCC-UHFFFAOYSA-N 0.000 description 1
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 1
- FEXBEKLLSUWSIM-UHFFFAOYSA-N 2-Butyl-4-methylphenol Chemical compound CCCCC1=CC(C)=CC=C1O FEXBEKLLSUWSIM-UHFFFAOYSA-N 0.000 description 1
- COBPKKZHLDDMTB-UHFFFAOYSA-N 2-[2-(2-butoxyethoxy)ethoxy]ethanol Chemical compound CCCCOCCOCCOCCO COBPKKZHLDDMTB-UHFFFAOYSA-N 0.000 description 1
- CNPVJWYWYZMPDS-UHFFFAOYSA-N 2-methyldecane Chemical compound CCCCCCCCC(C)C CNPVJWYWYZMPDS-UHFFFAOYSA-N 0.000 description 1
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000256059 Culex pipiens Species 0.000 description 1
- RDOFJDLLWVCMRU-UHFFFAOYSA-N Diisobutyl adipate Chemical compound CC(C)COC(=O)CCCCC(=O)OCC(C)C RDOFJDLLWVCMRU-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- SSMBXPJYHMZLOJ-UHFFFAOYSA-N Isopropyl phenylacetate Chemical compound CC(C)OC(=O)CC1=CC=CC=C1 SSMBXPJYHMZLOJ-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
- 231100000460 acute oral toxicity Toxicity 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- DHAZIUXMHRHVMP-UHFFFAOYSA-N butyl tetradecanoate Chemical compound CCCCCCCCCCCCCC(=O)OCCCC DHAZIUXMHRHVMP-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- XLOPRKKSAJMMEW-UHFFFAOYSA-N chrysanthemic acid Chemical group CC(C)=CC1C(C(O)=O)C1(C)C XLOPRKKSAJMMEW-UHFFFAOYSA-N 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- YMGUBTXCNDTFJI-UHFFFAOYSA-N cyclopropanecarboxylic acid Chemical class OC(=O)C1CC1 YMGUBTXCNDTFJI-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- 229940031769 diisobutyl adipate Drugs 0.000 description 1
- QKIUAMUSENSFQQ-UHFFFAOYSA-N dimethylazanide Chemical group C[N-]C QKIUAMUSENSFQQ-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003640 drug residue Substances 0.000 description 1
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- XUGNVMKQXJXZCD-UHFFFAOYSA-N isopropyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC(C)C XUGNVMKQXJXZCD-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- KVSRWNPBUMDYOQ-WDSKDSINSA-N methyl (1r,3s)-3-formyl-2,2-dimethylcyclopropane-1-carboxylate Chemical compound COC(=O)[C@@H]1[C@H](C=O)C1(C)C KVSRWNPBUMDYOQ-WDSKDSINSA-N 0.000 description 1
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 description 1
- 229940073769 methyl oleate Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229960003424 phenylacetic acid Drugs 0.000 description 1
- 239000003279 phenylacetic acid Substances 0.000 description 1
- 229910052700 potassium Chemical group 0.000 description 1
- 239000011591 potassium Chemical group 0.000 description 1
- CZYGEVQQOCNIML-UHFFFAOYSA-N propan-2-yl tridecanoate Chemical compound CCCCCCCCCCCCC(=O)OC(C)C CZYGEVQQOCNIML-UHFFFAOYSA-N 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 125000000391 vinyl group Chemical class [H]C([*])=C([H])[H] 0.000 description 1
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
- 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
- A01N25/20—Combustible or heat-generating compositions
-
- 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
- A01N25/18—Vapour or smoke emitting compositions with delayed or sustained release
-
- 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
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P17/00—Pest repellants
-
- 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
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- 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
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Abstract
本发明公开了一种长效挥发电热蚊香液及其制备方法，包括以下重量百分比的组分：0.4％‑3％的组分A、7％‑99.5％的组分B、0.01％‑90％的组分C和0.01％～3％的其他助剂；所述的组分A为式(I)所示的化合物；所述的组分B为溶剂；所述的组分C为芯棒疏通剂。本发明的电热蚊香液配制不同含量均能持续稳定挥发，不会堵塞芯棒，满足长效挥发时长需求。且活性成分毒性低，对人的安全性高； The invention discloses a long-lasting volatile electric heating mosquito repellent liquid and a preparation method thereof, which includes the following components by weight: 0.4%-3% component A, 7%-99.5% component B, 0.01%-90% Component C and 0.01% to 3% of other additives; the component A is a compound represented by formula (I); the component B is a solvent; the component C is a mandrel rod dredging agent. The electric mosquito-repellent liquid prepared with different contents of the present invention can volatilize continuously and stably without clogging the mandrel, thus meeting the demand for long-lasting volatilization time. And the active ingredients have low toxicity and high safety to humans;
Description
技术领域Technical field
本发明涉及一种长效挥发电热蚊香液及其制备方法，可用于配制不同含量液体蚊香，仍能保证原药持续稳定挥发，不会堵塞芯棒，避免药剂损失，满足长效挥发时长需求。The invention relates to a long-lasting volatile electric heating mosquito-repellent liquid and a preparation method thereof, which can be used to prepare liquid mosquito-repellent liquid with different contents, and can still ensure the continuous and stable volatilization of the original drug without clogging the mandrel, avoid the loss of the medicine, and meet the long-lasting volatilization time requirement.
