CN102715152B - Indoxacarb microemulsion and preparation method of indoxacarb microemulsion - Google Patents
Indoxacarb microemulsion and preparation method of indoxacarb microemulsion Download PDFInfo
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- CN102715152B CN102715152B CN201210224841.1A CN201210224841A CN102715152B CN 102715152 B CN102715152 B CN 102715152B CN 201210224841 A CN201210224841 A CN 201210224841A CN 102715152 B CN102715152 B CN 102715152B
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- 239000005907 Indoxacarb Substances 0.000 title claims abstract description 62
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- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000593 microemulsion method Methods 0.000 title description 4
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- 238000003756 stirring Methods 0.000 claims description 8
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- 239000000575 pesticide Substances 0.000 abstract description 7
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- 239000004615 ingredient Substances 0.000 abstract description 4
- 229940079593 drug Drugs 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 230000002265 prevention Effects 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
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- 230000003449 preventive effect Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- 241000238631 Hexapoda Species 0.000 description 8
- 150000001450 anions Chemical class 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 8
- -1 polyoxyethylene Polymers 0.000 description 8
- 239000004094 surface-active agent Substances 0.000 description 8
- 239000004480 active ingredient Substances 0.000 description 7
- 238000009472 formulation Methods 0.000 description 7
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- 239000000203 mixture Substances 0.000 description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 6
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000000361 pesticidal effect Effects 0.000 description 5
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 4
- 241001147381 Helicoverpa armigera Species 0.000 description 4
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- 125000002877 alkyl aryl group Chemical group 0.000 description 4
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- 125000002243 cyclohexanonyl group Chemical group *C1(*)C(=O)C(*)(*)C(*)(*)C(*)(*)C1(*)* 0.000 description 2
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- Agricultural Chemicals And Associated Chemicals (AREA)
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Abstract
The invention relates to the field of pesticide preparation and discloses an indoxacarb microemulsion and a preparation method of the indoxacarb microemulsion. The indoxacarb microemulsion provided by the invention comprises the following ingredients in percentage by weight (accounting for the total weight of the microemulsion): 1 to 30 percent of indoxacarb, 10 to 20 percent of solvents, 10 to 30 percent of emulsifying agents, 0.5 to 10 percent of cosolvents and the balance water. The indoxacarb microemulsion provided by the invention has the advantages that the cost is low, the preparation process is simple, the package requirement is low, meanwhile, the consumption of organic solvents is reduced, the residue is little, the environment pollution is little, in addition, the prevention effect is higher than that of indoxacarb water dispersible granules, the medication quantity can be reduced, and the indoxacarb microemulsion is suitable for large-area popularization.
Description
Technical field
The present invention relates to pesticidal preparations field, relate to specifically a kind of indoxacarb microemulsion and preparation method thereof.
Background technology
Indoxacarb (Indoxacarb); chemical name is 7-chloro-2; 5-dihydro-2-[N-(methoxy methyl acyl group)-4-(trifluoromethoxy) aniline formyl] indeno [1,2-e] [1,3; 4] oxadiazines-4a (3H)-methyl formate; be the oxadiazines class sodium channel blockers that du pont company develops and develops, have and tag and stomach poison function, by the sodium-ion channel in blocking-up insect nerve cell; make nerve cell loss of function, almost all effective to all lepidoptera pests.Medicament enters in insect bodies by contacting and taking food, and in 0-4 hour, insect stops taking food, and is benumbed immediately, and the coordination ability of insect can decline (can cause larva to fall from crop), generally dead in 24-60 hour after medicine.Be applicable to prevent and treat the insects such as beet armyworm on the crops such as wild cabbage, flower coconut palm class, cabbage mustard, tomato, capsicum, cucumber, little cucumber, eggplant, lettuce, apple, pears, peach, apricot, cotton, potato, grape, diamond-back moth, cabbage caterpillar, prodenia litura, tomato moth, cotton bollworm, oriental tobacco budworm, leaf rollers, codling moth, leafhopper, spark, colorado potato beetle.
The formulation of the indoxacarb pesticide product of applying on pesticide market at present mainly be take water dispersible granules as main, yet if the preventive effect of indoxacarb water dispersible granules wants the level that reaches higher just need to increase formulation rate, this can cause very large pressure to environment.
Simultaneously, raising along with people's environmental consciousness, restriction increasingly stringent to 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, the pesticides new formulation that the water of wherein take is matrix has become the direction of world pesticide dosage form research and development.
Microemulsion (microemulsion, ME) is to 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 research and develop a kind of efficient, low toxicity, environment amenable indoxacarb pest killing micro emulsion is 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 indoxacarb microemulsion of formulation rate.
For realizing object of the present invention, the present invention adopts following technical scheme:
A kind of indoxacarb microemulsion, comprise indoxacarb, solvent, emulsifier, cosolvent and water, wherein, the percentage by weight that each component accounts for described microemulsion gross weight is indoxacarb 1-30%, solvent 10-20%, emulsifier 10-30%, cosolvent 0.5-10%, and surplus is water; Described solvent is cyclohexanone, toluene, dimethylbenzene or methyl alcohol; Described emulsifier 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, styrylphenol polyoxyethylene ether, alkylaryl polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene; Described cosolvent is selected from C
1-C
4alcohols.
