CN102415405B - Dinotefuran micron-emulsion and preparation method thereof - Google Patents

Dinotefuran micron-emulsion and preparation method thereof Download PDF

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CN102415405B
CN102415405B CN201110339065.5A CN201110339065A CN102415405B CN 102415405 B CN102415405 B CN 102415405B CN 201110339065 A CN201110339065 A CN 201110339065A CN 102415405 B CN102415405 B CN 102415405B
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emulsion
dinotefuran
micron
dinotefuran micron
mti
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CN102415405A (en
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王洲
卢桂鲜
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Lianbao Crop Technology Co Ltd
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Lianbao Crop Technology Co Ltd
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Abstract

The invention relates to the field of pesticide preparations, and provides a dinotefuran micron-emulsion and a preparation method thereof. The dinotefuran micron-emulsion comprises components of, by weight: 1-40% of dinotefuran, 10-30% of a solvent, 10-25% of a surfactant, 5-15% of a co-solvent, and balance of water. The dinotefuran micron-emulsion provided by the invention is advantaged in low cost, simple preparation process, low packaging requirement, reduced organic solvent dosage, low residue, and small pollution on the environment. The controlling effect provided by the dinotefuran micron-emulsion is higher than that of dinotefuran particle preparations. Therefore, the dinotefuran micron-emulsion is suitable to be broadly popularized.

