CN106538525A - Many wall thickness microcapsule formulations of jamaicin and preparation method thereof - Google Patents
Many wall thickness microcapsule formulations of jamaicin and preparation method thereof Download PDFInfo
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- CN106538525A CN106538525A CN201610952922.1A CN201610952922A CN106538525A CN 106538525 A CN106538525 A CN 106538525A CN 201610952922 A CN201610952922 A CN 201610952922A CN 106538525 A CN106538525 A CN 106538525A
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- Prior art keywords
- jamaicin
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- wall thickness
- parts
- capsule
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- WITLAWYGGVAFLU-UHFFFAOYSA-N 3-(6-methoxy-1,3-benzodioxol-5-yl)-8,8-dimethylpyrano[2,3-f]chromen-4-one Chemical compound C1=CC(C)(C)OC2=CC=C(C(C(C3=CC=4OCOC=4C=C3OC)=CO3)=O)C3=C21 WITLAWYGGVAFLU-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 239000003094 microcapsule Substances 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000000203 mixture Substances 0.000 title claims abstract description 26
- 238000009472 formulation Methods 0.000 title claims abstract description 22
- 206010011732 Cyst Diseases 0.000 claims abstract description 24
- 208000031513 cyst Diseases 0.000 claims abstract description 24
- 239000007864 aqueous solution Substances 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 38
- 239000000375 suspending agent Substances 0.000 claims description 25
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 22
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 238000004220 aggregation Methods 0.000 claims description 11
- 230000002776 aggregation Effects 0.000 claims description 11
- 235000011187 glycerol Nutrition 0.000 claims description 11
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 239000003995 emulsifying agent Substances 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 239000012895 dilution Substances 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 7
- 238000012695 Interfacial polymerization Methods 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- 239000002775 capsule Substances 0.000 claims description 5
- 239000004530 micro-emulsion Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- YBHILYKTIRIUTE-UHFFFAOYSA-N berberine Chemical compound C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 YBHILYKTIRIUTE-UHFFFAOYSA-N 0.000 claims description 3
- 239000003225 biodiesel Substances 0.000 claims description 3
- 244000299492 Thespesia populnea Species 0.000 claims description 2
- 235000009430 Thespesia populnea Nutrition 0.000 claims description 2
- 229940093265 berberine Drugs 0.000 claims description 2
- QISXPYZVZJBNDM-UHFFFAOYSA-N berberine Natural products COc1ccc2C=C3N(Cc2c1OC)C=Cc4cc5OCOc5cc34 QISXPYZVZJBNDM-UHFFFAOYSA-N 0.000 claims description 2
- 230000003111 delayed effect Effects 0.000 claims description 2
- 125000005442 diisocyanate group Chemical group 0.000 claims description 2
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 claims description 2
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 claims description 2
- 229940073769 methyl oleate Drugs 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims 1
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 19
- 201000010099 disease Diseases 0.000 abstract description 9
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 abstract description 9
- 230000002045 lasting effect Effects 0.000 abstract description 8
- 230000002265 prevention Effects 0.000 abstract description 8
- 240000008067 Cucumis sativus Species 0.000 abstract description 7
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 abstract description 7
- 235000007688 Lycopersicon esculentum Nutrition 0.000 abstract description 6
- 241000607479 Yersinia pestis Species 0.000 abstract description 6
- 239000000575 pesticide Substances 0.000 abstract description 5
- 239000004480 active ingredient Substances 0.000 abstract description 4
- 230000000977 initiatory effect Effects 0.000 abstract description 4
- 231100000572 poisoning Toxicity 0.000 abstract description 4
- 230000000607 poisoning effect Effects 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 238000004166 bioassay Methods 0.000 abstract description 2
- 240000003768 Solanum lycopersicum Species 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 45
- 239000000725 suspension Substances 0.000 description 24
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 21
- 238000005259 measurement Methods 0.000 description 18
- 239000010779 crude oil Substances 0.000 description 17
- 239000003814 drug Substances 0.000 description 16
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 15
- 239000007764 o/w emulsion Substances 0.000 description 15
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 description 8
- 229920000147 Styrene maleic anhydride Polymers 0.000 description 8
- 229920001577 copolymer Polymers 0.000 description 7
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 7
- 229920000053 polysorbate 80 Polymers 0.000 description 7
- 241001083847 Berberis Species 0.000 description 6
- 235000016068 Berberis vulgaris Nutrition 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 6
- 241000227653 Lycopersicon Species 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000295 complement effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 235000013311 vegetables Nutrition 0.000 description 5
- 108010010803 Gelatin Proteins 0.000 description 4
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 4
- 239000003905 agrochemical Substances 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 239000008273 gelatin Substances 0.000 description 4
- 229920000159 gelatin Polymers 0.000 description 4
- 235000019322 gelatine Nutrition 0.000 description 4
- 235000011852 gelatine desserts Nutrition 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 4
- 239000000080 wetting agent Substances 0.000 description 4
- 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 description 3
- 241000233679 Peronosporaceae Species 0.000 description 3
- 210000000481 breast Anatomy 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 241000221785 Erysiphales Species 0.000 description 2
