CN103783050B - A kind of azoles quinoline grass ester water dispersible granules and preparation method thereof - Google Patents
A kind of azoles quinoline grass ester water dispersible granules and preparation method thereof Download PDFInfo
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- CN103783050B CN103783050B CN201410026961.XA CN201410026961A CN103783050B CN 103783050 B CN103783050 B CN 103783050B CN 201410026961 A CN201410026961 A CN 201410026961A CN 103783050 B CN103783050 B CN 103783050B
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Abstract
The present invention relates to field of pesticide preparation, disclose a kind of azoles quinoline grass ester water dispersible granules and preparation method thereof.The percentage by weight of each component of azoles quinoline grass ester water dispersible granules of the present invention is azoles quinoline grass ester 10-85%, and wetting agent 2-5%, dispersant 3-10%, disintegrant 1-5%, binding agent 0.5-5%, surplus is carrier.Its preparation method is: accurately take active ingredient by formula rate, auxiliary agent, carrier mix, then by granulation after its ultramicro grinding.Finally by oven dry, screening, the qualified warehouse-in of analytical control.Instant invention overcomes the environmental hazard of missible oil and the shortcoming of pulvis environmental pollution in processing and use procedure, preparation process is simple, is easy to use, and is a main trend of current pesticidal preparations formulation development.
Description
[technical field]
The present invention relates to field of pesticide preparation, be specifically related to a kind of azoles quinoline grass ester water dispersible granules and preparation method thereof.
[background technology]
Azoles quinoline grass ester (pinoxaden) belongs to neophyl pyrazolines weed killer herbicide, molecular formula: C
23h
32n
24, chemical name: 8-(2,6-diethyl-4-aminomethyl phenyl) and-1,2,4,5-tetrahydrochysene-7-oxygen-7H-pyrazoles [1,2-d] [Isosorbide-5-Nitrae, 5] oxygen phenodiazine Zhuo-9-base PA esters.Azoles quinoline grass ester is acetyl-CoA carboxylase inhibitor, and cause fatty acid biosynthesis block, cell division is stopped, cell membrane is destructurized containing fat, causes weeds dead.This weed killer herbicide is mainly used in barley field and prevents and kill off annual gramineous weed, has good preventive effect to wild oat, hard Cao, Wang grass, amur foxtail etc.After general dispenser, 48 hours susceptible weeds stop growing, and in 1 ~ 2 week, grass cutting blade starts jaundice, and in 3 ~ 4 weeks, weeds are thoroughly dead.High to barley safety, (low temperature or high humidity) dispenser under bad climate condition, may there is temporary transient chlorosis symptom in barley leaves, but do not affect the growth of its normal growth and ultimate output.
Azoles quinoline grass ester because of its low toxicity, efficient, environmentally safe, so have broad application prospects.The main formulation of existing product is missible oil, the organic solvent of a great deal of is had in azoles quinoline grass emulsifiable concentrate, these organic solvent flash-points are low, volatile, belong to inflammable and explosive dangerous material, make the storage of solvent and the formulations of pesticide dangerous with transport, once occur revealing, there is very large potential safety hazard, and pollute the environment after the use of missible oil formulation, cause soil compaction, fertility declines, larger to the harm of environment.
Water dispersible granules is a kind of environment-friendly pesticide novel form of the research and development eighties in 20th century, is to grow up on the basis of wetting powder and suspending agent.This formulation, in processing and use procedure, reduces the pollution to environment, and convenient metering, packaging and transport, and reducing peasant's use cost, is a main trend of current Agrochemicals.Therefore research and develop a kind of efficient, cost low, environment amenable azoles quinoline grass ester water dispersible granules to the protection of the development of modern agriculture and environment all tool be of great significance.
[summary of the invention]
The object of the invention is to overcome exist in prior art contaminated environment, be detrimental to health, the high and storage uneasy congruent shortcoming of transport of use cost and a kind of environmental protection, the cost researched and developed azoles quinoline grass ester water dispersible granules low, easy to use.Another object of the present invention is to provide the preparation method of a kind of azoles quinoline grass ester water dispersible granules.
