CN103210933A - Bispyribac-sodium and penoxsulam-containing pesticide microcapsule suspending agent - Google Patents
Bispyribac-sodium and penoxsulam-containing pesticide microcapsule suspending agent Download PDFInfo
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- CN103210933A CN103210933A CN2013100945618A CN201310094561A CN103210933A CN 103210933 A CN103210933 A CN 103210933A CN 2013100945618 A CN2013100945618 A CN 2013100945618A CN 201310094561 A CN201310094561 A CN 201310094561A CN 103210933 A CN103210933 A CN 103210933A
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Abstract
The invention discloses a bispyribac-sodium and penoxsulam-containing pesticide microcapsule suspending agent, including 1%-30% of bispyribac-sodium and penoxsulam, wherein the parts by weight of bispyribac-sodium and penoxsulam are 10:1-1:10, 3%-20% of a capsule core solvent, 5%-20% of a capsule wall material, 3%-10% of an emulsifier, 1%-5% of a dispersant, and 0.1%-10% of a pH adjusting agent, the balance being deionized water. The invention is applicable to controlling annual weeds in paddy fields. The microcapsule suspending agent has obvious synergies for prevention of annual weeds in paddy fields than a single dose, and helps to reduce use amount and pesticide costs, extend the service life of the pesticide, and reduce adverse effects of the pesticide on the ecological environment.
Description
Technical field
The composition pesticide micro-capsule suspension that the present invention relates to is to be active ingredient with two careless ethers and penoxsuam, is used to prevent and kill off farmland weed, is particularly useful for preventing and kill off paddy field annual weed etc.
Background technology
Two careless ethers, English common name bispyribac-sodium, the genus benzoic acid derivative, this product absorbs by the root leaf and suppresses sour synthesizing of vinegar milk and hindered aminoacid biosynthesis side chain.Be selective herbicide, can effectively prevent and kill off barnyard grass in paddy field and other grassy weeds, double most of broad leaved weeds, some sedge weeds and the resistance barnyard grass grass controlled.
Penoxsuam, English common name penoxsulam, the sulfanilamide (SN) carbamide herbicides is translocated herbicide, absorbs through cauline leaf, young shoot and root system, conduct to meristematic tissue by xylem and phloem, suppress plant strain growth, make the growing point chlorosis, handle back 7 ~ 14d terminal bud and redden, necrosis, 2 ~ 4 all plant death; This agent is strong inhibitor of acetolactate synthetase, and medicament presents slower, needs the certain hour weeds just dead gradually.Can be used for preventing and kill off barnyard grass in paddy field and annual sedge weed, and effective to multiple broad leaved weed.
The pesticide micro capsule suspending agent is to utilize the capsule-core that microencapsulation technology will contain former medicine to be encapsulated in the suspending agent that forms fine particle in the special cyst material, and the capsule diameter of agricultural chemicals microcapsule suspending agent is generally 1～20 μ m.The agricultural chemicals microcapsule suspending agent is compared following advantage with conventional dosage forms: prolonged the lasting period of agricultural chemicals, the stability that has improved active component, active substance be wrapped in improved in the cyst wall safety, effectively reduce former medicine composition to the stimulus to the sense organ of human body, reduce poisoning, help the composite, friendly more of agricultural chemicals environment to crop.
Being mixed of different pesticide species is the common methods of preventing and kill off agriculture resistance disease pest and weed.By the formulation of pesticide screening, filter out rational prescription, can effectively improve actual preventive effect, reduce dosage, reduce cost, delay the drug-fast generation of disease pest and weed, be the important means that agricultural synthesis is administered.The inventor furthers investigate the prescription screening of two careless ethers and penoxsuam, find that two careless ethers and penoxsuam are mixed, in certain mixed ratio scope weeds there are certain synergy or summation action, can prevent and kill off the paddy field annual weed effectively.