背景技术Background technique
式I所示的拟除虫菊酯化合物是一种新颖的卫生杀虫剂，有很好的防治卫生害虫的基础活性；式I所示的拟除虫菊酯化合物可按如下反应路线制备：The pyrethroid compound represented by formula I is a novel sanitary insecticide with good basic activity in preventing and controlling sanitary pests; the pyrethroid compound represented by formula I can be prepared according to the following reaction route:
其中R为甲基或乙基，M为钠或钾R1为氢。Where R is methyl or ethyl, M is sodium or potassium and R1 is hydrogen.
例如，以3-甲酰基-2,2-二甲基环丙烷羧酸甲酯(CAS号62138-41-4)为起始原料，和乙腈在60℃，乙醇钠作用下发生缩合反应4小时，加烯盐酸中和pH到8，加入乙酸乙酯及水分液，油层脱溶得到中间体3-(2-氰基-1-乙烯基)-2,2-二甲基环丙烷羧酸甲酯。For example, 3-formyl-2,2-dimethylcyclopropanecarboxylic acid methyl ester (CAS No. 62138-41-4) is used as the starting material, and acetonitrile undergoes a condensation reaction under the action of sodium ethoxide at 60°C for 4 hours. , add enene hydrochloric acid to neutralize the pH to 8, add ethyl acetate and water to separate, and desolubilize the oil layer to obtain the intermediate 3-(2-cyano-1-vinyl)-2,2-dimethylcyclopropanecarboxylic acid methyl ester.
在得到的3-(2-氰基-1-乙烯基)-2,2-二甲基环丙烷羧酸甲酯中加入2,3,5,6-四氟苄醇(CAS号4084-38-2)、催化量钛酸四异丙酯及甲苯溶剂，缓慢升温至回流采出副产甲醇，气相中控，待原料转化完全后，降温至0-5℃，滴加少量的水，分液，脱溶，得到式I的拟除虫菊酯化合物。Add 2,3,5,6-tetrafluorobenzyl alcohol (CAS No. 4084-38) to the obtained methyl 3-(2-cyano-1-vinyl)-2,2-dimethylcyclopropanecarboxylate. -2), use catalytic amounts of tetraisopropyl titanate and toluene solvent, slowly heat up to reflux to extract the by-product methanol, and control the gas phase. After the raw materials are completely converted, cool down to 0-5°C, add a small amount of water dropwise, and separate. liquid and desolvated to obtain the pyrethroid compound of formula I.
以不同单一构型的环丙烷羧酸酯为起始原料，可以得到相应构型的式I的拟除虫菊酯化合物，例如以(1R,3R)-3-甲酰基-2,2-二甲基环丙烷羧酸甲酯(CAS号27335-33-7)为起始原料合成，得到的是菊酸部分1R，3R的产物，再进行分布结晶，分离双键CN基Z,E异构体，可得到单一的2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯或2,3,4,5-四氟苄基-(1R，3R)-3-[(1E)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯。以(1R,3S)-3-甲酰基-2,2-二甲基环丙烷羧酸甲酯(CAS号55701-02-5)，可得到2,3,4,5-四氟苄基-(1R，3S)-3-(-2-氰基-1-乙烯基)-2,2-二甲基环丙基羧酸酯或2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯或2,3,4,5-四氟苄基-(1R，3S)-3-[(1E)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯。Using cyclopropanecarboxylic acid esters of different single configurations as starting materials, pyrethroid compounds of formula I with corresponding configurations can be obtained, for example, (1R,3R)-3-formyl-2,2-dimethyl Methyl cyclopropanecarboxylate (CAS No. 27335-33-7) is used as the starting raw material for synthesis. What is obtained is the 1R and 3R products of the chrysanthemic acid part. Distribution crystallization is then carried out to separate the double bond CN group Z and E isomers. A single 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropane can be obtained carboxylate or 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1E)-2-cyano-1-vinyl]-2,2-dimethylcyclo Propyl carboxylate. Using (1R,3S)-3-formyl-2,2-dimethylcyclopropanecarboxylic acid methyl ester (CAS No. 55701-02-5), 2,3,4,5-tetrafluorobenzyl- (1R,3S)-3-(-2-cyano-1-vinyl)-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-(1R , 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-( 1R,3S)-3-[(1E)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate.
