CN101268777B - Quizalofop-p-ethyl water suspension agent and production thereof - Google Patents

Quizalofop-p-ethyl water suspension agent and production thereof Download PDF

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Publication number
CN101268777B
CN101268777B CN200810015992XA CN200810015992A CN101268777B CN 101268777 B CN101268777 B CN 101268777B CN 200810015992X A CN200810015992X A CN 200810015992XA CN 200810015992 A CN200810015992 A CN 200810015992A CN 101268777 B CN101268777 B CN 101268777B
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agent
ethyl
quizalofop
water
preparation
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CN101268777A (en
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张黎辉
李波
陶琳
于天丛
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QINGDAO HANSEN BIOLOGIC SCIENCE CO Ltd
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QINGDAO HANSEN BIOLOGIC SCIENCE CO Ltd
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Abstract

A quizalofop-ethyl water suspending agent and a preparation method thereof belong to the technical field of herbicide containing a heterocyclic compound. The problem to be solved is as follows: the missible oil preparation in the prior art adopts a plurality of organic solvent and the active ingredient is low. The quizalofop-ethyl water suspending agent and the preparation method thereof have the key technical point that: quizalofop-ethyl is matched with a suitable moistening dispersing agent, an osmotic agent, a thickening agent, an antifreezing agent, a defoaming agent, water, etc., which are evenly dispersed in a water phase through mixing sand grind, thereby making a water based agricultural chemical preparation with high concentration. The preparation method uses less dosage, can save a plurality of wrappages and can effectively reduce the pollution of the environment and the disservice of a medicine applying person.