- 241001272567 Hominoidea Species 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 235000010489 acacia gum Nutrition 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 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 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 229920000136 polysorbate Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 229910001948 sodium oxide Inorganic materials 0.000 description 2
- 244000215068 Acacia senegal Species 0.000 description 1
- 241000198596 Alternaria tomatophila Species 0.000 description 1
- 241000133570 Berberidaceae Species 0.000 description 1
- -1 Chloroalkyl Acrylates Chemical class 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UDHMTPILEWBIQI-UHFFFAOYSA-N butyl naphthalene-1-sulfonate;sodium Chemical group [Na].C1=CC=C2C(S(=O)(=O)OCCCC)=CC=CC2=C1 UDHMTPILEWBIQI-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012395 formulation development Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000003810 morphinanes Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- UZRCGISJYYLJMA-UHFFFAOYSA-N phenol;styrene Chemical compound OC1=CC=CC=C1.C=CC1=CC=CC=C1 UZRCGISJYYLJMA-UHFFFAOYSA-N 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 229940113124 polysorbate 60 Drugs 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- ARENMZZMCSLORU-UHFFFAOYSA-N propan-2-yl naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)OC(C)C)=CC=CC2=C1 ARENMZZMCSLORU-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000003643 water by type Substances 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
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- 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
- A01N25/02—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 containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/16—Interfacial polymerisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Dentistry (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Plant Pathology (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses many wall thickness microcapsule formulations of a kind of jamaicin and preparation method thereof, said preparation includes the microcapsules of at least two different wall thickness scopes, wherein, the peak value of each wall thickness scope is different；The microcapsules include capsule-core and cyst wall, and the active ingredient in capsule-core is jamaicin.Pesticide bioassay result of the test shows, the microcapsule formulation of the present invention, and to tomato and the prevention effect of Cucumber Pests And Diseases, initial activity is very nearly the same with aqua, but the lasting period rises appreciably, and can be effectively reduced the poisoning to crop.
Description
Technical field
The present invention relates to a kind of novel formulation, and in particular to a kind of many wall thickness microcapsule formulations of jamaicin and its preparation side
Method.Belong to formulations of pesticide processing and applied technical field.
Background technology
With the main disease such as the continuous expansion of vegetable protecting field cultivated area, leaf spot, gray mold, powdery mildew, downy mildew
Evil is on the rise, and the medicament of the preventing and treating protecting field disease promoted at present is mostly chemical pesticide, and toxicity is high, and residual is serious, both
Pollution vegetables, affect people healthy, and cause potential threat to environment, have an effect on the foreign exchange earning of vegetables.Jamaicin is
A kind of alkaloid, it is present in many plants of the section ten of Berberidaceae etc. four category, to leaf spot, gray mold, powdery mildew, frost
The diseases such as mildew have preferable prevention effect, due to being natural extract, to vegetables, Environmental security, can be with green organic vegetable
Dish production.
Jamaicin is a kind of common morphinane alkaloid, molecular formula C20H18NO4.From nature, it is a kind of new
Natural bactericide.At present jamaicin is mainly processed into the use of 0.5% aqua, and due to the medicament it is easy under field conditions (factors)
Decompose and photodissociation, the lasting period is very short.
Pesticide micro capsule suspending agent due to the protective effect of cyst wall reduce capsule-core agricultural chemicals by external environment (as illumination,
Moisture) impact, reduce volatility, medicament outwards can be slowly discharged through cyst wall, extend the agricultural chemicals lasting period, thus gradually
Become one of new direction of agricultural chemicals green formulation development, be one of first-elected formulation of decrement agricultural chemicals.At present, with situ aggregation method or boundary
Though face polymerization preparation prepares microcapsules and has been reported that, generally existing rate of release is difficult to control to, field efficacy is complied with one's wishes not to the utmost etc.
Problem, such as parcel are too thick, just imitate very poor；The problems such as wrapping up too thin, the lasting period is too short.
The content of the invention
The purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, there is provided a kind of many wall thickness microcapsules of jamaicin
Preparation, drug release rate are controllable, and drug release time is longer.
Present invention also offers the preparation method of this kind of microcapsule formulation.
For achieving the above object, the present invention adopts following technical proposals：
The many wall thickness microcapsule formulations of jamaicin, including the microcapsules of at least two different wall thickness scopes, wherein,
The peak value of each wall thickness scope is different；The microcapsules include capsule-core and cyst wall, and the active ingredient in capsule-core is jamaicin.
Preferably, the microcapsules include two kinds, and its wall thickness is respectively 0.2～0.6 μm and 0.4～1.0 μm, both
Weight accounting in the formulation is respectively 0.1～10%, 0.1～10%.
Preferably, the microcapsules include three kinds, and its wall thickness is respectively 0.2～0.5 μm, 0.4～0.8 μm and 0.5
～1.1 μm, three's weight accounting in the formulation is respectively 0.1～10%, 0.1～20% and 0.1～10%.
Preferably, the cyst wall is obtained by polymerisation or oil-soluble monomer and polymerisation.