目前市场电热蚊香液使用时长受限，配制高时长需要提高药液原药含量，而原药含量的提高会带来一系列问题，如出现原药挥发不均匀现象，造成芯棒堵塞、后期原药残留含量较高的问题，从而影响药效。为了解决上述问题，本发明通过优选溶剂，并添加可协助原药挥发的芯棒疏通剂，确保高含量电热蚊香液仍可持续均匀挥发，无堵塞芯棒的风险，从而为不同时长液体蚊香的开发提供了可能。另一方面目前人们对生活品质的要求越来越高，低毒、环保、无刺激等概念深入人心，通过开发长效挥发电热蚊香液，相同体积药液使用时间更久，满足低碳环保的发展理念。本发明的式(I)所示的化合物急性经口毒性评级为微毒，使用安全性更高，开发这类安全性更高的原药配制液体蚊香符合社会发展需要。At present, the use time of electric mosquito-repellent liquid in the market is limited. To prepare the liquid for a long time, the content of the original drug in the liquid must be increased. The increase in the content of the original drug will bring about a series of problems, such as uneven volatilization of the original drug, resulting in clogging of the mandrel and late-stage original drug. The problem of high drug residue content affects the efficacy of the drug. In order to solve the above problems, the present invention optimizes the solvent and adds a mandrel dredging agent that can assist the volatilization of the original drug to ensure that the high-content electric mosquito-repellent liquid can continue to evaporate evenly without the risk of clogging the mandrel, thereby providing solutions for the production of liquid mosquito-repellent incense of different durations. Development offers possibilities. On the other hand, people are now having higher and higher requirements for the quality of life, and concepts such as low toxicity, environmental protection, and non-irritation are deeply rooted in the hearts of the people. Through the development of long-lasting volatile electric heating mosquito repellent liquid, the same volume of liquid can be used longer, meeting the requirements of low carbon and environmental protection. development concept. The acute oral toxicity of the compound represented by formula (I) of the present invention is rated as slightly toxic, and it is safer to use. The development of such safer original drugs to prepare liquid mosquito coils meets the needs of social development.
发明内容Contents of the invention
本发明所要解决的技术问题是针对现有技术中存在的不足，而提供一种长效挥发电热蚊香液及其制备方法，能够稳定可持续的均匀挥发，不会堵塞芯棒，避免药剂损失，满足长效挥发时长需求。The technical problem to be solved by the present invention is to provide a long-lasting volatile electric heating mosquito repellent liquid and a preparation method thereof in view of the deficiencies in the existing technology, which can evaporate stably and sustainably evenly without clogging the core rod and avoiding the loss of the medicine. Meet the demand for long-lasting evaporation time.
为了实现上述目的，本发明采用如下技术方案：In order to achieve the above objects, the present invention adopts the following technical solutions:
一种长效挥发电热蚊香液，按重量计，包含0.4％-3％的组分A、7％-99.5％的组分B、0.01％-90％的组分C和0.01％～3％的其他助剂；A long-lasting volatile electric heating mosquito repellent liquid, by weight, contains 0.4%-3% component A, 7%-99.5% component B, 0.01%-90% component C and 0.01%-3% Other auxiliaries;
所述的组分A为式(I)所示的化合物，即2,3,4,5-四氟苄基-3-[-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯；The component A is a compound represented by formula (I), namely 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate;
所述的组分B为溶剂；The component B is a solvent;
所述的组分C为芯棒疏通剂；The component C is a mandrel dredging agent;
上述技术方案中，所示的组分A，优选自2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯、2,3,4,5-四氟苄基-(1S，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯、2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯、2,3,4,5-四氟苄基-(1S，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯四个异构体中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the component A shown is preferably from 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl] -2,2-Dimethylcyclopropylcarboxylate, 2,3,4,5-tetrafluorobenzyl-(1S,3R)-3-[(1Z)-2-cyano-1-vinyl ]-2,2-Dimethylcyclopropylcarboxylate, 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-ethylene [(1Z)-2-cyano-1- A mixture of any one or two or more of the four isomers of vinyl]-2,2-dimethylcyclopropylcarboxylate in any proportion.
上述技术方案中，所述的组分A，进一步优选为2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯。In the above technical solution, the component A is further preferably 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl ]-2,2-dimethylcyclopropylcarboxylate.