Description

Quizalofop-p-ethyl water suspension agent and method for making thereof
Technical field
The invention belongs to the herbicide technology field that contains heterocyclic compound, be specifically related to a kind of quizalofop-p-ethyl water suspension agent and method for making thereof.
Background technology
Quizalotop-ethyl (quizalofop-p-ethyl), chemical name (R)-2-[4-(6-chlorine quinoxaline-2-base oxygen) phenoxy group] ethyl propionate, Quizalotop-ethyl is the improvement goods removed inactive optical isomer (laevoisomer) in the process of synthetic quizalofop-ethyl after, its mechanism of action is with the grass spectrum is identical with quizalofop-ethyl extremely, absorb by the weeds cauline leaf, two-way up and down conduction is accumulated in top and intercalary meristem in plant corpus, and the inhibition cell fatty acid synthesizes makes the weeds necrosis.Quizalotop-ethyl is a kind of novel dry land cauline leaf inorganic agent of high selectivity, and the selectivity of height is arranged between grassy weed and dicotyledonous crops, and the grassy weed in broad leaf crop field is had good preventive effect.Quizalotop-ethyl the degraded in soil half life period within one day, degradation speed soon, mainly based on microbial degradation.Be widely used in various crop such as soybean, beet, rape, potato, flax, Peas, broad bean, tobacco, watermelon, cotton, peanut, broad-leaved vegetables and fruit tree, nursery forest bed, clover etc., prevent and kill off annual and perennial grassy weed.
Pesticide suspension concentrate (aqueous suspension concentrate, SC) be water-insoluble solid agricultural chemicals or the dispersion of immiscible liquids agricultural chemicals in water, consider from the production angle, generally require former medicine at room temperature for solid, and the solvability in dispersion medium (20 ℃~40 ℃ time) is lower than the pesticide species of 100mg/L.The advantage of agricultural chemicals suspension agent is evenly to mix dispersion with arbitrary proportion with water, is subjected to the influence of water quality little, easy to use, is difficult for contaminated environment, can directly or after the dilution spray.Preparation for processing can be made the suspension of high dispersive, continuous phase by waterproof pulverization, and the average grain diameter of its particle has improved the suspensibility of particle in aqueous medium greatly generally below 3 microns, has strengthened the absorption of crops to medicament.
Present Quizalotop-ethyl preparation is low content missible oil.Publication number is that the Chinese patent of CN1717993 discloses a kind of Quizalotop-ethyl herbicide microemulsion and preparation method thereof, and its technical essential is its raw material components and percentage by weight thereof: Quizalotop-ethyl 1~20, solvent 1~20, cosolvent 1~10, surfactant 0.5~30, antifreezing agent 0.5~10, water complement to 100; The oil droplet fineness of the sprinkling emulsion that this microemulsion is joined is owing to be narrower than 0.005 micron, approached true solution, so improved the dispersity of pesticide active ingredient Quizalotop-ethyl in emulsion, make emulsion approach true solution, thereby strengthened the penetrating ability of Quizalotop-ethyl, improved the effective rate of utilization of control efficiency and host plant; Simultaneously, environmentally safe, pollute little.Its weak point is: 1) wherein solvent is an organic solvent, and for example: the inferior maple hexamethylene of toluene, dimethylbenzene, methyl alcohol, ethanol, isopropyl alcohol, third reward, hexamethylene a heatable brick bed, worker's methyl is intoxicated, and using has bigger pollution to environment; 2) effective component content low (being generally 5~15% during use) causes serious waste to packing material, gives to produce and store and transport and brings a lot of inconvenience.
Summary of the invention
The present invention is directed to problems of the prior art, one of purpose has provided a kind of quizalofop-p-ethyl water suspension agent, under the prerequisite that guarantees drug effect, can effectively reduce environmental pollution and save packing material and production and use cost; The present invention provides the method for making of described quizalofop-p-ethyl water suspension agent simultaneously.
The technical solution used in the present invention is:
A kind of quizalofop-p-ethyl water suspension agent is characterized in that, is made by following components in weight percentage:
The former medicine 1~40 of Quizalotop-ethyl
Wetting dispersing agent 1~5
Bleeding agent 0.5~10
Thickener 0.1~2
Antifreezing agent 0.5~5
Defoamer 0.1~0.5
Surplus is a dispersion medium;
Described wetting dispersing agent is one or more in alkylphenol polyoxyethylene, phenethyl phenol polyethenoxy ether, alkyl phenol formaldehyde resin polyoxyethylene ether, alkylaryl polyoxyethylene poly-oxygen propylene aether, alkylphenol polyoxyethylene sulfosuccinate, aliphatic alcohol polyoxyvinethene phosphate and the polyoxyethylene nonylphenol ether phosphate;