It is further preferred that jamaicin is dissolved in organic solvent, the organic solvent is biodiesel or methyl oleate, little
Bark of a cork tree alkali is 5～30 with the mass ratio of organic solvent：3～10.
Preferably, the preparation is suspending agent, missible oil, aqueous emulsion or microemulsion.
It is further preferred that the preparation is suspending agent, it is by microcapsules and wetting agent, dispersant I and structure regulator
It is mixed, wherein, microcapsules are 5～250 with the mass ratio of wetting agent, dispersant I, structure regulator：1～50：1～
100：1～50.
Still more preferably, the wetting agent is sodium butylnaphthalenesulfonate salt, NPE (NP-10), benzene
Any one in vinyl benzene phenol polyethenoxy ether (agricultural emulsifier NO.600), isopropyl naphthalene sulfonate or alkylnaphthalene sulfonate, dispersant
I is naphthalenesulfonate formaldehyde condensation compound NNO, maleic-acrylic acid sodium salt, sodium lignin sulfonate, APES formaldehyde
Any one in condensate sulfonates, structure regulator are any one in sodium cellulose glycolate, gelatin or gum arabic.
The preparation method of many wall thickness microcapsule formulations of above-mentioned jamaicin, including step：
(1) jamaicin of at least two different wall thickness scopes is prepared by situ aggregation method or interfacial polymerization
Microcapsules；
(2) at least two jamaicin microcapsules described in step (1) are carried out into mixture according to proportioning, then according to preparation class
Type adds corresponding auxiliary material, and then prepares corresponding preparations.
Preferably, using situ aggregation method, the preparation method of step (1) Berberine microcapsules is：Capsule-core is added to
In cyst material I, emulsifying agent and dispersant II are added, dispersed with stirring forms O/W emulsions, slow to adjust pH to 2.5, heats up solid
Change, adjust pH=7, obtain final product microcapsules.
It is further preferred that the mass ratio of capsule-core, cyst material I, emulsifying agent and dispersant II is 8～40：60：2～10：
1.5～5.
It is further preferred that the temperature of elevated cure is 60 DEG C, the time used of heating up is 90 minutes.
It is further preferred that the cyst material I for different quality containing the urea resin prepolymer aqueous solution, its be by
The urea resin prepolymer aqueous solution dilution of mass fraction 25% is obtained, and the preparation method of the latter is：Urea and formaldehyde are mixed,
Dissolving, adds deionized water, adjusts pH to 8, and 70 DEG C are incubated 1 hour, obtain final product；Wherein, the mol ratio of urea and formaldehyde is 1：1.5
～2.5, the mass ratio of urea and deionized water is 10：42.
Preferably, using interfacial polymerization, in step (1), the preparation method of microcapsules is：Jamaicin is dissolved in organic molten
Agent, is formed capsule-core, and is mixed with cyst material II, be added in emulsifying agent, after quickly stirring, be slowly dropped into glycerine,
Stir speed (S.S.) is reduced, 35 DEG C are incubated 30 minutes, obtain final product.
It is further preferred that the cyst material II is diisocyanate (TDI).
It is further preferred that the mass ratio of capsule-core, cyst material II, emulsifying agent and glycerine is 5～250：5～20：5～
250：5～20.
It is further preferred that the stir speed (S.S.) of quick stirring is 1000～1600r/min, the stir speed (S.S.) after reduction is
300r/min。
It is further preferred that the emulsifying agent is APES, naphthalene sulfonic acid-formaldehyde condensation product, detergent alkylate
Sodium sulfonate, polyvinyl alcohol, polysorbate60, Tween 80, styrene-maleic anhydride copolymer, Arabic gum and Styrene And Chloroalkyl Acrylates are altogether
Any one in polymers.
It is further preferred that the dispersant II is NNO or sodium lignin sulfonate.
Preferably, the preparation type in step (2) includes suspending agent, missible oil, aqueous emulsion or microemulsion.
It is further preferred that the concrete grammar of step (2) is：By at least two microcapsules obtained by step (1) according to matching somebody with somebody
Than carrying out mixture, wetting agent, dispersant or the structure regulator of formula ratio are subsequently adding, suspending agent is prepared.
Beneficial effects of the present invention：
The active ingredient of the present invention is jamaicin, and which makes microcapsule formulation, changes that effect microcapsule wall thickness is uniform, deposits
In the present situation of single peak value, including the microcapsules of at least two different wall thickness scopes, also, each wall thickness scope
Peak value is different, that is, there are two or more multiple peak values, and during use, the microcapsules of low wall thickness preferentially break capsule release effectively
Composition, shows excellent first effect, and the microcapsules of high wall thickness are delayed brokenly capsule release active ingredient, extend the preparation lasting period.
, there are multiple release peaks, effectively reduces times for spraying in the microcapsules mixing of different wall thickness during medication, reduce dispenser to plant
The injury that root system is caused, reduces labour intensity, while reducing cost accounting.
Pesticide bioassay result of the test shows, the microcapsule formulation of the present invention, the preventing and treating to tomato and Cucumber Pests And Diseases
Effect, initial activity are very nearly the same with aqua, but the lasting period rises appreciably, and can be effectively reduced the poisoning to crop.