Description

A kind of dinotefuran micron-emulsion and preparation method thereof
Technical field
The present invention relates to pesticidal preparations field, relate to specifically a kind of dinotefuran micron-emulsion and preparation method thereof.
Background technology
MTI-446 (dinotefuran), chemical name is (RS)-1-methyl-2-nitro-3-[(3-oxolane)-methyl] guanidine, it is the third generation nicotinic insecticide of Mitsui chemical company exploitation, the chemical constitution of itself and existing nicotinic insecticide is far from each other, chloro-pyridine base, chloro thiazolyl before its tetrahydrofuran base has replaced, containing halogen.Meanwhile, also different with nicotine at aspect of performance.Be mainly used in preventing and treating aphid, leafhopper, plant hopper, thrips, aleyrodid and the resistant strain thereof in the various crop such as wheat, paddy rice, cotton, vegetables, fruit tree, tobacco leaf, coleoptera, diptera, Semiptera, Lepidoptera, beetle order and total wing order insect are had efficiently simultaneously, and the sanitary insect pests such as blattaria, termite, housefly are had efficiently.Fool proof to mammal, rat acute is low toxicity through skin and Oral toxicity; To fish and water flea low toxicity; To honeybee safety; Without teratogenesis, carcinogenic and mutagenesis.
The formulation of the MTI-446 pesticide product of applying on pesticide market is at present mainly take granule as main, if but the preventive effect of MTI-446 granule wants the level that reaches higher just need to increase formulation rate, this understands cause very large pollution to environment.
Simultaneously, along with the raising of people's environmental consciousness, to the restriction increasingly stringent of the organic solvent using in pesticidal preparations, thereby impel pesticidal preparations along efficient, low toxicity, with the good future development of Environmental compatibility, exploitation uses no or little the novel form of organic solvent, to replace pesticidal preparations, wherein the pesticides new formulation take water as matrix has become the direction of world pesticide dosage form research and development.
Microemulsion (microemulsion, ME) is take water as matrix, the novel green pesticidal preparations that utilize that physicochemical liquid-liquid dispersion system is theoretical and that method is prepared is efficient, store and transport safety, environmental pollution is low.Microemulsion has reduced consumption of organic solvent, has greatly alleviated the pressure to environment, significant for protection Agro-ecology balance, is more conducive to agriculture sustainable development.Therefore a kind of efficient, low toxicity of research and development, environment amenable MTI-446 pest killing micro emulsion are of great significance.
Summary of the invention
In view of this, the object of the invention is to provide a kind of efficient, little, environment amenable dinotefuran micron-emulsion of formulation rate.
For realizing object of the present invention, the present invention adopts following technical scheme:
A kind of dinotefuran micron-emulsion, comprise MTI-446, solvent, surfactant, cosolvent and water, wherein, the percentage by weight that each component accounts for described microemulsion gross weight is MTI-446 1-40%, organic solvent 10-30%, surfactant 10-25%, cosolvent 5-15%, and surplus is water;
Dinotefuran micron-emulsion of the present invention is take MTI-446 as active component, and as preferably, the percentage by weight that described MTI-446 accounts for described microemulsion gross weight is 5-20%.
Solvent of the present invention is selected from cyclohexanone, toluene, dimethylbenzene, DMSO, dimethyl formamide.
As preferably, the percentage by weight that described solvent accounts for described microemulsion gross weight is 15-20%.
Surfactant of the present invention is selected from one or more in compound, anion and the non-ionic surface active agent of anion and non-ionic surface active agent and the compound of solvent, calcium dodecyl benzene sulfonate, styryl phenol formaldehyde resin PULLRONIC F68 block type polyethers, the polyoxyethylene nonylphenol ether of nonionic or the OPEO of nonionic.
In certain embodiments, described surfactant is agriculture breast 0201B, agriculture breast 0203B, agriculture breast 0204C, agriculture breast 2201, OP series agriculture breast or agriculture breast 500, described OP series agriculture breast is preferably agriculture breast OP-10 or agriculture breast OP-21, and described surfactant is preferably agriculture breast 0204C, agriculture breast OP-10 or agriculture breast OP-21
Cosolvent of the present invention is ethanol, propyl alcohol, isopropyl alcohol or the tert-butyl alcohol, is preferably ethanol or isopropyl alcohol.As preferably, the percentage by weight that described cosolvent accounts for described microemulsion gross weight is 10-15%.
Dinotefuran micron-emulsion of the present invention can also comprise stabilizing agent, antifreezing agent and short bleeding agent, and wherein, the percentage by weight that each component accounts for described microemulsion gross weight is: stabilizing agent 1-5% antifreezing agent, 1-5% and short bleeding agent 1-10%.
Antifreezing agent of the present invention is selected from one or more in ethylene glycol, propane diols, glycerine, polyethylene glycol, sorbierite, urea, sucrose, glucose.Described short bleeding agent is azone, lauryl alcohol sodium sulphate, sodium lignin sulfonate or alkylphenol polyoxyethylene.Described stabilizing agent can be selected from well known in the art, conventional stabilizing agent.
The present invention also provides the preparation method of described dinotefuran micron-emulsion, according to described percentage by weight, MTI-446 is fully mixed with surfactant, cosolvent, then add other compositions, mixes, and finally adds water, after fully stirring, can be made into microemulsion.
Physicochemical property and field control effectiveness test result show, dinotefuran micron-emulsion stable performance of the present invention, transparent wide ranges, resolution ratio are low, rice fulgorid is had to significant drug effect, and compared with the MTI-446 granule of same dose (in active component), preventive effect is apparently higher than the preventive effect of granule.Show that dinotefuran micron-emulsion of the present invention need not increase formulation rate and can reach higher preventive effect, alleviated farm chemical ingredients and increased the pressure bringing to environment.
From above technical scheme, Diacloden microemulsion cost of the present invention is low, and preparation process is simple, packing instructions are low, reduced the usage amount of organic solvent simultaneously, residual few, environmental pollution is little, and preventive effect is higher than MTI-446 granule, suits large area to popularize.
Embodiment
The embodiment of the invention discloses a kind of dinotefuran micron-emulsion and preparation method thereof.Those skilled in the art can use for reference content herein, suitably improve technological parameter and realize.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the artly, they are all deemed to be included in the present invention.Product of the present invention is described by preferred embodiment, and related personnel obviously can change product as herein described in content of the present invention, spirit and scope or suitably change and combination not departing from, and realizes and apply the technology of the present invention.
In order further to understand the present invention, below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1:5% dinotefuran micron-emulsion
Figure BDA0000104187890000031
MTI-446 is fully mixed with solvent, surfactant, cosolvent, then add water, after fully stirring, can be made into microemulsion.
Embodiment 2: physicochemical property is measured
Get dinotefuran micron-emulsion prepared by embodiment 1 and carry out physicochemical property test, result is as follows:
Outward appearance: as clear as crystal single-phase liquid;
Transparency temperature region: bear 5 ℃ to more than 60 ℃;
Low-temperature stability: do not occur layering, crystallization for 2 weeks at-5 ℃;
Heat storage stability: 2 weeks active ingredient resolution ratios are less than 3% at (54 ± 2) ℃;
Stability of emulsion: with the water-reducible emulsion-stabilizing of any ratio;
Ageing stability: stable under normal temperature.
Embodiment 3: field control effectiveness test
Get dinotefuran micron-emulsion and commercially available certain MTI-446 granule prepared by embodiment 1 and carry out field control effectiveness test.5 processing are established in test, and each formulation rate is in table 1, and every processing repeats for 4 times, and with reference to the Ministry of Agriculture " pesticide field efficacy medicine test criterion ", after dispenser, a borer population of each investigation in 1-3 days, 7 days, adds up and calculate preventive effect and the results are shown in Table 1.Insect population decline rate and control efficiency are calculated by following formula.
Figure BDA0000104187890000041
Figure BDA0000104187890000043
Wherein, PT 0represent the front borer population of living of chemicals treatment district medicine; PT 1borer population alive after expression chemicals treatment district medicine; CK 0represent the front borer population of living of blank district medicine; CK 1borer population alive after expression blank district medicine; PT represents chemicals treatment district insect population decline rate; CK represents blank district insect population decline rate.
Table 1 5% dinotefuran micron-emulsion to rice fulgorid control efficiency (7d)
Figure BDA0000104187890000044
From table 1 result, the drug effect of 5% dinotefuran micron-emulsion 20g/ mu is 71.5%, drug effect significant difference with 1% MTI-446 granule 100g/ mu, both effective ingredient consumption are 1g/ mu, show the good drug efficacy of dinotefuran micron-emulsion of the present invention, need not increase formulation rate and can reach higher preventive effect, alleviate farm chemical ingredients and increased the pressure bringing to environment.
Embodiment 4:10% dinotefuran micron-emulsion
Figure BDA0000104187890000051
MTI-446 is fully mixed with solvent, surfactant, cosolvent, and then add other compositions to mix, then add water, after fully stirring, can be made into microemulsion.Physicochemical property test indices and field control effectiveness test result are similar to embodiment 1.
Embodiment 5:15% dinotefuran micron-emulsion
Figure BDA0000104187890000052
MTI-446 is fully mixed with solvent, surfactant, cosolvent, and then add other compositions to mix, then add water, after fully stirring, can be made into microemulsion.Physicochemical property test indices and field control effectiveness test result are similar to embodiment 1.
Embodiment 6:20% dinotefuran micron-emulsion
Figure BDA0000104187890000061
MTI-446 is fully mixed with solvent, surfactant, cosolvent, and then add other compositions to mix, then add water, after fully stirring, can be made into microemulsion.Physicochemical property test indices and field control effectiveness test result are similar to embodiment 1.
Embodiment 7:25% dinotefuran micron-emulsion
MTI-446 is fully mixed with solvent, surfactant, cosolvent, then add water, after fully stirring, can be made into microemulsion.Physicochemical property test indices and field control effectiveness test result are similar to embodiment 1.
Embodiment 8:30% dinotefuran micron-emulsion
Figure BDA0000104187890000063
MTI-446 is fully mixed with solvent, surfactant, cosolvent, then add water, after fully stirring, can be made into microemulsion.Physicochemical property test indices and field control effectiveness test result are similar to embodiment 1.
Embodiment 9:40% dinotefuran micron-emulsion
Figure BDA0000104187890000071
MTI-446 is fully mixed with solvent, surfactant, cosolvent, and then add other compositions to mix, then add water, after fully stirring, can be made into microemulsion.Physicochemical property test indices and field control effectiveness test result are similar to embodiment 1.
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.