The present invention is achieved by the following technical solutions:
A kind of azoles quinoline grass ester water dispersible granules, its active ingredient is azoles quinoline grass ester, and the percentage that each component accounts for described water dispersible granules gross weight is: azoles quinoline grass ester 10-85%, wetting agent 2-5%, dispersant 3-10%, disintegrant 1-5%, binding agent 0.5-5%, surplus is carrier.
A kind of azoles quinoline grass ester water dispersible granules, the preferred weight ratio of its active ingredient azoles quinoline grass ester is 45-70%.
Described wetting agent is the combination of one or more in alkylbenzenesulfonate, alkylsulfonate, alkyl sulfate, alkylnaphthalene sulfonate, fatty alcohol-polyoxyethylene ether, lauryl sodium sulfate, dialkyl succinylsuccinate sulfonate.
Described dispersant is the combination of one or more in lignosulfonates, naphthalenesulfonate formaldehyde condensation compound, alkylnaphthalene sulfonate formaldehyde condensation products, alkylphenol polyoxyethylene formaldehyde condensation products, alkyl benzene calcium sulfonate, polycarboxylate.
Described disintegrant is one or more in bentonite, urea, modified starch, mineral salt, silica gel, sodium carboxymethylcellulose.
Described binding agent be sucrose, soluble starch, xanthans, carboxymethyl cellulose, polyvinyl alcohol one or more.
Described carrier is one or more in kaolin, diatomite, white carbon, precipitated calcium carbonate, attapulgite, bentonite, starch.
The preparation method of azoles quinoline grass ester water dispersible granules is: after 10-85% azoles quinoline grass ester, 2-5% wetting agent, 3-10% dispersant, 1-5% disintegrant, carrier being mixed in a mixer, through ultra micro air-flow crushing, co-grinding obtains female powder again; Mixed with female powder with after water-soluble solution by 0.5-5% binding agent, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains required azoles quinoline grass ester water dispersible granules.
The azoles quinoline grass content of ester and the choose reasonable of corresponding each auxiliary agent, kind of carrier and proportioning in azoles quinoline grass ester water dispersible granules of the present invention, the present invention is had be uniformly dispersed rapidly, wetability is good, suspensibility is high, disintegration rate is fast and hot storage steady performance, in use consumption is little, weeding usefulness is high, safety good.
[embodiment]
Below in conjunction with embodiment, the present invention is described further, but the present invention is not limited thereto.
Embodiment 1:10% azoles quinoline grass ester water dispersible granules
Azoles quinoline grass ester 10%, sodium alkyl benzene sulfonate 3%, sodium lignin sulfonate 3%, bentonite 5%, sucrose 5%, diatomite 20%, kaolin complements to 100%
Preparation method: accurately take azoles quinoline grass ester, sodium alkyl benzene sulfonate, sodium lignin sulfonate, bentonite, diatomite, kaolin by above-mentioned formula, through ultra micro air-flow crushing after being mixed, co-grinding obtains female powder again.Mix with female powder after fully being dissolved by sucrose water, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains 10% azoles quinoline grass ester water dispersible granules.
Physicochemical property measures: azoles quinoline grass ester content 10.1%, fineness test >=98%(is by 325 mesh sieves), moisture≤2.0%, suspensibility >=90%, persistent foamability (1min)≤10ml, wetability≤1min, pH value 6-8, be uniformly dispersed rapidly, acceleration heat storage stability is qualified, meets the quality and technical index of water dispersible granules.
Application: for preventing and treating cornfield gramineae weed, have good preventive effect to wild oat, hard Cao, Wang grass, amur foxtail, dosage is 45-75 gram of (active ingredient)/hectare, and preventive effect is 80-88%.
Embodiment 2:15% azoles quinoline grass ester water dispersible granules
Azoles quinoline grass ester 15%, fatty alcohol-polyoxyethylene ether 2%, sodium lignin sulfonate 5%, bentonite 5%, soluble starch 4.5%, diatomite 20%, kaolin complements to 100%
Preparation method: accurately take azoles quinoline grass ester, fatty alcohol-polyoxyethylene ether, sodium lignin sulfonate, bentonite, diatomite, kaolin by above-mentioned formula, through ultra micro air-flow crushing after being mixed, co-grinding obtains female powder again.Mix with female powder after fully being dissolved by soluble starch water, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains 15% azoles quinoline grass ester water dispersible granules.
