CN107417640B - The preparation method of nanometer zinc thiazole - Google Patents
The preparation method of nanometer zinc thiazole Download PDFInfo
- Publication number
- CN107417640B CN107417640B CN201710215759.5A CN201710215759A CN107417640B CN 107417640 B CN107417640 B CN 107417640B CN 201710215759 A CN201710215759 A CN 201710215759A CN 107417640 B CN107417640 B CN 107417640B
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- China
- Prior art keywords
- sodium
- zinc
- salt
- thiazole
- zinc thiazole
- Prior art date
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- FXVNBZGTAWLLNE-UHFFFAOYSA-N 1,3-thiazole;zinc Chemical compound [Zn].C1=CSC=N1 FXVNBZGTAWLLNE-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 239000003814 drug Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 150000003751 zinc Chemical class 0.000 claims abstract description 13
- 239000012266 salt solution Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 33
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 14
- -1 alcohol fatty acid ester Chemical class 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 12
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 159000000000 sodium salts Chemical class 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical group [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 6
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 5
- 235000005074 zinc chloride Nutrition 0.000 claims description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- 229920001400 block copolymer Polymers 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 239000003995 emulsifying agent Substances 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- JSYPRLVDJYQMAI-ODZAUARKSA-N (z)-but-2-enedioic acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)\C=C/C(O)=O JSYPRLVDJYQMAI-ODZAUARKSA-N 0.000 claims description 2
- 229920002126 Acrylic acid copolymer Polymers 0.000 claims description 2
- 229920005682 EO-PO block copolymer Polymers 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 claims description 2
- 229920000136 polysorbate Polymers 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- YEDTWOLJNQYBPU-UHFFFAOYSA-N [Na].[Na].[Na] Chemical compound [Na].[Na].[Na] YEDTWOLJNQYBPU-UHFFFAOYSA-N 0.000 claims 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims 4
- 229910019142 PO4 Inorganic materials 0.000 claims 2
- 239000000654 additive Substances 0.000 claims 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 2
- 239000010452 phosphate Substances 0.000 claims 2
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 claims 2
- 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 claims 1
- 241000047703 Nonion Species 0.000 claims 1
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 1
- WWBXZKQQXUFSED-UHFFFAOYSA-N [Na].O=C.C1=CC=C2C(S(=O)(=O)OC)=CC=CC2=C1 Chemical compound [Na].O=C.C1=CC=C2C(S(=O)(=O)OC)=CC=CC2=C1 WWBXZKQQXUFSED-UHFFFAOYSA-N 0.000 claims 1
- 125000000217 alkyl group Chemical group 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- RRTCFFFUTAGOSG-UHFFFAOYSA-N benzene;phenol Chemical compound C1=CC=CC=C1.OC1=CC=CC=C1 RRTCFFFUTAGOSG-UHFFFAOYSA-N 0.000 claims 1
- LLEMOWNGBBNAJR-UHFFFAOYSA-N biphenyl-2-ol Chemical compound OC1=CC=CC=C1C1=CC=CC=C1 LLEMOWNGBBNAJR-UHFFFAOYSA-N 0.000 claims 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims 1
- 150000001734 carboxylic acid salts Chemical class 0.000 claims 1
- PKJZYOFPPJHDRW-UHFFFAOYSA-N formaldehyde;sulfuric acid Chemical compound O=C.OS(O)(=O)=O PKJZYOFPPJHDRW-UHFFFAOYSA-N 0.000 claims 1
- 239000002563 ionic surfactant Substances 0.000 claims 1
- 229920000058 polyacrylate Polymers 0.000 claims 1
- 229920000642 polymer Polymers 0.000 claims 1
- 239000011736 potassium bicarbonate Substances 0.000 claims 1
- 235000015497 potassium bicarbonate Nutrition 0.000 claims 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims 1
- 235000011181 potassium carbonates Nutrition 0.000 claims 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims 1
- 235000011118 potassium hydroxide Nutrition 0.000 claims 1
- 239000002002 slurry Substances 0.000 claims 1