Claims (2)

1. a dinotefuran micron-emulsion, is characterized in that, is made up of the component of following mass percent:
Figure FDA0000421672780000011
2. the preparation method of dinotefuran micron-emulsion described in claim 1, is characterized in that, MTI-446 is fully mixed with cyclohexanone, ethanol, agriculture breast OP-10, agriculture breast 0204C, finally adds water, after fully stirring, can be made into microemulsion.
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CN105145617B (en) * 2015-10-19 2018-06-26 中国农业科学院棉花研究所 A kind of composite synergistic pesticide
CN105532656B (en) * 2016-01-28 2018-05-22 南京善思生物科技有限公司 A kind of environmental-friendly dinotefuran micron-emulsion and preparation method thereof
CN105638650B (en) * 2016-01-28 2018-06-01 南京善思生物科技有限公司 A kind of environmental-friendly dinotefuran micron-emulsion of organic solvent-free and preparation method thereof
CN105746566B (en) * 2016-03-29 2018-09-25 西北农林科技大学 A kind of trunk injection liquor containing dinotefuran
CN106359474A (en) * 2016-08-31 2017-02-01 江苏星源生物科技有限公司 Fungicidal composition for preventing and treating rice planthopper and application thereof
CN109984141A (en) * 2017-12-31 2019-07-09 海南正业中农高科股份有限公司 A kind of microemulsion containing dinotefuran
CN109511671A (en) * 2018-10-19 2019-03-26 江西博邦生物药业有限公司 Pesticide dinotefuran aqua and its preparation method

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CN100450360C (en) * 2006-11-14 2009-01-14 华南理工大学 Rotenone and dinotefuran mixed microemulsion and preparation method thereof
CN102204563A (en) * 2011-04-08 2011-10-05 湖南大方农化有限公司 Pesticide composition containing dinotefuran
CN102217639A (en) * 2011-04-21 2011-10-19 青岛海利尔药业有限公司 Insecticidal composition containing dinotefuran and chlorantraniliprole

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100450360C (en) * 2006-11-14 2009-01-14 华南理工大学 Rotenone and dinotefuran mixed microemulsion and preparation method thereof
CN102204563A (en) * 2011-04-08 2011-10-05 湖南大方农化有限公司 Pesticide composition containing dinotefuran
CN102217639A (en) * 2011-04-21 2011-10-19 青岛海利尔药业有限公司 Insecticidal composition containing dinotefuran and chlorantraniliprole

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