Physicochemical property measures: azoles quinoline grass ester content 15.2%, fineness test >=98%(is by 325 mesh sieves), moisture≤2.0%, suspensibility >=90%, persistent foamability (1min)≤10ml, wetability≤1min, pH value 6-8, be uniformly dispersed rapidly, acceleration heat storage stability is qualified, meets the quality and technical index of water dispersible granules.
Application: for preventing and treating cornfield gramineae weed, have good preventive effect to wild oat, hard Cao, Wang grass, amur foxtail, dosage is 45-75 gram of (active ingredient)/hectare, and preventive effect is 82-90%.
Embodiment 3:30% azoles quinoline grass ester water dispersible granules
Azoles quinoline grass ester 30%, fatty alcohol-polyoxyethylene ether 4%, Negel formaldehyde condensation products 6%, urea 3%, soluble starch 3%, diatomite 15%, kaolin complements to 100%
Preparation method: accurately take azoles quinoline grass ester, fatty alcohol-polyoxyethylene ether, Negel formaldehyde condensation products, urea, diatomite, kaolin by above-mentioned formula, through ultra micro air-flow crushing after being mixed, co-grinding obtains female powder again.Mix with female powder after fully being dissolved by soluble starch water, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains 30% azoles quinoline grass ester water dispersible granules.
Physicochemical property measures: azoles quinoline grass ester content 30.1%, fineness test >=98%(is by 325 mesh sieves), moisture≤2.0%, suspensibility >=90%, persistent foamability (1min)≤10ml, wetability≤1min, pH value 6-8, be uniformly dispersed rapidly, acceleration heat storage stability is qualified, meets the quality and technical index of water dispersible granules.
Application: for preventing and treating cornfield gramineae weed, have good preventive effect to wild oat, hard Cao, Wang grass, amur foxtail, dosage is 45-75 gram of (active ingredient)/hectare, and preventive effect is 85-92%.
Embodiment 4:45% azoles quinoline grass ester water dispersible granules
Azoles quinoline grass ester 45%, Negel 4%, sodium lignin sulfonate 6%, bentonite 3%, polyvinyl alcohol 0.5%, diatomite 10%, kaolin complements to 100%
Preparation method: accurately take azoles quinoline grass ester, Negel, sodium lignin sulfonate, bentonite, diatomite, kaolin by above-mentioned formula, through ultra micro air-flow crushing after being mixed, co-grinding obtains female powder again.Mix with female powder after fully being dissolved by polyvinyl alcohol water, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains 45% azoles quinoline grass ester water dispersible granules.
Physicochemical property measures: azoles quinoline grass ester content 45.2%, fineness test >=98%(is by 325 mesh sieves), moisture≤2.0%, suspensibility >=90%, persistent foamability (1min)≤10ml, wetability≤1min, pH value 6-8, be uniformly dispersed rapidly, acceleration heat storage stability is qualified, meets the quality and technical index of water dispersible granules.
Application: for preventing and treating cornfield gramineae weed, have good preventive effect to wild oat, hard Cao, Wang grass, amur foxtail, dosage is 45-75 gram of (active ingredient)/hectare, and preventive effect is 90-95%.
Embodiment 5:50% azoles quinoline grass ester water dispersible granules
Azoles quinoline grass ester 50%, dialkyl succinylsuccinate sodium sulfonate 3%, alkylphenol polyoxyethylene formaldehyde condensation products 10%, sodium sulphate 2%, polyvinyl alcohol 2%, diatomite 10%, kaolin complements to 100%
Preparation method: accurately take azoles quinoline grass ester, dialkyl succinylsuccinate sodium sulfonate, alkylphenol polyoxyethylene formaldehyde condensation products, sodium sulphate, diatomite, kaolin by above-mentioned formula, through ultra micro air-flow crushing after being mixed, co-grinding obtains female powder again.Mix with female powder after fully being dissolved by polyvinyl alcohol water, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains 50% azoles quinoline grass ester water dispersible granules.