上述技术方案中，所述组分B，选自酰胺类溶剂，一元羧酸酯类溶剂，二元羧酸酯类溶剂，三元羧酸酯类溶剂，C8-20的烷烃类溶剂，水，十二烷基苯，十烷基苯，C2-8的醇类溶剂中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the component B is selected from amide solvents, monocarboxylic acid ester solvents, dicarboxylic acid ester solvents, tricarboxylic acid ester solvents, C8-20 alkane solvents, water, A mixture of any one or two or more of dodecylbenzene, dedecylbenzene, and C2-8 alcohol solvents in any proportion.
上述技术方案中，所述的酰胺类溶剂选自N，N-二甲基葵酰胺。In the above technical solution, the amide solvent is selected from N, N-dimethyl amide.
上述技术方案中，所述的一元羧酸酯类溶剂选自油酸甲酯、十三酸异丙酯、十四酸异丙酯、十六酸异丙酯、苯乙酸异丙酯、苯乙酸乙酯、十四酸正丁酯中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the monocarboxylic acid ester solvent is selected from the group consisting of methyl oleate, isopropyl tridecanoate, isopropyl myristate, isopropyl hexadecanoate, isopropyl phenylacetate, and phenylacetic acid. Any one or a mixture of two or more of ethyl ester and n-butyl myristate in any proportion.
上述技术方案中，所述的二元羧酸酯类溶剂选自戊二酸二异丙酯、己二酸二异丙酯、己二酸二异丁酯中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the dicarboxylic acid ester solvent is selected from any one or two or more of diisopropyl glutarate, diisopropyl adipate, and diisobutyl adipate. Mixtures in any proportions.
上述技术方案中，所述的三元羧酸酯类溶剂选自柠檬酸三丁酯、乙酰柠檬酸三丁酯中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the tricarboxylic acid ester solvent is selected from any one of tributyl citrate and acetyl tributyl citrate or a mixture of two or more in any proportion.
上述技术方案中，所述的醇醚类溶剂选自三乙二醇单丁醚、二乙二醇单丁醚、丙二醇甲醚中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the alcohol ether solvent is selected from any one or two or more of triethylene glycol monobutyl ether, diethylene glycol monobutyl ether, and propylene glycol methyl ether in any proportion. mixture.
上述技术方案中，所述的C8-18的烷烃类溶剂，选自D60(埃克森美孚石油化工公司)、D80(埃克森美孚石油化工公司)、D100(埃克森美孚石油化工公司)、D110(埃克森美孚石油化工公司)、D130(埃克森美孚石油化工公司)、Isopar-E(埃克森美孚石油化工公司)、Isopar-G(埃克森美孚石油化工公司)、Isopar-H(埃克森美孚石油化工公司)、Isopar-L(埃克森美孚石油化工公司)、Isopar-M(埃克森美孚石油化工公司)、辛烷、壬烷、奎烷、十一碳烷、十二碳烷、十三碳烷、十四碳烷、十五碳烷、十六碳烷中的任意一种、两种及以上以任意比例混合而成的混合物。In the above technical solution, the C8-18 alkane solvent is selected from D60 (ExxonMobil Petrochemical Company), D80 (ExxonMobil Petrochemical Company), D100 (ExxonMobil Petrochemical Company) , D110 (ExxonMobil Petrochemical Company), D130 (ExxonMobil Petrochemical Company), Isopar-E (ExxonMobil Petrochemical Company), Isopar-G (ExxonMobil Petrochemical Company), Isopar -H (ExxonMobil Petrochemical Company), Isopar-L (ExxonMobil Petrochemical Company), Isopar-M (ExxonMobil Petrochemical Company), octane, nonane, quinane, undecane A mixture of any one, two or more of alkane, dodecane, tridecane, tetradecane, pentadecane and hexadecane in any proportion.
上述技术方案中，所述的C2-8的醇类溶剂，选自乙醇、异丙醇、正丙醇、正丁醇、仲丁醇、叔丁醇、正戊醇及其异构体、正己醇及其异构体、正庚醇及其异构体、正辛醇及其异构体中的任意一种、两种及以上以任意比例混合而成的混合物。In the above technical solution, the C2-8 alcohol solvent is selected from ethanol, isopropanol, n-propanol, n-butanol, sec-butanol, tert-butanol, n-amyl alcohol and its isomers, n-hexyl alcohol. A mixture of any one, two or more of alcohol and its isomers, n-heptanol and its isomers, n-octanol and its isomers in any proportion.
上述技术方案中，所述组分C，选自碳酸丙烯酯、碳酸丁烯酯、三辛酸甘油酯、山梨醇酐单油酸酯、脂肪醇与环氧乙烷缩合物、γ-丁内酯、乙烷基乙氧基酯、二丙二醇甲醚乙酸酯、式(II)所示化合物、式(III)所示化合物、式(IV)所示化合物的任意一种或两种及以上以任意比例混合而成的混合物；In the above technical solution, the component C is selected from the group consisting of propylene carbonate, butylene carbonate, tricaprylin, sorbitan monooleate, fatty alcohol and ethylene oxide condensate, γ-butyrolactone , any one or two or more of ethyl ethoxy ester, dipropylene glycol methyl ether acetate, the compound represented by formula (II), the compound represented by formula (III), the compound represented by formula (IV) A mixture of any proportions;
其中R1、R2和R3均为C1-C10的烷基。Wherein R 1 , R 2 and R 3 are all C1-C10 alkyl groups.