- 235000011121 sodium hydroxide Nutrition 0.000 claims 1
- RCIJACVHOIKRAP-UHFFFAOYSA-M sodium;1,4-dioctoxy-1,4-dioxobutane-2-sulfonate Chemical compound [Na+].CCCCCCCCOC(=O)CC(S([O-])(=O)=O)C(=O)OCCCCCCCC RCIJACVHOIKRAP-UHFFFAOYSA-M 0.000 claims 1
- 239000000600 sorbitol Substances 0.000 claims 1
- 150000004867 thiadiazoles Chemical class 0.000 abstract description 28
- 238000009938 salting Methods 0.000 abstract description 8
- 238000001035 drying Methods 0.000 abstract description 2
- 239000000575 pesticide Substances 0.000 description 18
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
- 239000007859 condensation product Substances 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 9
- 241000894006 Bacteria Species 0.000 description 6
- 239000004721 Polyphenylene oxide Substances 0.000 description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 6
- 230000001580 bacterial effect Effects 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229920000570 polyether Polymers 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 240000007594 Oryza sativa Species 0.000 description 5
- 235000007164 Oryza sativa Nutrition 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012875 nonionic emulsifier Substances 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000003090 pesticide formulation Substances 0.000 description 1
- 230000003285 pharmacodynamic effect Effects 0.000 description 1
- 229940044654 phenolsulfonic acid Drugs 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- WQQPDTLGLVLNOH-UHFFFAOYSA-M sodium;4-hydroxy-4-oxo-3-sulfobutanoate Chemical compound [Na+].OC(=O)CC(C([O-])=O)S(O)(=O)=O WQQPDTLGLVLNOH-UHFFFAOYSA-M 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000009469 supplementation Effects 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
-
- 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/18—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, directly attached to a heterocyclic or cycloaliphatic ring
-
- 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D285/00—Heterocyclic compounds containing rings having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by groups C07D275/00 - C07D283/00
- C07D285/01—Five-membered rings
- C07D285/02—Thiadiazoles; Hydrogenated thiadiazoles
- C07D285/04—Thiadiazoles; Hydrogenated thiadiazoles not condensed with other rings
- C07D285/12—1,3,4-Thiadiazoles; Hydrogenated 1,3,4-thiadiazoles
- C07D285/125—1,3,4-Thiadiazoles; Hydrogenated 1,3,4-thiadiazoles with oxygen, sulfur or nitrogen atoms, directly attached to ring carbon atoms, the nitrogen atoms not forming part of a nitro radical
- C07D285/135—Nitrogen atoms
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of preparation methods of nanoscale zinc thiazole, comprising the following steps: 1), intermediate thiadiazoles salt synthesis: thiadiazoles mixes in a solvent with alkali, is prepared into thiadiazoles salting liquid；2), nanometer zinc thiazole raw medicine synthesizes: a kind of optionally following mode, it is mode one, zinc salt and auxiliary agent is soluble in water, the resulting thiadiazoles salting liquid of step 1) is then added, uniform stirring is until form suspension, it is dry after suspension is separated, obtain powdered zinc thiazole；Auxiliary agent is added in the resulting thiadiazoles salting liquid of step 1) in mode two, and zinc salt solution is then added, and uniform stirring is until form suspension, and drying, obtains powdered zinc thiazole after suspension is separated.
Description
Technical field
The present invention relates to a kind of preparation methods of novel fungicide-nanoscale zinc thiazole.
Background technique
China is the big country of the production estimations such as rice, fruit tree and vegetables, and the bacterial disease type of crop is more, harm is tight
Weight, bacterial blight of rice, bacterial leaf streak of rice, vegetative bacteria bacterial wilt, vegetative bacteria black rot, c itrus canker
The important crops bacteriosises such as disease, melon bacterial angular leaf spot are persistently caused disaster.