Described bleeding agent is a kind of in JFC, the fast penetrant T, is the commercial goods, and supplier is a Shanghai Tiantan Accessory Ingredient Co., Ltd;
Described thickener has a kind of or any two kinds of mixtures in gum Arabic, xanthans, methylcellulose, carboxymethyl cellulose, hydroxyethylcellulose, PAA, polyvinyl alcohol, white carbon, bentonite, the aluminium-magnesium silicate;
Described antifreezing agent is a kind of or any mixture in ethylene glycol, urea, propane diols, the glycerine;
Described defoamer has a kind of in n-octyl alcohol, the silicone defoaming agent;
Described dispersion medium is a water.
All raw materials that the present invention adopts are the commercial goods.
Described quizalofop-p-ethyl water suspension agent is characterized in that, is made by following components in weight percentage:
The former medicine 20~40 of Quizalotop-ethyl
Wetting dispersing agent 4~5
Bleeding agent 0.5~10
Thickener 0.1~2
Antifreezing agent 0.5~5
Defoamer 0.1~0.5
Surplus is a dispersion medium.
The method for making of described quizalofop-p-ethyl water suspension agent comprises the steps:
1) add the former medicine of Quizalotop-ethyl, wetting dispersing agent, bleeding agent, thickener, antifreezing agent, defoamer and water in mixing kettle, stirring fully mixes material;
2) above-mentioned material is squeezed into ball mill, ball milling is to there not being visible bulk particle;
3) ball milling is good material is squeezed into sand milling in the sand mill again, and making its particle diameter is 2~3 microns;
4) commentaries on classics is expected to reactor, check, qualified back packing.
Compared with prior art, the present invention has following beneficial effect:
Improve active constituent content, reduced production cost.The active constituent content of conventional cream preparation is generally between 5%~15%, the mu consumption is between 20~60ml, and the mu consumption of the present invention's 40% quizalofop-p-ethyl water suspension agent is 5~8ml, can save a large amount of packing materials and cost of transportation and storage space by the improvement of formulation.Pesticides packaging thing major part is a polyester bottles, supposes that an agricultural chemicals enterprise annual production 10% Quizalotop-ethyl missible oil is 300 tons, and the price of a 200ml bottle is 0.7 yuan, needs 1,500,000 bottles altogether, and total price is 1,050,000 yuan.If produce 40% quizalofop-p-ethyl water suspension agent, under the prerequisite that satisfies the same medicine area, producing 75 tons of preparations gets final product, need 37.5 ten thousand bottles like this, total price is 26.25 ten thousand yuan, just can save 78.75 ten thousand yuan by the independent Packaging Bottle of the improvement of formulation, wherein the expense of chest, label does not count.In addition, a large amount of costs of material have also been saved simultaneously, organic solvent in the conventional cream preparation is up to 60%~80%, the price of toluene or dimethylbenzene is about 8000 yuan/ton, the solvent of producing 300 tons of cream preparation consumption per year is about 1,440,000 yuan~1,920,000 yuan, can ignore if produce the quizalofop-p-ethyl water suspension agent solvent cost, can save production cost 222.75 ten thousand yuan~270.75 ten thousand yuan so altogether.Reduced environmental pollution.Organic solvent addition in the conventional cream preparation is very high, and does not contain organic solvent in the aqueous suspension agent of the present invention fully, the substitute is the water of the environmentally safe that is easy to get in a large number.The raising of active constituent content simultaneously can be saved a large amount of pesticides packaging bottles again, reduces the pollution of packing material to environment.The plastic bottle of some pbz polymer resins second after second is embedded in the soil, is difficult for degraded under natural environment, can be residual 200~700 years, and caused chemical contamination residual to soil environment, greatly affect crop growth.Before not having better processing packing object space method, the use that as far as possible reduces the pesticides packaging bottle also is a good environmental protection behave.
Embodiment
Embodiment 1
(1) raw material proportioning: the former medicine 5Kg of Quizalotop-ethyl, phenethyl phenol polyethenoxy ether 1Kg, polyoxyethylene nonylphenol ether phosphate 1.5Kg, JFC3Kg, white carbon 1Kg, xanthans 0.2Kg, ethylene glycol 3Kg, silicone defoaming agent 0.1Kg, running water 85.2Kg.
(2) preparation process: in mixing kettle, add whole phenethyl phenol polyethenoxy ether 1Kg, polyoxyethylene nonylphenol ether phosphate 1.5Kg, JFC3Kg,, ethylene glycol 3Kg, silicone defoaming agent 0.1Kg, running water 85.2Kg, stir 30 minutes even to mixing of materials.Under stirring, add Quizalotop-ethyl 5Kg then, white carbon 1Kg, xanthans 0.2Kg stirred 1 hour.Afterwards material is squeezed in the ball mill, ball milling is to there not being visible bulk particle.The material that ball milling is good is squeezed into sand milling in the sand mill again, makes its particle diameter reach regulation and requires (the average particle diameter is below 3 microns).Change at last and expect, by the every index of GB requirement chemical examination, qualified back packing to reactor.