Indoxacarb microemulsion of the present invention be take indoxacarb as active component, as preferably, the percentage by weight that described indoxacarb accounts for described microemulsion gross weight is 10-30%, described emulsifier percentage by weight is 20-25%, described cosolvent percentage by weight is 3-7%, and described solvent weight percent is 12-15%.
In the present invention, the compound of described anion and non-ionic surface active agent is preferably agriculture breast 0201B or agriculture breast 0204C, the compound of described anion and non-ionic surface active agent and solvent is preferably agriculture breast 0203B or agriculture breast 2201, described alkylphenol polyoxyethylene is preferably OPEO (OP series emulsifier) or polyoxyethylene nonylphenol ether (NP series emulsifier), and described polyoxyethylene nonylphenol ether (NP series emulsifier) is preferably emulsifier NP-10-P; Described alkylaryl polyoxyethylene polyoxypropylene ether is preferably No. 33, agriculture breast.As most preferred technique scheme, emulsifier of the present invention is No. 33, agriculture breast and emulsifier NP-10-P.
C of the present invention
1-C
4alcohols be preferably methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol or n-butanol, more preferably ethanol or n-butanol, most preferably be n-butanol.
Solvent of the present invention is preferably cyclohexanone.
The present invention also provides the preparation method of described indoxacarb microemulsion, by weight percentage, 1-30% indoxacarb is dissolved with 10-20% solvent and 0.5-10% cosolvent, then add 10-30% emulsifier to mix, finally add water to mend to 100%, after fully stirring, can be made into microemulsion;
Wherein, described solvent is cyclohexanone, toluene, dimethylbenzene or methyl alcohol; Described emulsifier 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, styrylphenol polyoxyethylene ether, alkylaryl polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene; Described cosolvent is selected from C
1-C
4alcohols.
As preferably, the percentage by weight of described indoxacarb is 10-30%, and described emulsifier percentage by weight is 20-25%, and described cosolvent percentage by weight is 3-7%, and described solvent weight percent is 12-15%.
In preparation process, the compound of described anion and non-ionic surface active agent is preferably agriculture breast 0201B or agriculture breast 0204C, the compound of described anion and non-ionic surface active agent and solvent is preferably agriculture breast 0203B or agriculture breast 2201, described alkylphenol polyoxyethylene is preferably OPEO (OP series emulsifier) or polyoxyethylene nonylphenol ether (NP series emulsifier), and described polyoxyethylene nonylphenol ether (NP series emulsifier) is preferably emulsifier NP-10-P; Described alkylaryl polyoxyethylene polyoxypropylene ether is preferably No. 33, agriculture breast.As most preferred technique scheme, emulsifier of the present invention is No. 33, agriculture breast and emulsifier NP-10-P.
C of the present invention
1-C
4alcohols be preferably methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol or n-butanol, more preferably ethanol or n-butanol, most preferably be n-butanol.
Solvent of the present invention is preferably cyclohexanone.
Physicochemical property and field control effectiveness test result show, indoxacarb microemulsion of the present invention stable performance, transparent wide ranges, resolution ratio are low, cotton bollworm is had to significant drug effect, and compare with the indoxacarb water dispersible granules of same dose (in active component), preventive effect is apparently higher than the preventive effect of water dispersible granules.Show that indoxacarb microemulsion 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, indoxacarb microemulsion cost of the present invention is low, and preparation process is simple, and packing instructions are low, reduced the usage amount of organic solvent, residual few, environmental pollution is little simultaneously, and preventive effect, higher than indoxacarb water dispersible granules, can reduce formulation rate, suits large area to popularize.
Embodiment
The embodiment of the invention discloses a kind of indoxacarb microemulsion 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 or suitably change and combination within not departing from content of the present invention, spirit and scope, 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% indoxacarb microemulsion
Indoxacarb is dissolved with solvent cyclohexanone and cosolvent n-butanol, then add agriculture breast to mix with emulsifier NP-10-P for No. 33, finally add distilled water, after fully stirring, can be made into microemulsion.
Get indoxacarb microemulsion prepared by the present embodiment 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 2:30% indoxacarb microemulsion
Indoxacarb is dissolved with solvent methanol and cosolvent ethanol, then add agriculture breast 0201B to mix, finally add distilled water, after fully stirring, can be made into microemulsion.
Get indoxacarb microemulsion prepared by the present embodiment 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 3:10% indoxacarb microemulsion
Indoxacarb is dissolved with solvent xylene and cosolvent propyl alcohol, then add agriculture breast to mix with agricultural emulsifier NO．600 for No. 500, finally add distilled water, after fully stirring, can be made into microemulsion.
Get indoxacarb microemulsion prepared by the present embodiment 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 4:15% indoxacarb microemulsion
Indoxacarb is dissolved with solvent toluene and cosolvent isopropyl alcohol, then add agriculture breast OP-10 and agriculture breast OP-7 to mix, finally add distilled water, after fully stirring, can be made into microemulsion.