Physicochemical property measures: azoles quinoline grass ester content 50.1%, fineness test >=98%(is by 325 mesh sieves), moisture≤2.0%, suspensibility >=90%, persistent foamability (1min)≤10ml, wetability≤1min, pH value 6-8, be uniformly dispersed rapidly, acceleration heat storage stability is qualified, meets the quality and technical index of water dispersible granules.
Application: for preventing and treating cornfield gramineae weed, have good preventive effect to wild oat, hard Cao, Wang grass, amur foxtail, dosage is 45-75 gram of (active ingredient)/hectare, and preventive effect is 90-97%.
Embodiment 6:70% azoles quinoline grass ester water dispersible granules
Azoles quinoline grass ester 70%, fatty alcohol-polyoxyethylene ether 5%, alkylphenol polyoxyethylene formaldehyde condensation products 8%, ammonium sulfate 3%, carboxymethyl cellulose 0.8%, kaolin complements to 100%
Preparation method: accurately take azoles quinoline grass ester, fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene formaldehyde condensation products, ammonium sulfate, kaolin by above-mentioned formula, through ultra micro air-flow crushing after being mixed, co-grinding obtains female powder again.Mix with female powder after fully being dissolved by carboxymethyl cellulose water, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains 70% azoles quinoline grass ester water dispersible granules.
Physicochemical property measures: azoles quinoline grass ester content 70.1%, fineness test >=98% is by (325 mesh sieve), moisture≤2.0%, suspensibility >=90%, persistent foamability (1min)≤10ml, wetability≤1min, pH value 6-8, be uniformly dispersed rapidly, acceleration heat storage stability is qualified, meets the quality and technical index of water dispersible granules.
Application: for preventing and treating cornfield gramineae weed, have good preventive effect to wild oat, hard Cao, Wang grass, amur foxtail, dosage is 45-75 gram of (active ingredient)/hectare, and preventive effect is 92-98%.
Embodiment 7:80% azoles quinoline grass ester water dispersible granules
Azoles quinoline grass ester 80%, lauryl sodium sulfate 2%, polycarboxylate 6%, urea 3%, carboxymethyl cellulose 0.5%, kaolin complements to 100%
Preparation method: accurately take azoles quinoline grass ester, lauryl sodium sulfate, polycarboxylate, urea, kaolin by above-mentioned formula, through ultra micro air-flow crushing after being mixed, co-grinding obtains female powder again.Mix with female powder after fully being dissolved by carboxymethyl cellulose water, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains 80% azoles quinoline grass ester water dispersible granules.
Physicochemical property measures: azoles quinoline grass ester content 80.2%, fineness test >=98%(is by 325 orders) sieve, moisture≤2.0%, suspensibility >=90%, persistent foamability (1min)≤10ml, wetability≤1min, pH value 6-8, be uniformly dispersed rapidly, acceleration heat storage stability is qualified, meets the quality and technical index of water dispersible granules.
Application: for preventing and treating cornfield gramineae weed, have good preventive effect to wild oat, hard Cao, Wang grass, amur foxtail, dosage is 45-75 gram of (active ingredient)/hectare, and preventive effect is 82-90%.
Embodiment 8:85% azoles quinoline grass ester water dispersible granules
Azoles quinoline grass ester 85%, lauryl sodium sulfate 2.5%, Negel formaldehyde condensation products 4%, urea 1%, carboxymethyl cellulose 0.5%, kaolin complements to 100%
Preparation method: accurately take azoles quinoline grass ester, lauryl sodium sulfate, Negel formaldehyde condensation products, urea, kaolin by above-mentioned formula, through ultra micro air-flow crushing after being mixed, co-grinding obtains female powder again.Mix with female powder after fully being dissolved by carboxymethyl cellulose water, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains 85% azoles quinoline grass ester water dispersible granules.
Physicochemical property measures: azoles quinoline grass ester content 85.1%, fineness test >=98%(is by 325 mesh sieves), moisture≤2.0%, suspensibility >=90%, persistent foamability (1min)≤10ml, wetability≤1min, pH value 6-8, be uniformly dispersed rapidly, acceleration heat storage stability is qualified, meets the quality and technical index of water dispersible granules.