Embodiment 2
(1) raw material proportioning: Quizalotop-ethyl 10Kg, phenethyl phenol polyethenoxy ether 1.5Kg, alkylphenol polyoxyethylene 2Kg, fast penetrant T 5Kg, aluminium-magnesium silicate 0.8Kg, xanthans 0.15Kg, glycerine 3Kg, n-octyl alcohol 0.5Kg, running water 77.05Kg.
(2) preparation process: in mixing kettle, add whole phenethyl phenol polyethenoxy ether 1.5Kg, alkylphenol polyoxyethylene 2Kg, fast penetrant T 5Kg, glycerine 3Kg, n-octyl alcohol 0.5Kg, running water 77.05Kg, stir 30 minutes even to mixing of materials.Under stirring, add Quizalotop-ethyl 10Kg then, aluminium-magnesium silicate 0.8Kg, xanthans 0.15Kg stirred 1 hour.Afterwards material is squeezed in the ball mill, ball milling is to there not being visible bulk particle.The material that ball milling is good is squeezed into sand milling in the sand mill again, makes its particle diameter reach regulation and requires (the average particle diameter is below 3 microns).Change at last and expect, by the every index of GB requirement chemical examination, qualified back packing to reactor.
Embodiment 3
(1) raw material proportioning: Quizalotop-ethyl 20Kg, alkylaryl polyoxyethylene poly-oxygen propylene aether 1.2Kg, polyoxyethylene nonylphenol ether phosphate 2.3Kg, fast penetrant T 6Kg, aluminium-magnesium silicate 0.5Kg, xanthans 0.12Kg, glycerine 3.5Kg, silicone defoaming agent 0.15Kg, running water 66.23Kg.
(2) preparation process: in mixing kettle, add whole alkylaryl polyoxyethylene poly-oxygen propylene aether 1.2Kg, polyoxyethylene nonylphenol ether phosphate 2.3Kg, fast penetrant T 6Kg, glycerine 3.5Kg, silicone defoaming agent 0.15Kg, running water 66.23Kg, stir 30 minutes even to mixing of materials.Under stirring, add Quizalotop-ethyl 20Kg then, aluminium-magnesium silicate 0.5Kg, xanthans 0.12Kg stirred 1 hour.Afterwards material is squeezed in the ball mill, ball milling is to there not being visible bulk particle.The material that ball milling is good is squeezed into sand milling in the sand mill again, makes its particle diameter reach regulation and requires (the average particle diameter is below 3 microns).Change at last and expect, by the every index of GB requirement chemical examination, qualified back packing to reactor.
Embodiment 4
(1) raw material proportioning: Quizalotop-ethyl 30Kg, alkylphenol polyoxyethylene sulfosuccinate 4Kg, JFC 7Kg, carboxymethyl cellulose 0.5Kg, bentonite 1Kg, urea 5Kg, silicone defoaming agent 0.15Kg, running water 52.35Kg.
(2) preparation process: in mixing kettle, add whole alkylphenol polyoxyethylene sulfosuccinate 4Kg, JFC 7Kg, silicone defoaming agent 0.15Kg, running water 52.35Kg, stir 30 minutes even to mixing of materials.Under stirring, add Quizalotop-ethyl 30Kg then, carboxymethyl cellulose 0.5Kg, bentonite 1Kg, urea 5Kg stirred 1 hour.Afterwards material is squeezed in the ball mill, ball milling is to there not being visible bulk particle.The material that ball milling is good is squeezed into sand milling in the sand mill again, makes its particle diameter reach regulation and requires (the average particle diameter is below 3 microns).Change at last and expect, by the every index of GB requirement chemical examination, qualified back packing to reactor.
Embodiment 5
(1) raw material proportioning: Quizalotop-ethyl 40Kg, alkyl phenol formaldehyde resin polyoxyethylene ether 1Kg, aliphatic alcohol polyoxyvinethene phosphate 3.5Kg, fast penetrant T 10Kg, xanthans 0.1Kg, bentonite 0.5Kg, propane diols 5Kg, silicone defoaming agent 0.2Kg, running water 39.7Kg.
(2) preparation process: in mixing kettle, add whole alkyl phenol formaldehyde resin polyoxyethylene ether 1Kg, aliphatic alcohol polyoxyvinethene phosphate 3.5Kg, fast penetrant T 10Kg, propane diols 5Kg, silicone defoaming agent 0.2Kg, running water 39.7Kg, stir 30 minutes even to mixing of materials.Under stirring, add Quizalotop-ethyl 40Kg then, xanthans 0.1Kg, bentonite 0.5Kg stirred 1 hour.Afterwards material is squeezed in the ball mill, ball milling is to there not being visible bulk particle.The material that ball milling is good is squeezed into sand milling in the sand mill again, makes its particle diameter reach regulation and requires (the average particle diameter is below 3 microns).Change at last and expect, by the every index of GB requirement chemical examination, qualified back packing to reactor.
The quizalofop-p-ethyl water suspension agent of embodiment of the invention 1-5 and existing Quizalotop-ethyl herbicide preparation (5% Quizalotop-ethyl missible oil) field efficacy comparable situation is as follows:
15 days investigation contrast tables behind table 1 field efficacy (%) medicine
Figure S200810015992XD00051
30 days investigation contrast tables behind table 2 field efficacy (%) medicine
Figure S200810015992XD00061