Get indoxacarb microemulsion prepared by the present embodiment 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 5:20% indoxacarb microemulsion
Indoxacarb is dissolved with solvent xylene and cosolvent n-butanol, then add agriculture breast 0203B to mix, finally add distilled water, after fully stirring, can be made into microemulsion.
Get indoxacarb microemulsion prepared by the present embodiment 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 6:25% indoxacarb microemulsion
Indoxacarb is dissolved with solvent methanol and the cosolvent tert-butyl alcohol, then add agriculture breast 0204C and agriculture breast 2201 to mix, finally add distilled water, after fully stirring, can be made into microemulsion.
Get indoxacarb microemulsion prepared by the present embodiment 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 7: field control effectiveness test
Get indoxacarb microemulsion and commercially available certain indoxacarb water dispersible granules prepared by each embodiment and carry out the Helicoverpa armigera test of pesticide effectiveness.Test repeats 4 Ci， community area 30m
2, community randomized arrangement.With reference to the < < of Ministry of Agriculture pesticide field efficacy medicine test criterion > >, within after dispenser 5 days, 10 days, 15 days, respectively investigate borer population one time, add 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.
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 indoxacarb microemulsion to cotton bollworm control efficiency
| Reagent agent | Effective ingredient consumption (g/ mu) | Average preventive effect (%) | The significance of difference (F 0.05) |
| Embodiment 1 microemulsion | 40 | 89.8 | a |
| Embodiment 2 microemulsions | 40 | 85.6 | b |
| Embodiment 3 microemulsions | 40 | 84.1 | b |
| Embodiment 4 microemulsions | 40 | 84.3 | b |
| Embodiment 5 microemulsions | 40 | 83.7 | b |
| Embodiment 6 microemulsions | 40 | 85.2 | b |
| 30% indoxacarb water dispersible granules | 40 | 80.3 | c |
| CK | 0 | d |
From table 1 result, in indoxacarb active ingredient, be under the prerequisite of 40g/ mu, there were significant differences for the preventive effect of the preventive effect of indoxacarb microemulsion of the present invention and commercially available certain 30% indoxacarb water dispersible granules, and the preventive effect of the most preferred technical scheme of the present invention (embodiment 1) and the preventive effect of other all indoxacarb medicaments there were significant differences, result of the test shows the good drug efficacy of indoxacarb microemulsion 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.
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. an indoxacarb microemulsion, is characterized in that, comprising:
2. the preparation method of an indoxacarb microemulsion claimed in claim 1, it is characterized in that, indoxacarb is dissolved with solvent cyclohexanone and cosolvent n-butanol, then add agriculture breast to mix with emulsifier NP-10-P for No. 33, finally add distilled water, after fully stirring, can be made into microemulsion.
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| EP3177141A4 (en) * | 2014-08-05 | 2018-01-03 | Dow Global Technologies LLC | Emulsifiable concentrates of indoxacarb |
| CN106259406B (en) * | 2016-08-03 | 2017-08-29 | 顾爱国 | A kind of microemulsion containing indoxacarb and HEXAFLUMURON |
| CN113940356A (en) * | 2021-07-08 | 2022-01-18 | 安徽广信农化股份有限公司 | Indoxacarb microemulsion and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101589723A (en) * | 2009-06-30 | 2009-12-02 | 江苏省绿盾植保农药实验有限公司 | Indenes worm prestige and pyridaphethione compounded pesticides |
| CN101755809A (en) * | 2010-01-12 | 2010-06-30 | 惠州市中迅化工有限公司 | Pesticidal composition containing indoxacarb and metaflumizone and application thereof |
| CN101999391A (en) * | 2010-04-16 | 2011-04-06 | 陕西美邦农药有限公司 | Indoxacarb-and-thiacloprid-containing insecticidal composition |
| CN102232383A (en) * | 2010-04-25 | 2011-11-09 | 青岛凯源祥化工有限公司 | Pesticidal composition containing spirotetramat and indoxacarb |
| CN102415394A (en) * | 2011-12-06 | 2012-04-18 | 海利尔药业集团股份有限公司 | Indoxacarb-containing high-efficiency pesticidal composition |
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2012
- 2012-06-29 CN CN201210224841.1A patent/CN102715152B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101589723A (en) * | 2009-06-30 | 2009-12-02 | 江苏省绿盾植保农药实验有限公司 | Indenes worm prestige and pyridaphethione compounded pesticides |
| CN101755809A (en) * | 2010-01-12 | 2010-06-30 | 惠州市中迅化工有限公司 | Pesticidal composition containing indoxacarb and metaflumizone and application thereof |
| CN101999391A (en) * | 2010-04-16 | 2011-04-06 | 陕西美邦农药有限公司 | Indoxacarb-and-thiacloprid-containing insecticidal composition |
| CN102232383A (en) * | 2010-04-25 | 2011-11-09 | 青岛凯源祥化工有限公司 | Pesticidal composition containing spirotetramat and indoxacarb |
| CN102415394A (en) * | 2011-12-06 | 2012-04-18 | 海利尔药业集团股份有限公司 | Indoxacarb-containing high-efficiency pesticidal composition |
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