Specific embodiment
With reference to embodiment, the present invention will be further elaborated, it should explanation, the description below merely to
The present invention is explained, its content is not defined.
" part " being hereinafter related to refers both to weight portion, and percentage refers both to mass percent.
Jamaicin crude oil, is provided by Shandong Sheng Peng Science and Technology Co., Ltd..
Reference implementation example：
The preparation of Lauxite (UF) the performed polymer aqueous solution of mass fraction 25%
By 10 parts of urea and 24 part of 37% formalin mixing, dissolving, after adding 42 parts of deionized waters, pH to 8,70 is adjusted
DEG C insulation 1 hour, obtains mass fraction for the 25% urea resin prepolymer aqueous solution, is designated as the UF aqueous solution (25%).
Embodiment 1：
0.5% jamaicin micro-capsule suspension of situ aggregation method
The UF aqueous solution (25%) the deionized water dilution of reference implementation example is obtained into the Lauxite of mass fraction 0.5%
The performed polymer aqueous solution, is designated as the UF aqueous solution (0.5%).
5 parts of jamaicin crude oil are dissolved in into 2 parts of biodiesel and obtain capsule-core oil phase, be added to 400 parts of UF aqueous solution (0.5%)
In, add 5 parts and 3 parts of NNO of emulsifying agent phenylethylene-maleic anhydride；1000r/min dispersed with stirring is into O/W emulsions；Use 1moL/
LHCl slowly adjusts pH to 2.5, is subsequently progressively warmed up to 60 DEG C, and the heating-up time is 90 minutes, solidifies encystation.Reach reaction end
Afterwards, pH ≈ 7 are adjusted with NaOH.
4 parts of 5 parts of NP-10,5 parts of dispersant NNO and structure regulator gelatin are subsequently adding, deionized water is complemented to always
Measure as 1000 parts, stir, as 0.5% jamaicin micro-capsule suspension.
The microcapsules average grain diameter and wall thickness measurement result of 1 gained suspending agent of embodiment is shown in Table 1.
The microcapsules average grain diameter and wall thickness measurement result of 1. embodiment of table, 1 gained suspending agent
| Microcapsules average grain diameter d (μm) | Effect microcapsule wall thickness (μm) |
| 6.98 | 0.34 |
Embodiment 2：
The many wall thickness micro-capsule suspensions of 0.5% jamaicin of situ aggregation method
By the UF aqueous solution (25%) of reference implementation example, deionized water dilution obtains mass fraction 0.4%, 0.6% respectively
The urea resin prepolymer aqueous solution with 0.8%, is designated as the UF aqueous solution (0.4%), the UF aqueous solution (0.6%) and UF water-soluble respectively
Liquid (0.8%).
Agent a：5 parts of jamaicin crude oil are dissolved in into 2 parts of methyl oleates and obtain capsule-core oil phase, be added to 400 parts of 0.4%UF water-soluble
In liquid, 4 parts and 2 parts of NNO of styrene-maleic anhydride copolymer is added；800r/min dispersed with stirring is into O/W emulsions；Use 1moL/L
HCl slowly adjusts pH to 2.5, is subsequently progressively warmed up to 60 DEG C, is warmed up to 60 DEG C of times for 90 minutes, solidifies encystation.Reach anti-
After answering terminal, pH ≈ 7 are adjusted with NaOH.0.2～0.5 μm of prepared effect microcapsule wall.
Agent b：5 parts of jamaicin crude oil are dissolved in into 2 parts of methyl oleates, are added in 400 parts of UF aqueous solution (0.6%), added
5 parts and 3 parts of NNO of styrene-maleic anhydride copolymer, 1000r/min dispersed with stirring is into O/W emulsions；It is slow with 1moL/L HCl
PH to 2.5 is adjusted, 60 DEG C are subsequently progressively warmed up to, the heating-up time is 90 minutes, solidifies encystation.After reaching reaction end, hydrogen is used
Sodium oxide molybdena adjusts pH ≈ 7.0.4～0.8 μm of prepared effect microcapsule wall.
Agent c：5 parts of jamaicin crude oil are dissolved in into 2 parts of methyl oleates, are added in 400 parts of UF aqueous solution (0.8%), added
6 parts and 4 parts of NNO of styrene-maleic anhydride copolymer, 1200r/min dispersed with stirring is into O/W emulsions；It is slow with 1moL/L HCl
PH to 2.5 is adjusted, 60 DEG C are subsequently progressively warmed up to, the heating-up time is 90 minutes, solidifies encystation.After reaching reaction end, hydrogen is used
Sodium oxide molybdena adjusts pH ≈ 7.0.5～1.1 μm of prepared effect microcapsule wall.
Agent a, agent b and agent c are pressed into 30：40：30 or needed for other mass ratio mixing, add 4 parts of NP-10,5 parts of NNO and
5 parts of sodium cellulose glycolate, deionized water complement to total amount for 1000 parts, stir, wall thickness as more than 0.5%
Jamaicin micro-capsule suspension.