But the duration of the present weed killer herbicide kind weeding of using is too short, causes the frequent medication of peasant and improves constantly dosing, and many areas have all caused drug-fast generation, and the lasting period that for this reason prolongs this medicament becomes the problem that needs to be resolved hurrily.In addition, the formulation of two careless ethers and penoxsuam use at present is still based on missible oil, pulvis, water dispersible granules.The organic solvent that missible oil consumption is a large amount of, pulvis exists big for environment pollution, and there are shortcomings such as power consumption of polymer processing height in water dispersible granules, and also appears in the newspapers at the end about two careless ethers and penoxsuam micro-capsule suspension.Therefore, research and development and the good environment friendly agricultural preparation of Environmental compatibility both can be brought into play its effectiveness to greatest extent, prolonged its operating period, overcame pesticide resistance, can save substantial contribution and labour again.
Summary of the invention
The objective of the invention is to solve in the prior art develop immunity to drugs problem and promote drug effect of farmland weed, a kind of efficient, low toxicity, environmental protection are provided, help the micro-capsule suspension of the farmland weed comprehensive regulation.
Another object of the present invention provides this composition pesticide is used to prevent and kill off farmland weed, is particularly useful for preventing and kill off paddy field annual weed etc.
The present invention is achieved by the following technical solutions:
A kind of pesticide micro capsule suspending agent that contains two careless ethers and penoxsuam, the ratio of weight and number of wherein two careless ethers and penoxsuam is 10:1～1:10.
Preferably, form by following components in weight percentage: two careless ethers and penoxsuam 1%～30%, capsule-core solvent 3%～20%, cyst material 5%～30%, emulsifier 3%～10%, dispersant 1%～5%, pH regulator agent 0.1%～10%, surplus is a deionized water.
Wherein said capsule-core solvent is one or more among dimethylbenzene, cyclohexanone, ethyl acetate, N-Methyl pyrrolidone, diethyl phthalate, dibutyl phthalate, Solvesso100, Solvesso150, the Solvesso200.
Described cyst material is the urea resin prepolymer aqueous solution, is to be mixed with weight ratio 1:1～1:2.5 by urea and formaldehyde, obtains by polycondensation reaction.
Described emulsifier is one or more in alkylphenol polyoxyethylene, styryl phenol polyethenoxy ether, alkaryl phenol polyethenoxy ether phosphate, castor oil polyoxyethylene ether, alkylbenzenesulfonate, alkylphenol-polyethenoxy phosphate, maleic acid di-sec-octyl sodium sulfonate, polyol fatty acid ester and the ethylene oxide adduct thereof.
Described dispersant is one or more in SOPA-270, dispersant NNO, sodium lignin sulfonate, the dispersant 2700.
Described pH regulator agent is sodium hydroxide or watery hydrochloric acid.
Described a kind of preparation method who contains the pesticide micro capsule suspending agent of two careless ethers and penoxsuam:
(1) urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:1～1:2.5, regulating the pH value with sodium hydroxide is 8～9, under 60～80 ℃ of conditions of temperature, stirring at low speed, insulation reaction 0.5～4 hour, generate the transparent Lauxite of thickness, the deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution.
(2) at normal temperatures two careless ethers and penoxsuam are dissolved in the capsule-core solvent fully, when stirring, add a certain amount of urea resin prepolymer aqueous solution,, obtain stable O/W emulsion with 1000～2000 rev/mins of rotating speed cutting 10～20 minutes.
(3) reduce the rotating speed of shearing, adding watery hydrochloric acid in batches and regulate the pH value in 1 hour is 3.0, polycondensation reaction takes place, progressively be warming up to 40～60 ℃ and solidify cyst wall, reacting after 1.5～2 hours cyst wall solidifies and finishes, add sodium hydroxide again and regulate pH value to 6.0～8.0, add an amount of emulsifier, dispersant, deionized water complements to 100%.With 2000～6000 rev/mins of rotating speed high shears 10～60 minutes, promptly obtain containing the micro-capsule suspension of two careless ethers and penoxsuam composition pesticide again.