上述技术方案中，所述的其他助剂包括抗氧剂、防腐剂、抗紫外线剂中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the other auxiliaries include any one or a mixture of two or more of antioxidants, preservatives, and anti-UV agents in any proportion.
上述技术方案中，所述的抗氧剂选自2,6-二叔丁基-4-甲基苯酚、β-(3,5-二叔丁基-4-羟基苯基)丙酸异辛醇酯、丁基羟基茴香醚、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八醇酯中的任意一种、两种及以上以任意比例混合而成的混合物。In the above technical solution, the antioxidant is selected from 2,6-di-tert-butyl-4-methylphenol, β-(3,5-di-tert-butyl-4-hydroxyphenyl) isooctyl propionate Any one, two or more of alcohol ester, butyl hydroxyanisole, β-(3,5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate in any proportion. mixture.
上述技术方案中，所述的防腐剂选自苯甲酸钠、脱氢乙酸钠、山梨酸钾、尼铂金甲酯或卡松。In the above technical solution, the preservative is selected from sodium benzoate, sodium dehydroacetate, potassium sorbate, niplatin methyl ester or kason.
上述技术方案中，所述抗紫外线剂为2-羟基-4-正辛氧基二苯甲酮或3,5-二叔丁基-4-羟基苯甲酸正十六酯。In the above technical solution, the anti-ultraviolet agent is 2-hydroxy-4-n-octyloxybenzophenone or 3,5-di-tert-butyl-4-hydroxybenzoic acid n-hexadecyl ester.
本发明还提供一种所述的长效挥发电热蚊香液的制备方法，包括以下步骤：The invention also provides a method for preparing the long-lasting volatile electric heating mosquito repellent liquid, which includes the following steps:
将所述比例的组分A、B、C和其他助剂在室温(或加热至溶剂沸点以下)条件下混合至澄清，搅拌均匀后灌装至包装瓶中，插入引流挥发芯棒，旋紧外盖，即可制得成品。Mix components A, B, C and other additives in the stated proportions at room temperature (or heat to below the boiling point of the solvent) until clear, stir evenly and then fill into packaging bottles, insert the drainage volatilization mandrel, and tighten The outer cover is used to prepare the finished product.
与现有技术相比，本发明配制的电热蚊香液，可达到驱赶和杀死卫生害虫的目的，所述电热蚊香液通过液体蚊香加热器即可使得有效成分挥发至空间中，挥发时长最长可达960h。Compared with the existing technology, the electric mosquito-repellent liquid prepared in the present invention can achieve the purpose of driving away and killing sanitary pests. The electric-heated mosquito-repellent liquid can volatilize the active ingredients into the space through the liquid mosquito-repellent heater, and the volatilization time is the longest. Up to 960h.
具体实施方式Detailed ways
以下对本发明技术方案的具体实施方式详细描述，但本发明并不限于以下描述内容：Specific embodiments of the technical solution of the present invention are described in detail below, but the present invention is not limited to the following description:
本发明各实施例中电热蚊香液的制备方法如下：将所述比例的组分A、B、C和其他助剂在室温(或加热至溶剂沸点以下)混合至澄清，搅拌均匀后灌装至包装瓶中，插入引流挥发芯棒，旋紧外盖，即可制得成品。The preparation method of the electric mosquito-repellent liquid in each embodiment of the present invention is as follows: mix the components A, B, C and other auxiliaries in the stated proportions at room temperature (or heat to below the boiling point of the solvent) until clear, stir evenly and then fill to Insert the drainage volatilization mandrel into the packaging bottle, tighten the outer cap, and the finished product is ready.
下面结合具体的实施例，对本发明进行阐述：The present invention is described below in conjunction with specific examples:
制剂实施例1：0.4％2,3,4,5-四氟苄基-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 1: 0.4% 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester electric heating mosquito repellent liquid
0.4g2,3,4,5-四氟苄基-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯((1R，3S)、(1S，3R)、(1R，3R)、(1S，3S)四种异构体各占25％)，0.2g2,6-二叔丁基-4-甲基苯酚，0.3g2-羟基-4-正辛氧基二苯甲酮，5g三辛酸甘油酯，19.1g己二酸二异丙酯，40gD100，35gD110按上述方法制得电热蚊香液。0.4g 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate ((1R,3S ), (1S, 3R), (1R, 3R), (1S, 3S) four isomers account for 25% each), 0.2g 2,6-di-tert-butyl-4-methylphenol, 0.3g 2-hydroxy -4-n-octyloxybenzophenone, 5g tricaprylic acid glyceryl ester, 19.1g diisopropyl adipate, 40gD100, 35gD110 and prepare the electric mosquito-repellent liquid according to the above method.