Effect microcapsule wall thickness measuring method：
Assume that microcapsules are spherical, and the particle size and cyst wall uniformity of microcapsules, thus can be quantitative
Analytical parameters between relation.By spheroid cubature formula and density formula：
In formula, W is quality, and ρ is density, and R is radius, and subscript w and n represent capsule-core and cyst wall, r respectively1For capsule-core radius, r2
For the radius of microcapsules (capsule-core adds wall thickness).If it is known that the radius r of the density and microcapsules of capsule-core, cyst wall2, Ke Yiji
Calculate r1Value, and then derive the wall thickness of microcapsules：
The Microcapsules Size and wall thickness measurement result of 2 gained suspending agent of embodiment is shown in Table 2.
The Microcapsules Size and wall thickness measurement result of 2. embodiment of table, 2 gained suspending agent
Embodiment 3：
The many wall thickness micro-capsule suspensions of 1.0% jamaicin of situ aggregation method
By the UF aqueous solution (25%) of reference implementation example, deionized water dilution obtains mass fraction 0.6%, 0.8% respectively
The urea resin prepolymer aqueous solution with 1.0%, is designated as the UF aqueous solution (0.6%), the UF aqueous solution (0.8%) and UF water-soluble respectively
Liquid (1.0%).
Take 10 parts of jamaicin crude oil and be dissolved in 4 parts of methyl oleates, agent a：(0.6%) 400 part of the UF aqueous solution, styrene-Malaysia
4 parts of acid anhydride copolymer, 2 parts of sodium lignin sulfonate, 1000r/min dispersed with stirring is into O/W emulsions.Agent b：The UF aqueous solution (0.8%)
400 parts, 5 parts of styrene-maleic anhydride copolymer, 2 parts of sodium lignin sulfonate, 1200r/min dispersed with stirring is into O/W emulsion agent c：
(1.0%) 400 part of the UF aqueous solution, 6 parts of styrene-maleic anhydride copolymer, 3 parts of sodium lignin sulfonate, 1500r/min stirrings point
Dissipate into O/W emulsions.Remaining is processed into many wall thickness micro-capsule suspensions of 1.0% jamaicin with embodiment 2.
The Microcapsules Size and wall thickness measurement result of 3 gained suspending agent of embodiment is shown in Table 3.
The Microcapsules Size and wall thickness measurement result of 3. embodiment of table, 3 gained suspending agent
Embodiment 4：
The many wall thickness micro-capsule suspensions of 2.5% jamaicin of situ aggregation method
By the UF aqueous solution (25%) of reference implementation example, deionized water dilution obtains mass fraction 0.8%, 1.0% respectively
The urea resin prepolymer aqueous solution with 1.2%, is designated as the UF aqueous solution (0.8%), the UF aqueous solution (1.0%) and UF water-soluble respectively
Liquid (1.2%).
Take 25 parts of jamaicin crude oil and be dissolved in 8 parts of methyl oleates, agent a：(0.8%) 400 part of the UF aqueous solution, 6 parts of Tween 80,
2 parts of NNO, 1000r/min dispersed with stirring is into O/W emulsions；Agent b：(1.0%) 400 part of the UF aqueous solution, 8 parts of Tween 80, NNO 3
Part, 1200r/min dispersed with stirring is into O/W emulsions；Agent c：(1.2%) 400 part of the UF aqueous solution, 10 parts of Tween 80,4 parts of NNO,
1500r/min dispersed with stirring is into O/W emulsions；Remaining is processed into many wall thickness microcapsules of 2.5% jamaicin and hangs with embodiment 2
Floating agent.
The Microcapsules Size and wall thickness measurement result of 4 gained suspending agent of embodiment is shown in Table 4.
The Microcapsules Size and wall thickness measurement result of 4. embodiment of table, 4 gained suspending agent
Embodiment 5：
The many wall thickness micro-capsule suspensions of 5.0% jamaicin of situ aggregation method
By the UF aqueous solution (25%) of reference implementation example, deionized water dilution obtains mass fraction 1.6%, 2.0% respectively
The urea resin prepolymer aqueous solution with 2.4%, is designated as the UF aqueous solution (1.6%), the UF aqueous solution (2.0%) and UF water-soluble respectively
Liquid (2.4%).
Take 50 parts of jamaicin crude oil and be dissolved in 10 parts of methyl oleates, agent a：(1.6%) 400 part of the UF aqueous solution, 8 parts of Tween 80,
3 parts of NNO, 1000r/min dispersed with stirring is into O/W emulsions；Agent b：(2.0%) 400 part of the UF aqueous solution, 10 parts of Tween 80, NNO 4
Part, 1200r/min dispersed with stirring is into O/W emulsions；Agent c：(2.4%) 400 part of the UF aqueous solution, 12 parts of Tween 80,5 parts of NNO,
1500r/min dispersed with stirring is into O/W emulsions；Remaining is processed into many wall thickness microcapsules of 5.0% jamaicin and hangs with embodiment 2
Floating agent.
The Microcapsules Size and wall thickness measurement result of 5 gained suspending agent of embodiment is shown in Table 5.