Therefore, it is badly in need of increasing the R&D intensity of bactericide, discovery and invention mechanism of action are novel as early as possible, pacify crop
Entirely, the high novel bactericide of bioactivity.
Zinc thiazole is efficient, less toxic, safety the disinfectant use in agriculture of a new generation for preventing and treating bacterial diseases of crops.
Zinc thiazole chemical name are as follows: bis- (2- amino -5- sulfydryl -1,3,4- thiadiazoles) zinc, english common name are as follows: Zn
thiazole.Structural formula is as follows:
Raw medicine is white powder, and sterling is white crystals, specific gravity: 1.94, fusing point > 300 DEG C；It is not soluble in water and organic molten
Agent.Active height, wide sterilization spectrum, to crop safety the features such as, the prevention and treatments of the bacterial diseases such as rice, citrus, vegetables is imitated
Fruit is prominent.Pharmacodynamic test extensively and profoundly the study found that zinc thiazole to crop soft rot, bacterial angular leaf spot, canker, bacterium
The chief crops bacterial diseases such as property cecospora spot, bacterial wilt, Bacterial septicaemia syndrome, wildfire, leaf blight, brown rot and heartrot
All have excellent preventive and therapeutic effect, zinc thiazole can prevent and treat rice, citrus, peach, jujube tree, cucumber, tomato, Chinese cabbage, garlic,
The rop bacterium venereal disease evils such as taro and tobacco, and have the function of certain to promote plant growth；It can compound containing thiophene
The serial bactericidal composition and its application technology of azoles zinc.
The domestic existing resulting zinc thiazole product cut size of production technology is in 50um or so, and domestic sales volume is larger, various compoundings
Preparation is also very much.Because raw medicine is organic metal chelate complex type, all it is difficult to dissolve in water and common organic solvents, limits
Its drug effect plays.Therefore preparation processing enterprise is usually used corase grinding, sand milling, shears again, is made into suspending agent, partial size is in 2-5 μ
Between m, but it is still relatively thick, its field efficacy is not only influenced, and machining cost is big, time-consuming, raw medicine effective rate of utilization
It is not high.
Nanotechnology refers to the technology that substance and material are processed and handled on nanoscale.Due to nano material
Size between single atom or molecule and corresponding conventional size material, the original physicochemical properties of material can be sent out
Changing shows the physicochemical properties different from stock size material, i.e. nano effect.
The validity and safety for improving traditional formulations of pesticide function using nanotechnology or nano material, improving pesticide
Property, break through and restrict the theoretical bottleneck problem with method development of formulations of pesticide initiative, disclosing nanometer material and technology improves pesticide agent
The mechanism of action of type function, the novel nano pesticide of development efficiently, safe and inexpensive are current domestic and international research hotspots.
The application of nano pesticide is a kind of raising pesticide dispersion and wettable, reinforces a kind of new skill of its controlled release fertilizer
Art, nano pesticide have the advantages that
1) extending lasting period nano level pesticide as sustained release agent can reduce light in environment, empty gas and water and microorganism to work
Property ingredient decomposition, and can be achieved the purpose that by the difference of its releasing mechanism control release or slow release, make its tool
There is apparent sustained release performance, can greatly extend the release time of active constituent, extends the lasting period.
2) by high-toxic pesticide low toxicity, reduce to some nano pesticide microballoons of the toxicity of non-target mark biology, activity at
Subpackage is rolled in softgel shell, realizes its slow release in use, avoids many pesticides to people and animals or bee, bird, fish, silkworm high poison,
It is easy to cause damages to non-target organism around when in use.To greatly reduce its toxicity.
3) it improves to target deposition nano pesticide microballoon, exists in the form of viscous gum, target will be easily adhered to
Site surface deposition is marked, or enhances its efficiency for penetrating into target, to increase drug effect, reduces the loss of effective component.
4) some nano pesticide microballoons of the waste of reduction drug wrap effective component with high molecular material, make
Pesticide active ingredient can be completely cut off with ambient enviroment, avoid the rings such as photodissociation, hydrolysis, volatilization, leaching and microbial degradation
Border factor, then can effectively improve the stability of pesticide active ingredient, to increase its lasting period, reduce the waste of pesticide.