制剂实施例2：0.6％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 2: 0.6% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
0.6g2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，5g三辛酸甘油酯，19.2g己二酸二异丙酯，40gD100，35gD110按上述方法制得电热蚊香液。0.6g 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 5g tricaprylin, 19.2g diisopropyl adipate, 40gD100, 35gD110 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例3：0.6％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 3: 0.6% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
0.6g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，5g三辛酸甘油酯,14.2g十四酸异丙酯，50gD100，30gD110按上述方法制得电热蚊香液。0.6g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 5g tricaprylin, 14.2g isopropyl myristate, 50gD100, 30gD110 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例4：0.75％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 4: 0.75% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
0.75g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.25g2,6-二叔丁基-4-甲基苯酚，5g碳酸丙烯酯，19g戊二酸二异丙酯，45gD100，30gD110按上述方法制得电热蚊香液。0.75g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.25g 2,6-di-tert-butyl-4-methylphenol, 5g propylene carbonate, 19g diisopropyl glutarate, 45gD100, 30gD110 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例5：0.9％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 5: 0.9% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
0.9g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，5g碳酸丙烯酯，23.9g十四酸异丙酯，34gD100，36gD110按上述方法制得电热蚊香液。0.9g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 5g propylene carbonate, 23.9g isopropyl myristate, 34gD100, 36gD110 to prepare electric mosquito-repellent liquid according to the above method.
制剂实施例6：1.2％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 6: 1.2% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
1.2g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，8g三辛酸甘油酯,20.6g戊二酸二异丙酯，32gD100，38gD110按上述方法制得电热蚊香液。1.2g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 8g tricaprylic acid glyceryl ester, 20.6g diisopropyl glutarate, 32gD100, 38gD110 were prepared according to the above method.
制剂实施例7：1.2％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 7: 1.2% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
1.2g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，5g乙烷基乙氧基酯，23.6g十四酸异丙酯，30gD100，40gD110按上述方法制得电热蚊香液。1.2g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 5g ethyl ethoxy ester, 23.6g isopropyl myristate, 30gD100, 40gD110 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例8：1.5％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 8: 1.5% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
1.5g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，8g碳酸丙烯酯，30.3g戊二酸二异丙酯，30gD110，30gD130按上述方法制得电热蚊香液。1.5g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 8g propylene carbonate, 30.3g diisopropyl glutarate, 30gD110, 30gD130 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例9：1.5％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 9: 1.5% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
1.5g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，8g乙烷基乙氧基酯，30.3g己二酸二异丙酯，40gD110，20gD130按上述方法制得电热蚊香液。1.5g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 8g ethyl ethoxy ester, 30.3g diisopropyl adipate, 40gD110, 20gD130 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例10：1.5％2,3,4,5-四氟苄基-3-[-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 10: 1.5% 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate electric mosquito coil liquid
1.5g2,3,4,5-四氟苄基-3-[-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，8g乙烷基乙氧基酯，30.3g己二酸二异丙酯，40gD110，20gD130按上述方法制得电热蚊香液。1.5g 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.2g 2,6-di-tert. Butyl-4-methylphenol, 8g ethyl ethoxy ester, 30.3g diisopropyl adipate, 40gD110, 20gD130 were used to prepare electric mosquito-repellent liquid according to the above method.
制剂实施例11：1.8％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 11: 1.8% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
1.8g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，6g式(II)所示化合物，32g己二酸二异丙酯，30gD110，30gD130按上述方法制得电热蚊香液。1.8g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 6g compound represented by formula (II), 32g diisopropyl adipate, 30gD110, 30gD130 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例12：1.8％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 12: 1.8% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
1.8g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，5g式(IV)所示化合物，32g己二酸二异丙酯，30gD110，31gD130按上述方法制得电热蚊香液。1.8g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 5g compound represented by formula (IV), 32g diisopropyl adipate, 30gD110, 31gD130 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例13：1.8％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 13: 1.8% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
1.8g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，5g式(IV)所示化合物，34g柠檬酸三丁酯，25gD110，34gD130按上述方法制得电热蚊香液。1.8g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 5g compound represented by formula (IV), 34g tributyl citrate, 25gD110, 34gD130 were used to prepare electric mosquito-repellent liquid according to the above method.