The Microcapsules Size and wall thickness measurement result of 5. embodiment of table, 5 gained suspending agent
Embodiment 6：
The many wall thickness micro-capsule suspensions of 10% jamaicin of situ aggregation method
By the UF aqueous solution (25%) of reference implementation example, deionized water dilution obtains 2.5% He of mass fraction respectively
The 3.5% urea resin prepolymer aqueous solution, is designated as the UF aqueous solution (2.5%) and the UF aqueous solution (3.5%) respectively.
Take 100 parts of jamaicin crude oil and be dissolved in 15 parts of methyl oleates, agent a：(2.5%) 400 part of the UF aqueous solution, Tween 80 15
6 parts of part and NNO, 1000r/min dispersed with stirring is into O/W emulsions；Agent b：(3.5%) 400 part of the UF aqueous solution, 20 parts of Tween 80 and
8 parts of NNO, 1200r/min dispersed with stirring is into O/W emulsions；Remaining is with embodiment 2.
By agent a and agent b with 50：50 or mass ratio mixing needed for other, add 8 parts of NP-10,15 parts of NNO and structure
10 parts of conditioning agent gelatin, deionized water complement to total amount for 1000 parts, stir, wall thickness jamaicin as more than 10%
Micro-capsule suspension.
The Microcapsules Size and wall thickness measurement result of 6 gained suspending agent of embodiment is shown in Table 6.
The Microcapsules Size and wall thickness measurement result of 6. embodiment of table, 6 gained suspending agent
Embodiment 7：
The many wall thickness micro-capsule suspensions of 0.5% jamaicin of interfacial polymerization
Agent a：5 parts of jamaicin crude oil are dissolved in into 2 parts of methyl oleates, and are mixed with 2 parts of TDI, be added to 300 part of 0.5% benzene
In the ethylene maleic acid anhydride copolymer aqueous solution, after 1000r/min quickly stirs, 2 parts of glycerine is taken, be slowly added dropwise into anti-
In answering container.Rotating speed is reduced to 300r/min, 30 minutes is incubated at 35 DEG C, that is, is obtained the barberry that wall thickness is 0.2～0.5 μm
Alkali microcapsules.
Agent b：5 parts of jamaicin crude oil are dissolved in into 2 parts of methyl oleates, and are mixed with 3 parts of TDI, be added to 320 part of 0.5% benzene
In the ethylene maleic acid anhydride copolymer aqueous solution, after 1200r/min quickly stirs, 3 parts of glycerine is taken, be slowly added dropwise into anti-
In answering container.Rotating speed is reduced to 300r/min, 30 minutes is incubated at 35 DEG C, that is, is obtained the barberry that wall thickness is 0.4～0.8 μm
Alkali microcapsules.
Agent c：5 parts of jamaicin crude oil are dissolved in into 2 parts of methyl oleates, and are mixed with 4 parts of TDI, be added to 340 part of 0.5% benzene
In the ethylene maleic acid anhydride copolymer aqueous solution, after 1500r/min quickly stirs, 4 parts of glycerine is taken, be slowly added dropwise into anti-
In answering container.Rotating speed is reduced to 300r/min, 30min is incubated at 35 DEG C, that is, is obtained the barberry that wall thickness is 0.5～1.1 μm
Alkali microcapsules.
By agent a, agent b and agent c with 30：40：30 or mass ratio mixing needed for other, add 2 parts of agriculture breast P-10, wooden
3 parts of 5 parts of plain sodium sulfonate and gelatin, deionized water complement to total amount for 1000 parts, stir, and as more than 0.5%, cyst wall is thick
Degree jamaicin micro-capsule suspension.
The Microcapsules Size and wall thickness measurement result of 7 gained suspending agent of embodiment is shown in Table 7.
The Microcapsules Size and wall thickness measurement result of 7. embodiment of table, 7 gained suspending agent
Embodiment 8：
The many wall thickness micro-capsule suspensions of 3.0% jamaicin of interfacial polymerization
Agent a：30 parts of jamaicin crude oil are dissolved in into 5 parts of methyl oleates, and are mixed with 4 parts of TDI, be added to 400 part of 0.5% benzene
In the ethylene maleic acid anhydride copolymer aqueous solution, after 1000r/min quickly stirs, 4 parts of glycerine is taken, be slowly added dropwise into anti-
In answering container.Rotating speed is reduced to 300r/min, 30 minutes is incubated at 35 DEG C, that is, is obtained the barberry that wall thickness is 0.2～0.5 μm
Alkali microcapsules.
Agent b：30 parts of jamaicin crude oil are dissolved in into 5 parts of methyl oleates, and are mixed with 5 parts of TDI, be added to 420 part of 0.5% benzene
In the ethylene maleic acid anhydride copolymer aqueous solution, after 1200r/min quickly stirs, 5 parts of glycerine is taken, be slowly added dropwise into anti-
In answering container.Rotating speed is reduced to 300r/min, 30 minutes is incubated at 35 DEG C, that is, is obtained the barberry that wall thickness is 0.4～0.8 μm
Alkali microcapsules.