Domestic nano-pesticide formulation is much with nano material, for example nano-titanium dioxide, more sky nano silicas, receives
Rice molecular sieve etc. nano materials carry out physical absorption, pesticide original medicine and nano material progress physical absorption, are then dispersed in
In water, the thinner dispersion liquid of particle is formed, for controlling release, raising drug effect etc..
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation methods of the nanoscale zinc thiazole of good dispersion degree.
In order to solve the above technical problem, the present invention provides a kind of preparation methods of nanoscale zinc thiazole, including following step
It is rapid:
1), intermediate thiadiazoles salt synthesizes:
Thiadiazoles mixes in a solvent with alkali, and being prepared into thiadiazoles salting liquid, (thiadiazoles salting liquid is that clear homogeneous is water-soluble
Liquid), the solid-liquid ratio of thiadiazoles and solvent is 10g:30~100ml, and the molar ratio of thiadiazoles and alkali is 1:1；
Remarks explanation: after thiadiazoles mixes in a solvent with alkali, system is in muddy shape, and temperature rising reflux to system is become by muddiness
For clear homogeneous aqueous solution, return time is generally 2h or so；
2), nanometer zinc thiazole raw medicine synthesizes:
A kind of optionally following mode:
Mode one,
Zinc salt and auxiliary agent is soluble in water, the resulting thiadiazoles salting liquid of step 1) is then added, uniform stirring is until shape
It is dry after suspension is separated at suspension, obtain powdered zinc thiazole (thin white, partial size is at 1-1000 nanometers)；
Remarks explanation: the anti-of thiadiazoles salting liquid progress is added in zinc salt and auxiliary agent formation colourless transparent liquid soluble in water
It should be homogeneous reaction, slowly generate solid, reaction solution is from the transparent suspension for becoming milky or milk yellow；
Mode two,
Auxiliary agent is added in the resulting thiadiazoles salting liquid of step 1), is then added zinc salt solution, uniform stirring until
Suspension is formed, it is dry after suspension is separated, obtain powdered zinc thiazole (thin white, partial size are 1-1000 nanometers)；
In aforesaid way one and mode two, the molar ratio of thiadiazoles and zinc salt is 1:1:0.5；The weight of auxiliary agent and thiadiazoles
Than for 0.01~50% (preferably 0.5%~10%).
Remarks: the mixing time of aforesaid way one and mode two generally requires 20min or more.In mode one dosage of water or
The dosage of water is 0.8~1.2 times of solvent volume amount in step 1) in zinc salt solution in person's mode two.
The improvement of preparation method as nanoscale zinc thiazole of the invention, in step 1):
Alkali is (the preferably hydrogen-oxygens such as sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, saleratus, ammonium hydroxide
Change sodium, potassium hydroxide)；
Solvent is the mixture of the alcohol of C1-4, water (preferably), C1-4 alcohol and water, and the volume of C1-4 alcohol is dense in the mixture
Degree is 10%~90%.
The further improvement of preparation method as nanoscale zinc thiazole of the invention, in step 2): zinc salt be zinc sulfate,
Zinc acetate, zinc chloride, zinc nitrate etc. (preferably sulfuric acid zinc).
The further improvement of preparation method as nanoscale zinc thiazole of the invention, in step 2):
Auxiliary agent be it is following any one: non-ionic dispersing agent, anionic dispersing agents, amphoteric ion dispersing agent, have dispersion
The emulsifier (including nonionic emulsifier, anion emulsifier etc.) of effect；Or other single auxiliary agents with peptizaiton
Or compound auxiliary.
The further improvement of preparation method as nanoscale zinc thiazole of the invention, auxiliary agent be it is following any one:
APES formaldehyde condensation product class dispersing agent；
Polyethenoxy ether class；
Phenethyl phenol polyethenoxy ether condensation product, APES formaldehyde condensation product, naphthalene sulfonic acid-formaldehyde condensation product,
Methyl naphthalene sulfonate formaldehyde condensate；
Block copolymerization species；
Span and its polyethenoxy ether class；
Anionic surfactant.