In the cyst wall solidify reaction process, every sampling in 15 minutes 1 time, use the capsule process of each stage of reaction of microscopic examination, use the pH value of pH meter monitoring reaction course.
The micro-capsule suspension of described composition pesticide is mainly used in prevents and kill off the paddy field annual weed.
Compared with prior art, the invention has the advantages that:
1, two kinds of active ingredients are mixed and have obvious synergistic effect, have improved preventive effect, have reduced the agricultural chemicals usage amount, have reduced cost and to the pollution of environment.
2, the combination of two kinds of active ingredients has enlarged herbicidal spectrum, and two kinds of active ingredient mechanism of action differences can overcome the shortcoming that single agent is easy to generate resistance simultaneously, prolongs the service life of medicament.The application of composition can delay or overcome the drug-fast generation of rice weed, helps agricultural synthesis and administers.Enlarged and prevented and kill off spectrum.
3, composition pesticide micro-capsule suspension provided by the invention, to crop safety, the lasting period is long, and environment is not had pressure.
Embodiment
The present invention describes by following specific embodiment, but the invention is not restricted to following specific embodiment.In these embodiments, unless otherwise indicated, all percentages all are weight percentage.
Biologicall test embodiment 1:
Be mixed to the synergy of weeds for further understanding two careless ethers and penoxsuam, the inventor is mixed to two careless ethers and penoxsuam and has carried out formulation screening test:
Test material: chickweed [
Stellaria media(L.) Cyrillus] (field is collected seed and is preserved).The barnyard grass grass [
Echinochloa crusgalli(L.) Beaw Setaria] (field is collected seed and is preserved).
Test apparatus: controlled illumination box; The accurate laboratory of POTTER spray tower; Electronic balance (sensibility reciprocal 0.1mg); Micropipette rifle etc.
Test method:
Take by weighing 93% pair of former medicine of careless ether of certain mass earlier, the former medicine of 98% penoxsuam, the Tween 80 aqueous solution with 0.1% after adding acetone fully dissolves dilutes, and is mixed with single agent mother liquor respectively, according to the purpose that is mixed serial proportioning is set, each proportioning is provided with 5～7 concentration gradients.Kill the grass spectrum according to single agent and select representative susceptible weeds seed, it is standby to be cultured to 2 leaves, 1 stamen.After the weeds cauline leaf of selecting numbering handled, be placed in the illumination box incubated at room temperature 5 days, calculate preventive effect (fresh weight), then with method of least squares calculate suppress in dense EC
50(95% confidence limit) calculates co-toxicity coefficient (CTC) with the abundant method of Sun Yun again.
Co-toxicity coefficient (CTC) 〉=120 shows as synergistic effect; Co-toxicity coefficient (CTC)≤80 shows as antagonism; 80＜co-toxicity coefficient (CTC)＜120 shows as summation action.
Actual measurement toxicity index (ATI)=(standard medicament EC
50/ reagent agent EC
50) * 100.
Theoretical toxicity index (TTI)=(percentage composition of A in toxicity index * mixture of A)+(B
Toxicity index * mixture in the percentage composition of B).
Co-toxicity coefficient (CTC)=[mixture actual measurement toxicity index (the ATI)/theoretical toxicity index (TTI) of mixture] * 100.
Measurement result shows that two careless ethers and penoxsuam are between 10:1～1:10 at ratio of weight and number, and co-toxicity coefficient has obvious synergistic effect more than 120.
Table 1, the two careless ethers of different proportioning and penoxsuam are measured the synergy of barnyard grass grass.
Table 2, the two careless ethers of different proportioning and penoxsuam are measured the synergy of chickweed.
Example of formulations 1: 11% pair of careless ether penoxsuam micro-capsule suspension.