Agent c：30 parts of jamaicin crude oil are dissolved in into 5 parts of methyl oleates, and are mixed with 6 parts of TDI, be added to 440 part of 0.5% benzene
In the ethylene maleic acid anhydride copolymer aqueous solution, after 1500r/min quickly stirs, 6 parts of glycerine is taken, be slowly added dropwise into anti-
In answering container.Rotating speed is reduced to 300r/min, 30 minutes is incubated at 35 DEG C, that is, is obtained the barberry that wall thickness is 0.5～1.1 μm
Alkali microcapsules.
By agent a, agent b and agent c with 30：40：30 or needed for other mass ratio mixing, add agriculture breast 601#5 part, lignin
5 parts of 8 parts of sodium sulfonate and sodium cellulose glycolate, deionized water complement to total amount for 1000 parts, stir, and as 3.0%
Many wall thickness jamaicin micro-capsule suspensions.
The Microcapsules Size and wall thickness measurement result of 8 gained suspending agent of embodiment is shown in Table 8.
The Microcapsules Size and wall thickness measurement result of 8. embodiment of table, 8 gained suspending agent
Embodiment 9：
The many wall thickness micro-capsule suspensions of 10% jamaicin of interfacial polymerization
Agent a：100 parts of jamaicin crude oil are dissolved in into 15 parts of methyl oleates, and are mixed with 10 parts of TDI, be added to 400 parts
In the 0.5% styrene-maleic anhydride copolymer aqueous solution, after 1200r/min quickly stirs, 10 parts of glycerine is taken, slowly
It is added dropwise in reaction vessel.Rotating speed is reduced to 300r/min, at 35 DEG C, 30 minutes is incubated, that is, wall thickness is obtained for 0.2～0.6
μm jamaicin microcapsules.
Agent b：100 parts of jamaicin crude oil are dissolved in into 15 parts of methyl oleates, and are mixed with 15 parts of TDI, be added to 450 parts
In the 0.5% styrene-maleic anhydride copolymer aqueous solution, after 1500r/min quickly stirs, 15 parts of glycerine is taken, slowly
It is added dropwise in reaction vessel.Rotating speed is reduced to 300r/min, at 35 DEG C, 30 minutes is incubated, that is, wall thickness is obtained for 0.4～1.0
μm jamaicin microcapsules.
By agent a and agent b with 50：50 or needed for other mass ratio mixing, add agriculture breast 601#5 part, sodium lignin sulfonate 6
5 parts of part and sodium cellulose glycolate, deionized water complement to total amount for 1000 parts, stir, and as more than 10%, cyst wall is thick
Degree jamaicin micro-capsule suspension.
The Microcapsules Size and wall thickness measurement result of 9 gained suspending agent of embodiment is shown in Table 9.
The Microcapsules Size and wall thickness measurement result of 9. embodiment of table, 9 gained suspending agent
Selected section product carries out preventing and treating tomato in greenhouse pest and disease damage field control effectiveness test
Medicament A：0.5% jamaicin aqua (is provided by Shandong Sheng Peng Science and Technology Co., Ltd.)
Medicament B：0.5% jamaicin micro-capsule suspension (embodiment 1)
Medicament C：The many cyst wall micro-capsule suspensions of 1.0% jamaicin (embodiment 3)
Medicament D：The many wall thickness micro-capsule suspensions of 0.5% jamaicin (embodiment 7)
Medicament E：The many wall thickness micro-capsule suspensions of 10% jamaicin (embodiment 9)
Blank is CK
Field plot arranging situation is shown in Table 10.
10. field plot arranging situation of table
| A | C | D | E | B | CK |
| B | E | A | CK | C | D |
| C | A | B | D | CK | E |
| E | D | CK | B | A | C |
4 repetitions of random alignment, per 10 square metres of plot area (5 meters × 2 meters).
Table 11～12 lists different agents respectively to graw mold of tomato and the prevention effect of early blight.
Prevention effect of 11. different agents of table to graw mold of tomato
Prevention effect of 12. different agents of table to early blight of tomato
From table 11～12 as can be seen that many wall thickness microcapsule formulations of the present invention, the preventing and treating effect to tomato pest and disease damage
Really, initial activity is very nearly the same with aqua, but the lasting period rises appreciably, and can be effectively reduced the poisoning to crop.
Selected section product carries out preventing and treating dependent territory cucumber pest and disease damage field control effectiveness test
Medicament A：0.5% jamaicin aqua (is provided by Shandong Sheng Peng Science and Technology Co., Ltd.)
Medicament B：0.5% jamaicin micro-capsule suspension (embodiment 1)
Medicament F：The many cyst wall micro-capsule suspensions of 2.0% jamaicin (embodiment 4)
Medicament G：The many wall thickness micro-capsule suspensions of 5.0% jamaicin (embodiment 5)
Medicament H：The many wall thickness micro-capsule suspensions of 3.0% jamaicin (embodiment 8)
Blank is CK
Field plot arranging situation is shown in Table 13.
13. field plot arranging situation of table
| A | F | G | CK | B | H |
| B | H | CK | G | A | F |
| g | A | F | B | H | CK |
| F | G | H | A | CK | B |
4 repetitions of random alignment, per 10 square metres of plot area (5 meters × 2 meters).