Claims (2)

1. a quizalofop-p-ethyl water suspension agent is characterized in that, is made by following components in weight percentage:
Figure FSB00000553169200011
Surplus is a dispersion medium;
Described wetting dispersing agent is one or more in alkylphenol polyoxyethylene, phenethyl phenol polyethenoxy ether, alkyl phenol formaldehyde resin polyoxyethylene ether, alkylaryl polyoxyethylene poly-oxygen propylene aether, alkylphenol polyoxyethylene sulfosuccinate, aliphatic alcohol polyoxyvinethene phosphate and the polyoxyethylene nonylphenol ether phosphate;
Described bleeding agent is a kind of in JFC, the fast penetrant T;
Described thickener has a kind of or any two kinds of mixtures in gum Arabic, xanthans, methylcellulose, carboxymethyl cellulose, hydroxyethylcellulose, PAA, polyvinyl alcohol, white carbon, bentonite, the aluminium-magnesium silicate;
Described antifreezing agent is a kind of or any mixture in ethylene glycol, urea, propane diols, the glycerine;
Described defoamer has a kind of in n-octyl alcohol, the silicone defoaming agent;
Described dispersion medium is a water.
2. the method for making of the described quizalofop-p-ethyl water suspension agent of claim 1 is characterized in that, comprises the steps:
1) add the former medicine of Quizalotop-ethyl, wetting dispersing agent, bleeding agent, thickener, antifreezing agent, defoamer and water in mixing kettle, stirring fully mixes material;
2) above-mentioned material is squeezed into ball mill, ball milling is to there not being visible bulk particle;
3) ball milling is good material is squeezed into sand milling in the sand mill again, makes its particle diameter less than 3 microns;
4) commentaries on classics is expected to reactor, check, qualified back packing.
CN200810015992XA 2008-05-14 2008-05-14 Quizalofop-p-ethyl water suspension agent and production thereof Expired - Fee Related CN101268777B (en)

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JP5032695B1 (en) * 2011-09-22 2012-09-26 大伍貿易株式会社 Water vapor pressure reducing agent
CN103493804B (en) * 2013-09-30 2014-12-17 浙江海正化工股份有限公司 Compound pesticide wetting agent and application of compound pesticide wetting agent in preparation of pesticide preparations

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1239640A (en) * 1999-07-08 1999-12-29 江苏省农药研究所 Suspending benzothiazole herbicide and its recompounding preparation
CN1409965A (en) * 2002-11-15 2003-04-16 王正权 Herbicide composition containing KIH 9201
US20030148887A1 (en) * 2001-12-17 2003-08-07 Matthias Bratz Process for the preparation of solvent-free suspensions
CN1568694A (en) * 2003-07-15 2005-01-26 沈阳化工研究院 Weed removal combination
CN1846495A (en) * 2005-04-16 2006-10-18 胡潜力 Dry quizalofop-ethyl suspension and its prepn process
WO2007145221A1 (en) * 2006-06-13 2007-12-21 Nissan Chemical Industries, Ltd. Aqueous suspension agricultural chemical composition

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1239640A (en) * 1999-07-08 1999-12-29 江苏省农药研究所 Suspending benzothiazole herbicide and its recompounding preparation
US20030148887A1 (en) * 2001-12-17 2003-08-07 Matthias Bratz Process for the preparation of solvent-free suspensions
CN1409965A (en) * 2002-11-15 2003-04-16 王正权 Herbicide composition containing KIH 9201
CN1568694A (en) * 2003-07-15 2005-01-26 沈阳化工研究院 Weed removal combination
CN1846495A (en) * 2005-04-16 2006-10-18 胡潜力 Dry quizalofop-ethyl suspension and its prepn process
WO2007145221A1 (en) * 2006-06-13 2007-12-21 Nissan Chemical Industries, Ltd. Aqueous suspension agricultural chemical composition

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