制剂实施例14：2.1％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 14: 2.1% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
2.1g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，6g式(IV)所示化合物，36.7g己二酸二异丙酯，25gD110，30gD130按上述方法制得电热蚊香液。2.1g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 6g compound represented by formula (IV), 36.7g diisopropyl adipate, 25gD110, 30gD130 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例15：2.1％2,3,4,5-四氟苄基-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 15: 2.1% 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester electric heating mosquito repellent liquid
2.1g2,3,4,5-四氟苄基-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯((1R，3S)、(1S，3R)、(1R，3R)、(1S，3S)四种异构体各占25％)，0.2g2,6-二叔丁基-4-甲基苯酚，6g式(IV)所示化合物，36.7g己二酸二异丙酯，22gD110，33gD130按上述方法制得电热蚊香液。2.1g 2,3,4,5-Tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate ((1R,3S ), (1S, 3R), (1R, 3R), (1S, 3S) four isomers each accounting for 25%), 0.2g 2,6-di-tert-butyl-4-methylphenol, 6g formula (IV ), 36.7g diisopropyl adipate, 22gD110, 33gD130 were used to prepare the electric mosquito-repellent liquid according to the above method.
制剂实施例16：2.4％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 16: 2.4% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
2.4g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，0.4g2-羟基-4-正辛氧基二苯甲酮，32g戊二酸二异丙酯，15g山梨醇酐单油酸酯，20gD110，30gD130按上述方法制得电热蚊香液2.4g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 0.4g 2-hydroxy-4-n-octyloxybenzophenone, 32g diisopropyl glutarate, 15g sorbitan monooleic acid Ester, 20gD110, 30gD130, prepare electric mosquito-repellent liquid according to the above method
制剂实施例17：2.7％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 17: 2.7% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
2.7g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，8g三辛酸甘油酯，34.1g己二酸二异丙酯，22gD110，33gD130按上述方法制得电热蚊香液。2.7g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, 0.2g 2,6-di-tert-butyl-4-methylphenol, 8g tricaprylin, 34.1g diisopropyl adipate, 22gD110, 33gD130 and prepare electric mosquito-repellent liquid according to the above method.
制剂实施例18：3％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 18: 3% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
3g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，0.4g2-羟基-4-正辛氧基二苯甲酮，8g三辛酸甘油酯，38.4g十四酸异丙酯，11gD110，39gD130按上述方法制得电热蚊香液。3g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate , 0.2g 2,6-di-tert-butyl-4-methylphenol, 0.4g 2-hydroxy-4-n-octoxybenzophenone, 8g tricaprylin, 38.4g isopropyl myristate, 11gD110, 39gD130 is used to prepare electric mosquito-repellent liquid according to the above method.
制剂实施例19：3％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 19: 3% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
3g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，0.4g2-羟基-4-正辛氧基二苯甲酮，37.4g己二酸二异丙酯，9g碳酸丙烯酯，12gD110，38gD130按上述方法制得电热蚊香液。3g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate , 0.2g 2,6-di-tert-butyl-4-methylphenol, 0.4g 2-hydroxy-4-n-octyloxybenzophenone, 37.4g diisopropyl adipate, 9g propylene carbonate, 12gD110, 38gD130 is used to prepare electric mosquito-repellent liquid according to the above method.
制剂实施例20：3％2,3,4,5-四氟苄基-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Formulation Example 20: 3% 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester electric heating mosquito repellent liquid
3g2,3,4,5-四氟苄基-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯((1R，3S)、(1S，3R)、(1R，3R)、(1S，3S)四种异构体各占25％)，0.2g2,6-二叔丁基-4-甲基苯酚，0.4g2-羟基-4-正辛氧基二苯甲酮，37.4g己二酸二异丙酯，7g式(IV)所示化合物，12gD110，40gD130按上述方法制得电热蚊香液。3g 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate ((1R, 3S) , (1S, 3R), (1R, 3R), (1S, 3S) four isomers each accounting for 25%), 0.2g2,6-di-tert-butyl-4-methylphenol, 0.4g2-hydroxy- 4-n-octyloxybenzophenone, 37.4g diisopropyl adipate, 7g compound represented by formula (IV), 12gD110, 40gD130 were used to prepare the electric mosquito-repellent liquid according to the above method.
对比实施例1:0.62％四氟甲醚电热蚊香液Comparative Example 1: 0.62% Tetrafluoromethyl Ether Electric Mosquito Repellent Liquid
0.62g四氟甲醚，0.2g2,6-二叔丁基-4-甲基苯酚，0.4g2-羟基-4-正辛氧基二苯甲酮，55.78gD80，43gD100。0.62g tetrafluoromethyl ether, 0.2g 2,6-di-tert-butyl-4-methylphenol, 0.4g 2-hydroxy-4-n-octyloxybenzophenone, 55.78gD80, 43gD100.