Following material all is weight percentage: at normal temperatures with two careless ethers 10%, penoxsuam 1.0% is dissolved in 10% N-Methyl pyrrolidone fully, adds the 10% urea resin prepolymer aqueous solution while stirring, with 2000 rev/mins of rotating speed cutting 10～20 minutes, obtain stable O/W emulsion.Reduce rotating speed to 1000 rev/min, 5 batches of branches added watery hydrochloric acid adjusting pH value in 1 hour be 3.0, polycondensation reaction takes place, progressively be warming up to 45 ℃ and solidified cyst wall 1.5 hours, add sodium hydroxide again and regulate pH value to 6.5, add emulsifier alkylphenol polyoxyethylene 4%, alkylbenzenesulfonate 1.5%, dispersant SOPA-2700 1.5%, complement to 100% with deionized water.With 4000 rev/mins of rotating speed high shears 15 minutes, promptly obtain 11% pair of careless ether penoxsuam micro-capsule suspension again.
This embodiment is used to prevent and kill off the paddy field annual weed, and 11% pair of careless ether penoxsuam micro-capsule suspension consumption 15 gram/mu is converted water spray, and 30 days preventive effects are 90.6% behind the medicine.Contrast 11% pair of careless ether suspending agent consumption 20 gram/mu of single agent and convert 45 kilograms of sprayings of water, 30 days preventive effects are 81.3% behind the medicine.Contrast single agent 11% penoxsuam oil-suspending agent consumption 80 gram/mus and convert 45 kilograms of sprayings of water, 30 days preventive effects are 84.7% behind the medicine.
11% pair of careless ether penoxsuam micro-capsule suspension is prevented and kill off paddy field annual weed effect significantly better than contrast 11% pair of careless ether suspending agent of single agent and 11% penoxsuam oil-suspending agent, illustrate that the present invention can prevent and kill off the paddy field annual weed preferably, reduce dosage, reduce cost, delay the drug-fast generation of weeds, reduced environmental pollution.
Example of formulations 2: 24% pair of careless ether penoxsuam micro-capsule suspension.
Following material all is weight percentage: at normal temperatures with two careless ethers 4%, penoxsuam 20%, be dissolved in 10% fully, in the cyclohexanone, 5% ethyl acetate, add the 10% urea resin prepolymer aqueous solution while stirring, with 2000 rev/mins of rotating speed cutting 10～20 minutes, obtain stable O/W emulsion.Reduce rotating speed to 1000 rev/min, 5 batches of branches added watery hydrochloric acid adjusting pH value in 1 hour be 3.0, polycondensation reaction takes place, progressively be warming up to 45 ℃ and solidified cyst wall 1.5 hours, add sodium hydroxide again and regulate pH value to 7.0, add emulsifier alkylphenol polyoxyethylene 4%, alkylbenzenesulfonate 1.5%, dispersant SOPA-2700 1.5%, complement to 100% with deionized water.With 4000 rev/mins of rotating speed high shears 15 minutes, promptly obtain 24% pair of careless ether penoxsuam micro-capsule suspension again.
This embodiment is used to prevent and kill off the paddy field annual weed, and 24% pair of careless ether penoxsuam micro-capsule suspension preparation consumption 15 gram/mu is converted 45 kilograms of sprayings of water, and 30 days preventive effects are 93.3% behind the medicine.Contrast 24% pair of careless ether suspending agent preparation consumption 20 gram/mu of single agent and convert 45 kilograms of sprayings of water, 30 days preventive effects are 81.3% behind the medicine.Contrast single agent 24% penoxsuam oil-suspending agent preparation consumption 80 gram/mus and convert 45 kilograms of sprayings of water, 30 days preventive effects are 80.7% behind the medicine.