The further improvement of preparation method as nanoscale zinc thiazole of the invention,
The APES formaldehyde condensation product class dispersing agent includes Nongru-700 number；
Polyethenoxy ether class includes alkyl phenol polyoxyethylene ether (preferably octyl phenol polyoxyethylene ether, Nonyl pheno
Ether), fatty alcohol polyethenoxy ether class；
Block copolymerization species include ethylene oxide propylene oxide block copolymer (EO/PO/EO block polyether), propylene oxide
Epoxyethane block copolymer (PO/EO/PO block polyether)；
The Span and its polyethenoxy ether class include Span series, TWEEN Series；
The anionic surfactant is alkyl phenol polyoxyethylene ether phosphoric acid ester, fatty alcohol polyoxyethylene ether phosphoric acid
Esters, sulfite cellulose solid dry substance, sodium lignin sulfonate, alkylphenol formaldehyde condensate sulfate, di-2-ethylhexylphosphine oxide naphthalene sulfonic acids
Sodium, to methoxyl group fatty acid amide benzene sulfonic acid sodium salt, polycarboxylate surfactant, APES formaldehyde condensation product sulfuric acid
Salt；Phenethyl phenol polyethenoxy ether sodium sulphate, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, sodium alkyl benzene sulfonate (dodecyl benzene sulfonic acid
Sodium), it is phenolsulfonic acid condensation product sodium salt, sodium metnylene bis-naphthalene sulfonate, acrylate homopolymer sodium salt, polymeric polycarboxylic acid salt, two pungent
One such or several composition such as base sulfosuccinic acid sodium salt, maleic acid-acrylic acid copolymer sodium salt, sodium alkyl sulfate.
The present invention is passed through using the method for chemistry from the key intermediate thiadiazoles salt and zinc salt of zinc thiazole synthesis
The change and optimization of synthesis technologic parameter, are added suitable auxiliary agent in committed step, and nanoscale zinc thiazole raw medicine is made.
This nanometer of zinc thiazole can be directly diluted with water, and form uniform milk-white coloured suspension, improve the dispersion degree of raw medicine, be reduced processed
The mechanically actuateds such as grinding, crushing in journey have saving of work and time, improve the effect of drug effect, have in usage economy, the feature of environmental protection
It is broken through.
The nanometer zinc thiazole good dispersion degree being prepared using the method for the present invention is milky milk after being directly diluted with water
Shape stablizes liquid or faint yellow emulsion, and stability is good, places 5-7 days and does not settle, and raw medicine is commercialized and directly adds after water then
Bottom is sunk at once.
Resulting nanometer zinc thiazole is prepared using the method for the present invention, can directly be sprayed on crops prevention and treatment plant pathogenetic bacteria
And fungi, and with the stronger purposes for promoting plant growth.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 is the grain size distribution (average grain diameter 4.721nm) of nanometer zinc thiazole；
Fig. 2 is nanometer zinc thiazole scanning electron microscope (SEM) photograph (SEM)；
Fig. 3 is nanometer zinc thiazole transmission electron microscope picture TEM；
Fig. 4 is the nanometer zinc thiazole XRD spectrum of synthesis；
The commercialization zinc thiazole raw medicine XRD spectrum of Fig. 5 buying；
Fig. 6 thiazole high-efficient liquid phase chromatogram spectrum, A, 98% zinc thiazole raw medicine B, nanometer zinc thiazole；
Fig. 7 nanometer raw medicine is followed successively by 10 with the dispersion degree after raw medicine is diluted with water, raw medicine concentration is commercialized from left to right,
5.0,1.0,0.5,0.1mg/ml),
A is nanometer zinc thiazole raw medicine, and raw medicine (bottom is directly deposited in water) is commercialized in B routine zinc thiazole.
Specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited in
This:
Embodiment 1, nanometer zinc thiazole are synthetically prepared:
1), intermediate thiadiazoles salt synthesizes
It weighs sodium hydroxide 3g (75mmol) to be added in 100ml water, thiadiazoles 10g is added to being completely dissolved in stirring
(75mmol), stirs evenly, the white muddy shape of system, and it is transparent that temperature rising reflux to system from white opacity becomes claret, returns
2h cooled to room temperature is flowed, thiadiazoles sodium salt solution is obtained, it is spare.
2), nanometer zinc thiazole raw medicine synthesizes
10.78g (37.5mmol) white vitriol is dissolved in 100ml water at room temperature, the dispersing agent NNO of 50mg is added
(sodium methylene bis-naphthalene sulfonate), stirring, is slowly added into above-mentioned steps 1) resulting thiadiazoles sodium salt solution, is stirred at room temperature
20min obtains white " milky " liquid.By the white " milky " liquid, 10~20min is centrifuged with 10000r/min, makes to be washed with deionized water
Wash precipitating twice (each dosage is about 50ml), precipitating is nanometer zinc thiazole, and vacuum decompression is dry (- 0.097MPa, 60 DEG C)
To constant weight to get arrive white nanoscale thiazole zinc powder 11.7g (yield 95%).The content 96% of gained nanometer zinc thiazole
(HPLC)。
Structural characterization:
The nanometer zinc thiazole 1mg prepared in embodiment 1 is weighed, is added in 2ml deionized water, is stirred evenly, obtain nanometer
Zinc thiazole emulsion takes out 1ml using Malvern particle size analyzer measurement zinc thiazole emulsion granularity between 4-5nm, average
Partial size is 4.721nm, and particle diameter distribution is uniform.It is analyzed by scanning electron microscope (SEM) and transmission electron microscope (TEM), solid nano thiazole
Zinc fraction is stablized, and particle size range is in 50-100nm or so.XRD diffraction analysis is finally done, by comparison nanometer zinc thiazole and often
The spectrogram of zinc thiazole raw medicine is advised, wherein characteristic peak corresponds, the nanometer zinc thiazole and commercialization thiophene that display the present embodiment 1 synthesizes
Azoles zinc raw medicine is consistent, illustrates that the two is same substance.
NNO (sodium methylene bis-naphthalene sulfonate) in embodiment 1 is changed to the contracting of dispersing agent naphthalenesulfonateformaldehyde formaldehyde by embodiment 2 respectively
Object sodium salt, EO/PO/EO block polyether, PO/EO/PO block polyether, sodium lignin sulfonate, alkylphenol formaldehyde condensation product sulfuric acid are closed,
Weight is constant；Remaining is equal to embodiment 1.
Acquired results are described in table 1 below.
Table 1
| The content of nanometer zinc thiazole | Nanometer zinc thiazole particle diameter distribution | |
| Naphthalene sulfonic acid-formaldehyde condensation product sodium salt | 96% | 50-200nm |
| EO/PO/EO block polyether | 95.8% | 50-200nm |
| PO/EO/PO block polyether | 95.6% | 50-200nm |
| Sodium lignin sulfonate | 95% | 50-200nm |
| Alkylphenol formaldehyde condensation product sulfuric acid | 94% | 50-500nm |
Embodiment 3, nanometer zinc thiazole are synthetically prepared:
1), intermediate thiadiazoles salt synthesizes
Weigh potassium hydroxide 4.2g (75mmol), be added in the ethanol water of 50ml 60% (V/V), stirring to being completely dissolved,
It is added thiadiazoles 10g (75mmol), stirs evenly, the white muddy shape of system, temperature rising reflux 2h to system is become by white opacity
To be transparent, cooled to room temperature is to get spare to thiadiazoles potassium salt soln.