Application: for preventing and treating cornfield gramineae weed, have good preventive effect to wild oat, hard Cao, Wang grass, amur foxtail, dosage is 45-75 gram of (active ingredient)/hectare.Preventive effect is 80-88%.
Embodiment 9: field control effectiveness test
1) profile test: Xiang Zhou district of Xiangyang City of Hubei Province Shuanggou Zhen one barley field is located in experimental field, in dispenser in the morning on March 4 in 2013, dispenser weather on the same day was clear to cloudy, temperature 5-18 DEG C, and gentle breeze is less than three grades.
2) test process: get azoles quinoline grass ester water dispersible granules prepared by each embodiment and carry out barley field control effectiveness test with commercially available azoles quinoline grass emulsifiable concentrate, test establishes 9 to process communities altogether, often processes plot area 20 square metres, the arrangement of random district group.Field main weeds has: wild oat, hard grass, not grass, amur foxtail etc.Add up each weeds strain number before dispenser respectively, be watered 30 ~ 40 kilograms by every mu, secondary dilution, stir, adopt 552 third type sprayer even spraying, within after dispenser 20 days, add up the dead strain number of weeds respectively.Calculate weeds strain preventive effect by following formula:
3) experimental result: in table 1
Table 1: azoles quinoline grass ester water dispersible granules is to the control efficiency of wheat weeds
From table 1 result, under azoles quinoline grass ester active ingredient is the prerequisite of 4g/ mu, the preventive effect of azoles quinoline of the present invention grass ester water dispersible granules is higher than the preventive effect of commercially available azoles quinoline grass emulsifiable concentrate, and preventive effect when the present invention's preferred active ingredient azoles quinoline grass ester weight ratio is 45-70% is higher than the preventive effect of other azoles quinolines grass ester medicaments.This result of the test shows the good drug efficacy of azoles quinoline grass ester water dispersible granules, and consumption is few, and slow down pesticide active ingredient increases the pressure brought to environment, is suitable for the needs of modern agricultural development.
Claims (2)
1. an azoles quinoline grass ester water dispersible granules, is characterized in that: its active ingredient is azoles quinoline grass ester, and the percentage that each component accounts for described water dispersible granules gross weight is azoles quinoline grass ester 45-70%, wetting agent 2-5%, dispersant 3-10%, disintegrant 1-5%, binding agent 0.5-5%, surplus is carrier;
Wherein, described wetting agent is selected from fatty alcohol-polyoxyethylene ether, dialkyl succinylsuccinate sodium sulfonate or Negel;
Described dispersant is selected from alkylphenol polyoxyethylene formaldehyde condensation products or sodium lignin sulfonate;
Described disintegrant is selected from ammonium sulfate, sodium sulphate or bentonite;
Described binding agent is selected from carboxymethyl cellulose or polyvinyl alcohol;
Described carrier is selected from kaolin or diatomite.
2. prepare a method for azoles quinoline grass ester water dispersible granules described in claim 1, it is characterized in that: after azoles quinoline grass ester, wetting agent, dispersant, disintegrant, carrier being mixed in a mixer, through ultra micro air-flow crushing, co-grinding obtains female powder again; Mixed with female powder with after water-soluble solution by binding agent, then carry out extruder grain, dry under 70-80 DEG C of condition, screening, through after the assay was approved, obtains required azoles quinoline grass ester water dispersible granules.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1376032A (en) * | 1999-09-07 | 2002-10-23 | 辛根塔参与股份公司 | Herbicidal composition |
CN101562978A (en) * | 2006-10-27 | 2009-10-21 | 先正达参股股份有限公司 | Herbicidal compositions |
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BR102012027914A2 (en) * | 2011-11-01 | 2016-01-26 | Dow Agrosciences Llc | granules with improved dispersion properties |
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CN1376032A (en) * | 1999-09-07 | 2002-10-23 | 辛根塔参与股份公司 | Herbicidal composition |
CN101562978A (en) * | 2006-10-27 | 2009-10-21 | 先正达参股股份有限公司 | Herbicidal compositions |
Non-Patent Citations (1)
Title |
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浅谈农药水分散粒剂的开发;冯建国 等;《中国农药》;20090630(第5期);第38-44页 * |
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