24% pair of careless ether penoxsuam micro-capsule suspension is prevented and kill off paddy field annual weed effect significantly better than contrast 24% pair of careless ether suspending agent of single agent and 24% penoxsuam oil-suspending agent, illustrate that two careless ethers of the present invention and penoxsulam amine composition can prevent and kill off the paddy field annual weed preferably, reduce dosage, reduce cost, delay the drug-fast generation of weeds, reduced environmental pollution.
Example of formulations 3: 30% pair of careless ether penoxsuam micro-capsule suspension.
Following material all is weight percentage: at normal temperatures with two careless ethers 20%, penoxsuam 10%, be dissolved in 10% fully, in the cyclohexanone, 10% N-Methyl pyrrolidone, add the 25% urea resin prepolymer aqueous solution while stirring, with 1500 rev/mins of rotating speed cutting 10～20 minutes, obtain stable O/W emulsion.Reduce rotating speed to 800 rev/min, 5 batches of branches added watery hydrochloric acid adjusting pH value in 1 hour be 3.0, polycondensation reaction takes place, progressively be warming up to 50 ℃ and solidified cyst wall 1.5 hours, add sodium hydroxide again and regulate pH value to 7.5, add emulsifier castor oil polyoxyethylene ether 3%, maleic acid di-sec-octyl sodium sulfonate 4%, alkylbenzenesulfonate 1.5%, dispersant NNO 1%, complement to 100% with deionized water.With 5000 rev/mins of rotating speed high shears 15 minutes, promptly obtain 30% pair of careless ether penoxsuam micro-capsule suspension again.
This embodiment is used to prevent and kill off the paddy field annual weed, and 30% pair of careless ether penoxsuam micro-capsule suspension preparation consumption 25 gram/mu is converted 45 kilograms of sprayings of water, and 30 days preventive effects are 87.2% behind the medicine.Contrast 30% pair of careless ether suspending agent preparation consumption 20 gram/mu of single agent and convert 45 kilograms of sprayings of water, 30 days preventive effects are 80.3% behind the medicine.Contrast single agent 30% penoxsuam oil-suspending agent preparation consumption 80 gram/mus and convert 45 kilograms of sprayings of water, 30 days preventive effects are 78.7% behind the medicine.
30% pair of careless ether penoxsuam micro-capsule suspension is prevented and kill off paddy field annual weed effect significantly better than contrast 30% pair of careless ether suspending agent of single agent and 30% penoxsuam oil-suspending agent, illustrate that two careless ethers of the present invention and penoxsulam amine composition can prevent and kill off the paddy field annual weed preferably, reduce dosage, reduce cost, delay the drug-fast generation of weeds, reduced environmental pollution.
Claims (4)
1. pesticide micro capsule suspending agent that contains two careless ethers and penoxsuam, it is characterized in that: the ratio of weight and number of two careless ethers and penoxsuam is 10:1～1:10.
2. the described a kind of pesticide micro capsule suspending agent that contains two careless ethers and penoxsuam of claim 1, it is characterized in that: described micro-capsule suspension is made up of following components in weight percentage: two careless ethers and penoxsuam 1%～30%, capsule-core solvent 3%～20%, cyst material 5%～30%, emulsifier 3%～10%, dispersant 1%～5%, pH regulator agent 0.1%～10%, surplus are deionized water;
Wherein said capsule-core solvent is one or more among dimethylbenzene, cyclohexanone, ethyl acetate, N-Methyl pyrrolidone, diethyl phthalate, dibutyl phthalate, Solvesso100, Solvesso150, the Solvesso200;
Described cyst material is the urea resin prepolymer aqueous solution, is to be mixed with weight ratio 1:1～1:2.5 by urea and formaldehyde, obtains by polycondensation reaction;
Described emulsifier is one or more in alkylphenol polyoxyethylene, styryl phenol polyethenoxy ether, alkaryl phenol polyethenoxy ether phosphate, castor oil polyoxyethylene ether, alkylbenzenesulfonate, alkylphenol-polyethenoxy phosphate, maleic acid di-sec-octyl sodium sulfonate, polyol fatty acid ester and the ethylene oxide adduct thereof;
Described dispersant is one or more in SOPA-270, dispersant NNO, sodium lignin sulfonate, the dispersant 2700;
Described pH regulator agent is sodium hydroxide or watery hydrochloric acid.