2), nanometer zinc thiazole raw medicine synthesizes
10.78g (37.5mmol) white vitriol is added the Nongru-700 number of 500mg, stirred in 50ml water at room temperature
Mix, be slowly added into above-mentioned steps 1) resulting thiadiazoles potassium salt soln, stirs 20min at room temperature, obtains white " milky " liquid.It should
White " milky " liquid, 1000r/min are centrifuged 10~20min, washing, vacuum decompression it is dry to constant weight to get to white nanoscale thiophene
Azoles zinc powder 9.98g (yield 81%).
The content 95.3% of gained nanometer zinc thiazole.It is measured using Malvern particle size analyzer, gained nanometer thiazole zinc granule
Diameter is distributed as between 20-300nm.
Embodiment 4, nanometer zinc thiazole are synthetically prepared:
1), intermediate thiadiazoles salt synthesizes
Weigh potassium hydroxide 4.2g (75mmol), be added 30ml 50% isopropanol water in, heating stirring to completely it is molten
Solution is added thiadiazoles 10g (75mmol), stirring be warming up to it is complete it is molten after, be cooled to room temperature to get to thiadiazoles potassium salt soln；
2), nanometer zinc thiazole raw medicine synthesizes
The neopelex of 1g is added in the resulting thiadiazoles potassium salt soln of step 1), cooled to room temperature,
It is spare.
5.2g (37.5mmol) zinc chloride is dissolved in 25ml water at room temperature, above-mentioned stock solution is added slowly under stirring
In, 20min is stirred at room temperature, obtains white " milky " liquid.By the white " milky " liquid, 1000r/min is centrifuged 10~20min, wash,
White nanoscale thiazole zinc powder 10.2g is arrived in vacuum decompression drying to constant weight.
The content 97.2% of gained nanometer zinc thiazole.It is measured using Malvern particle size analyzer, gained nanometer thiazole zinc granule
Diameter is distributed between 300-900nm.
" water " in 1 step 1) of embodiment is changed to that " methanol ", " ethyl alcohol ", " 50% methanol is water-soluble by embodiment 5 respectively
Liquid ", " 50% ethanol water ", volume is constant, is still 100ml；Remaining is equal to embodiment 1.Acquired results such as the following table 2 institute
It states.
Table 2
| Reaction yield | The content of nanometer zinc thiazole | Nanometer zinc thiazole particle diameter distribution | |
| Water | 95% | 96% | 50-100nm |
| Methanol | 46% | 75% | 1000-2000nm |
| Ethyl alcohol | 44% | 68% | 1000-2000nm |
| 50% methanol aqueous solution | 71% | 87% | 400-1000nm |
| 50% ethanol water | 75% | 79% | 300-1000nm |
" sodium hydroxide " in 1 step 1) of embodiment is changed to " sodium carbonate ", " sodium bicarbonate ", " ammonia by embodiment 6 respectively
Water ", mole are constant, are still 75mmol；Remaining is equal to embodiment 1.Acquired results are described in table 3 below.
Table 3
| The content of nanometer zinc thiazole | Nanometer zinc thiazole particle diameter distribution | |
| Sodium hydroxide | 96% | 50-100nm |
| Sodium carbonate | 30% | > 50um |
| Sodium bicarbonate | 30% | > 50um |
| Ammonium hydroxide | 10% | > 50um |
" zinc sulfate " in 1 step 1) of embodiment is changed to " zinc acetate ", " zinc chloride ", " nitric acid by embodiment 7 respectively
Zinc ", mole are constant, are still 37.5mmol；Remaining is equal to embodiment 1.Acquired results are described in table 4 below.
Table 4
| The content of nanometer zinc thiazole | Nanometer zinc thiazole particle diameter distribution | |
| Zinc sulfate | 96% | 50-100nm |
| Zinc acetate | 89% | 200-500nm |
| Zinc chloride | 93% | 100-200nm |
| Zinc nitrate | 94% | 100-200nm |
Experiment one: nanometer zinc thiazole content analysis
Zinc thiazole standard specimen 0.02g (being accurate to 0.0002g) is weighed in 100mL cleaning, dry volumetric flask, with acetonitrile+
Water+trifluoroacetic acidScale is dissolved and be diluted to, surpasses 5min with ultrasonic wave, shakes up.It is cooled to room temperature to solution, uses
Pipette accurately pipettes the 5.0mL prepared solution and cleans in another 50mL, in dry volumetric flask, with acetonitrile+water+trifluoro
Acetic acidScale is dissolved and be diluted to, is shaken up.