Table 14～15 lists different agents respectively to gray mold of cucumber and the prevention effect of downy mildew.
Prevention effect of 14. different agents of table to gray mold of cucumber
Prevention effect of 15. different agents of table to cucumber downy mildew
From table 14～15 as can be seen that many wall thickness microcapsule formulations of the present invention, the preventing and treating effect to Cucumber Pests And Diseases
Really, initial activity is very nearly the same with aqua, but the lasting period rises appreciably, and can be effectively reduced the poisoning to crop.
Although the above-mentioned specific embodiment to the present invention is described, not the limit to the scope of the present invention
System, on the basis of technical scheme, it is each that those skilled in the art are made by need not paying creative work
Kind modification or deformation are still within protection scope of the present invention.
Claims (10)
1. many wall thickness microcapsule formulations of jamaicin, it is characterised in that including the micro- of at least two different wall thickness scopes
Capsule, wherein, the peak value of each wall thickness scope is different；The microcapsules include capsule-core and cyst wall, in capsule-core it is effective into
It is divided into jamaicin.
2. microcapsule formulation according to claim 1, it is characterised in that the cyst wall is by polymerisation or oil
Soluble monomers and polymerisation and obtain.
3. microcapsule formulation according to claim 1, it is characterised in that jamaicin is dissolved in organic solvent, described organic
Solvent is biodiesel or methyl oleate, and jamaicin is 5～30 with the mass ratio of organic solvent：3～10.
4. microcapsule formulation according to claim 1, it is characterised in that the preparation be suspending agent, missible oil, aqueous emulsion or
Microemulsion.
5. the preparation method of the microcapsule formulation any one of Claims 1 to 4, it is characterised in that including step：
(1) the micro- glue of jamaicin of at least two different wall thickness scopes is prepared by situ aggregation method or interfacial polymerization
Capsule；
(2) at least two jamaicin microcapsules described in step (1) are carried out into mixture according to proportioning, then according to preparation type adds
Enter corresponding auxiliary material, and then prepare corresponding preparations.
6. preparation method according to claim 5, it is characterised in that adopt situ aggregation method, step (1) Berberine is micro-
The preparation method of capsule is：Capsule-core is added in cyst material I, adds emulsifying agent and dispersant II, dispersed with stirring to form O/W
Emulsion, slow to adjust pH to 2.5, elevated cure adjusts pH=7, obtains final product microcapsules.
7. preparation method according to claim 6, it is characterised in that urea of the cyst material I for different quality containing
The urea formaldehyde performed polymer aqueous solution, which is obtained by the urea resin prepolymer aqueous solution dilution of mass fraction 25%, the system of the latter
Preparation Method is：By urea and formaldehyde mixing, dissolving, deionized water being added, pH being adjusted to 8,70 DEG C are incubated 1 hour, obtain final product；Its
In, the mol ratio of urea and formaldehyde is 1：1.5～2.5, the mass ratio of urea and deionized water is 10：42.
8. preparation method according to claim 5, it is characterised in that the preparation method of microcapsules is in step (1)：Will be little
Bark of a cork tree alkali soluble is formed capsule-core, and is mixed with cyst material II, be added in emulsifying agent in organic solvent, after quickly stirring, is delayed
It is slow to instill glycerine, stir speed (S.S.) is reduced, 35 DEG C are incubated 30 minutes, obtain final product.
9. preparation method according to claim 8, it is characterised in that the cyst material II is diisocyanate.
10. preparation method according to claim 5, it is characterised in that the preparation type in step (2) include suspending agent,
Missible oil, aqueous emulsion or microemulsion.
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| CN101574083A (en) * | 2009-06-19 | 2009-11-11 | 北京化工大学 | Preparation methods of sustained-release microcapsule and sustained-release composite membrane for inhibiting monilinia fructicola |
| US20140274716A1 (en) * | 2013-03-14 | 2014-09-18 | Dow Agrosciences Llc | Capsule suspension formulations of dithiopyr herbicide |
| CN105724399A (en) * | 2016-03-28 | 2016-07-06 | 天峨县平昌生态农业有限公司 | Sterilization composition containing berberine and azoxystrobin |
| CN105919971A (en) * | 2016-06-23 | 2016-09-07 | 潘元明 | Berberine-glucan microcapsule as well as preparation method and application thereof |
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2016
- 2016-11-03 CN CN201610952922.1A patent/CN106538525A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101574083A (en) * | 2009-06-19 | 2009-11-11 | 北京化工大学 | Preparation methods of sustained-release microcapsule and sustained-release composite membrane for inhibiting monilinia fructicola |
| US20140274716A1 (en) * | 2013-03-14 | 2014-09-18 | Dow Agrosciences Llc | Capsule suspension formulations of dithiopyr herbicide |
| CN105724399A (en) * | 2016-03-28 | 2016-07-06 | 天峨县平昌生态农业有限公司 | Sterilization composition containing berberine and azoxystrobin |
| CN105919971A (en) * | 2016-06-23 | 2016-09-07 | 潘元明 | Berberine-glucan microcapsule as well as preparation method and application thereof |
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Application publication date: 20170329 |