对比实施例2：3％2,3,4,5-四氟苄基-(1R，3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯电热蚊香液Comparative Example 2: 3% 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethyl cyclopropylcarboxylate electric mosquito repellent liquid
3g2,3,4,5-四氟苄基-(1R，3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯，0.2g2,6-二叔丁基-4-甲基苯酚，0.4g2-羟基-4-正辛氧基二苯甲酮，40.4g己二酸二异丙酯，16gD110，40gD130按上述方法制得电热蚊香液。3g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate , 0.2g 2,6-di-tert-butyl-4-methylphenol, 0.4g 2-hydroxy-4-n-octyloxybenzophenone, 40.4g diisopropyl adipate, 16gD110, 40gD130 prepared according to the above method Get electric mosquito repellent liquid.
测试实施例1：Test Example 1:
试验方法：参照《GB/T 13917.6-2009农药登记用卫生杀虫剂室内药效试验及评价第6部分：电热蚊香液》分别在点样240h、480h、720h和960h进行药效测试。采用圆筒装置：每次试验吸取试蚊30只，由圆板(F)的中央圆孔处放入，塞紧胶塞(H)。待试虫恢复正常活动后，将连续通电至相应的时段点载有待测电热蚊香液的加热器放置在圆板(F)的中央空下方，靠紧中央孔，熏杀1min，立即塞上胶塞(H)，并计时，每隔一定的时间记录被击倒的试虫数。观察时间为20min。测试应三次及以上重复。每次试验结束，应清洗试验装置。试验结果如表1所示。Test method: Refer to "GB/T 13917.6-2009 Indoor Efficacy Test and Evaluation of Hygienic Insecticides for Pesticide Registration Part 6: Electric Mosquito Repellent Liquid" to conduct efficacy tests at 240h, 480h, 720h and 960h respectively. Using a cylindrical device: 30 test mosquitoes are sucked out for each test, put into the central round hole of the circular plate (F), and tightly plugged with the rubber stopper (H). After the test insects resume normal activities, continuously energize the heater until the corresponding time period and place the heater containing the electric mosquito-repellent liquid to be tested under the central hole of the circular plate (F), close to the central hole, fumigate for 1 minute, and plug it immediately. Rubber stopper (H), and timer, record the number of test insects knocked down at certain intervals. The observation time is 20min. The test should be repeated three or more times. After each test, the test device should be cleaned. The test results are shown in Table 1.
表1不同样品电热蚊香液圆筒药效试验结果Table 1 Efficacy test results of different samples of electric mosquito repellent liquid cylinders
测试结果显示，添加组分C后可确保高含量电热蚊香液仍可持续均匀挥发，药效在整体时长中更稳定，不会影响点样后期药效。Test results show that adding component C can ensure that the high-content electric mosquito-repellent liquid can continue to volatilize evenly, and the efficacy is more stable over the entire duration, without affecting the efficacy in the later stages of spotting.
测试实施例2：Test Example 2:
将制剂实施例4、制剂实施例8、制剂实施例18，按照测试实施例1的方法进行测试，结果如表2所示。Preparation Example 4, Preparation Example 8, and Preparation Example 18 were tested according to the method of Test Example 1, and the results are shown in Table 2.
表2不同样品电热蚊香液圆筒药效试验结果Table 2 Efficacy test results of different samples of electric mosquito repellent liquid cylinders
测试结果显示，采用不同本发明的组分B组合可以控制药液挥发时间，从而可以配制不同时长的样品。The test results show that the volatilization time of the medicinal solution can be controlled by using different combinations of component B of the present invention, so that samples of different durations can be prepared.
测试实施例3：Test Example 3:
参考GB/T 13917.10-2009，使用模拟房在倒数第二时间点进行药效测试，并按照标准进行评价，评价标准是1小时淡色库蚊击倒率≥90％的为A级活性，击倒率≥70％为B级活性，测试结果如表3所示。Refer to GB/T 13917.10-2009, use a simulation room to conduct efficacy tests at the penultimate time point, and evaluate according to the standard. The evaluation standard is that the knockdown rate of Culex pipiens in 1 hour is ≥90%, which is Class A activity. Rate ≥70% is Class B activity, and the test results are shown in Table 3.
表3不同样品电热蚊香液模拟房药效试验结果Table 3 The efficacy test results of different samples of electric mosquito repellent liquid simulation room
上述实例只是为说明本发明的技术构思以及技术特点，并不能以此限制本发明的保护范围。凡根据本发明的实质所做的等效变换或修饰，都应该涵盖在本发明的保护范围之内。The above examples are only for illustrating the technical concept and technical features of the present invention, and are not intended to limit the scope of the present invention. All equivalent transformations or modifications made based on the essence of the present invention should be included in the protection scope of the present invention.
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