Weigh about 0.02g preparation nanometer zinc thiazole (being accurate to 0.0002g) as sample in 100mL cleaning, dry
In volumetric flask, with acetonitrile+water+trifluoroacetic acidScale is dissolved and is diluted to, surpasses 5min with ultrasonic wave, shakes up,
It stands, is cooled to room temperature to solution, the supernatant liquor 5.0mL that the solution is accurately pipetted with pipette is cleaned in another 50mL, is dry
Volumetric flask in, with acetonitrile+water+trifluoroacetic acidScale is dissolved and be diluted to, is shaken up.
Under the operating conditions described above, after instrumental baseline is stablized, several needle standard specimen solutions is continuously injected into, each needle zinc thiazole is calculated
The repeatability of the ratio between peak area, when the opposite variation of adjacent two needles zinc thiazole peak area ratio is less than 1%, according to standard specimen solution,
Sample solution, sample solution, standard specimen solution sequence be measured.
Zinc thiazole area in two needle standard specimen solutions before and after the two needle sample solutions and sample that measure is averaged respectively.
The mass fraction X of zinc thiazole in sample1(%), (1) calculates as the following formula:
X1=r2·m1·p/r1·m2…………………(1)
R in formula1--- the average value of zinc thiazole peak area in standard specimen solution；
r2--- the average value of zinc thiazole peak area in sample solution；
m1--- the quality of standard specimen, g；
m2--- the quality of sample, g；
P --- the mass fraction of zinc thiazole, % in standard specimen.
Nanometer zinc thiazole content measuring result:
Assay is carried out using nanometer zinc thiazole of the high performance liquid chromatography to preparation, the nanometer zinc thiazole of different batches contains
Amount is between 95.5-96.5%.
Test two, nanometer zinc thiazole and commercialization raw medicine zinc thiazole dispersion degree comparative test in water
Nanometer zinc thiazole 100mg, 50mg, 10mg, 5mg, the 1mg for weighing 95.8% preparation of embodiment 1 uniformly divide respectively
It dissipates in 10ml water, is configured to the emulsion of 10,5.0,1.0,0.5,0.1mg/ml, appearance is milky uniform liquid, static
Place 7 days or milky mixed liquor.The zinc thiazole of raw medicine 96% is commercialized, also weighs 100mg, 50mg, 10mg, 5mg, 1mg
It is dispersed in 10ml water respectively, is configured to the dispersion liquid of 10,5.0,1.0,0.5,0.1mg/ml, appearance is muddy shape liquid
Body, particle just sinks down into bottom after 5min.
The present invention prepares the milk that the emulsion after resulting nanometer zinc thiazole is directly diluted with water is appearance stable homogeneous
Shape liquid, as nanometer zinc thiazole are directly sprayed on plant leaf blade prevention and treatment plant pathogenetic bacteria and fungi, and have after can diluting
Certain better zinc supplementation effect.
Comparative example 1,
Cancel the use of " the dispersing agent NNO " in 1 step 2) of embodiment, that is, the dosage of dispersing agent NNO is 0, remaining is equivalent
In embodiment 1.
The content 81% of gained zinc thiazole.Yield 43.5% is measured using Malvern particle size analyzer, gained thiazole zinc granule
Diameter is distributed as between 10-50 μm.
The above list is only a few specific embodiments of the present invention for finally, it should also be noted that.Obviously, this hair
Bright to be not limited to above embodiments, acceptable there are many deformations.Those skilled in the art can be from present disclosure
All deformations for directly exporting or associating, are considered as protection scope of the present invention.
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