3. preparation method who contains the pesticide micro capsule suspending agent of two careless ethers and penoxsuam is characterized in that may further comprise the steps:
(1) urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:1～1:2.5, regulating the pH value with sodium hydroxide is 8～9, under 60～80 ℃ of conditions of temperature, stirring at low speed, insulation reaction 0.5～4 hour, generate the transparent Lauxite of thickness, the deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution;
(2) at normal temperatures two careless ethers and penoxsuam are dissolved in the capsule-core solvent fully, when stirring, add a certain amount of urea resin prepolymer aqueous solution,, obtain stable O/W emulsion with 1000～2000 rev/mins of rotating speed cutting 10～20 minutes;
(3) reduce the rotating speed of shearing, adding watery hydrochloric acid in batches and regulate the pH value in 1 hour is 3.0, polycondensation reaction takes place, progressively be warming up to 40～60 ℃ and solidify cyst wall, reacting after 1.5～2 hours cyst wall solidifies and finishes, add sodium hydroxide again and regulate pH value to 6.0～8.0, add an amount of emulsifier, dispersant, deionized water complements to 100%;
With 2000～6000 rev/mins of rotating speed high shears 10～60 minutes, promptly obtain containing the micro-capsule suspension of two careless ethers and penoxsuam composition pesticide again;
In the cyst wall solidify reaction process, every sampling in 15 minutes 1 time, use the capsule process of each stage of reaction of microscopic examination, use the pH value of pH meter monitoring reaction course.
4. the described a kind of pesticide micro capsule suspending agent that contains two careless ethers and penoxsuam of claim 1 is characterized in that being applicable to and prevents and kill off the paddy field annual weed.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104488914A (en) * | 2014-11-20 | 2015-04-08 | 江苏省激素研究所股份有限公司 | Complex herbicide for rice field |
| CN106508925A (en) * | 2016-11-08 | 2017-03-22 | 广东中迅农科股份有限公司 | A weeding composition containing penoxsulam, bispyribac sodium and pretilachlor |
| CN106998687A (en) * | 2014-12-16 | 2017-08-01 | 美国陶氏益农公司 | Include the synergistic herbicidal compositions of penoxsuam, Triclopyr and double phonetic benzoic acid |
| WO2022023912A1 (en) * | 2020-07-25 | 2022-02-03 | Coromandel International Limited | Synergistic herbicidal formulations, process for preparing thereof |
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| WO2010093970A2 (en) * | 2009-02-13 | 2010-08-19 | Monsanto Technology Llc | Encapsulation of herbicides to reduce crop injury |
| CN102165956A (en) * | 2011-03-24 | 2011-08-31 | 广东中迅农科股份有限公司 | Pesticide composite containing bispyribac-sodium and penoxsulam and application thereof |
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| CN104488914A (en) * | 2014-11-20 | 2015-04-08 | 江苏省激素研究所股份有限公司 | Complex herbicide for rice field |
| CN106998687A (en) * | 2014-12-16 | 2017-08-01 | 美国陶氏益农公司 | Include the synergistic herbicidal compositions of penoxsuam, Triclopyr and double phonetic benzoic acid |
| CN106508925A (en) * | 2016-11-08 | 2017-03-22 | 广东中迅农科股份有限公司 | A weeding composition containing penoxsulam, bispyribac sodium and pretilachlor |
| WO2022023912A1 (en) * | 2020-07-25 | 2022-02-03 | Coromandel International Limited | Synergistic herbicidal formulations, process for preparing thereof |
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Application publication date: 20130724 |