CN103202290A - Cyhalofop-butyl suspending agent and preparation method thereof - Google Patents
Cyhalofop-butyl suspending agent and preparation method thereof Download PDFInfo
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- CN103202290A CN103202290A CN2013101626997A CN201310162699A CN103202290A CN 103202290 A CN103202290 A CN 103202290A CN 2013101626997 A CN2013101626997 A CN 2013101626997A CN 201310162699 A CN201310162699 A CN 201310162699A CN 103202290 A CN103202290 A CN 103202290A
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Abstract
The invention belongs to the field of pesticide preparations and particularly relates to cyhalofop-butyl suspending agent and a preparation method of the cyhalofop-butyl suspending agent. The suspending agent comprises the following components in percentage by mass: 1.0-40.0% of cyhalofop-butyl original medicine, 1.0-15.0% of an emulsion dispersant, 1.0-8.0% of an anti-freezing agent, 0-3.0% of a thickening agent and the balance of water. The preparation method is a phase inversion emulsification method. The cyhalofop-butyl suspending agent prepared by adopting the method disclosed by the invention has good hot storage stability and good pesticide effect.
Description
Technical field
The invention belongs to the pesticidal preparations field, be specifically related to a kind of cyhalofop-butyl suspending agent and preparation method thereof.
Background technology
Cyhalofop-butyl is a kind of interior conductivity low toxicity herbicide of inhaling, and is the only kind that paddy rice is had tight security in the fragrant phenoxy propionic acid class weed killer herbicide.Former medicine is white crystalline solid, and proportion is 1.2375(20 ℃), 363 ℃ of boiling points, 48 ℃ ~ 50 ℃ of fusing points are dissolved in most of solvents, and are water insoluble.Because the fusing point of cyhalofop-butyl is lower, preparation is generally 10%, 15%, 20% missible oil, aqueous emulsion or microemulsion at present, is about to the former medicine of cyhalofop-butyl and is dissolved in the organic solvent, can prevent that former medicine is owing to variations in temperature is separated out.Though cyhalofop-butyl is water insoluble, can make suspending agent, it is made suspending agent is inconvenient, this is that this variation is irreversible because when suspending agent carried out heat storage test, former medicine was separated out the formation oil droplet easily.As long as analyse oily problem when having solved the storage of cyhalofop-butyl suspending agent heat, just can make suspending agent and use.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, a kind of cyhalofop-butyl suspending agent and preparation method thereof is provided, solved hot storage and analysed oily instability problem.
Purpose of the present invention is achieved through the following technical solutions:
A kind of cyhalofop-butyl suspending agent, each component and mass percent thereof are in it is characterized in that filling a prescription: the former medicine 1.0% ~ 40.0% of cyhalofop-butyl, emulsifying dispersant 1.0% ~ 15.0%, antifreezing agent 1.0% ~ 8.0%, thickener 0% ~ 3.0%, surplus is water; Described emulsifying dispersant is alkylphenol polyoxyethylene (for example OP-10), alkylphenol polyoxyethylene phosphate (for example OP-10P), the alkylphenol polyoxyethylene carboxylate, the alkylphenol polyoxyethylene sulfuric ester, aryl phenol APEO (for example the farming breast 601), aryl phenol polyoxyethylene ether phosphate (for example agricultural newborn 601P), (for example the farming breast 1601 for the aryl phenol polyoxyethylene poly-oxygen propylene aether, 1602), aryl phenol polyoxyethylene poly-oxygen propylene aether phosphate (for example agricultural newborn 1601P), polyol fatty acid ester and ethylene oxide adduct thereof (Span60 for example, Tween80), alkylbenzenesulfonate (for example the farming breast 500), castor oil polyoxyethylene ether (EL40 for example, EL80), sulfated castor oil, fatty alcohol polyoxyethylene ether sulfate (for example AES), one or more combinations in the penetrant t; Described antifreezing agent is one or more combinations in mineral salt, urea, ethylene glycol, glycerine, propane diols, the diethylene glycol (DEG); Described thickener is one or more combinations in aluminium-magnesium silicate, xanthans, gelatin, gum Arabic, sodium alginate, the polyacrylate.
The preparation method of this cyhalofop-butyl suspending agent is phase conversion emulsifying, and concrete steps are as follows:
(1) according to the proportioning in the prescription, the former medicine of load weighted cyhalofop-butyl, emulsifying dispersant are added in the high shear reactor, be heated to 50 ℃ ~ 70 ℃, the system of being stirred to is the oil phase of homogeneous;
(2) water in will filling a prescription is heated to 50 ℃ ~ 70 ℃, under high speed shear stirs, slowly joins in the above-mentioned oil phase, adds to continue high speed shear again after finishing and stir 5min ~ 30min, obtains uniform emulsion;
(3) be cooled to room temperature, remaining antifreezing agent and thickener are joined in the system, stir.
The present invention has utilized the low-melting characteristics of the former medicine of cyhalofop-butyl, be higher than melting temperature, emulsifying dispersant and water in the presence of can form emulsion, the former medicine in cooling back becomes the solid-state suspension system that forms by liquid state, the characteristics of present technique are: (1) is being higher than under the melting temperature, system forms emulsion, emulsifying dispersant can be good at former cartridge bag is wrapped up in dispersion, has solved and has analysed oily problem when traditional suspending agent sand milling mode can not effectively be wrapped up the former medicine of solid the storage of scattering problem and preparation heat; (2) this preparation method has reduced the secondary sand milling step among traditional suspending agent preparation technology, has only increased heating steps, and the comprehensive equipment input that reduced has reduced the loss of material, has improved production efficiency.
Need to prove, because the use storage temperature of agricultural chemicals generally all is lower than 40 ℃, according to the definition of suspending agent and aqueous emulsion, the cyhalofop-butyl preparation that the method is prepared is called suspending agent, because below 40 ℃ the time, the cyhalofop-butyl in the preparation is solid-state rather than liquid; The pesticidal preparations term of validity was generally 2 years, in order to investigate the long storage stability of preparation, when the research and development preparation, in order to simulate long storage stability, generally the preparation sealing is placed 54 ℃ of heat two weeks of storage, under this temperature, by the solid-state liquid state that becomes, system is in the system status between suspending agent and the aqueous emulsion to the former medicine in the preparation gradually.
The suspending agent of the method preparation has generality, and for example the former medicines of other low melting points such as the former medicine of organic phosphor such as chlopyrifos and chrysanthemum ester class can be prepared into suspending agent with this method.
Embodiment
In order to understand the present invention better, the invention will be further described below in conjunction with embodiment.But the scope of protection of present invention is not limited to the scope that embodiment indicates.Except no specified otherwise, " % " representative " mass percent " among the following embodiment.
Embodiment 1 10.0% cyhalofop-butyl suspending agent
The former medicine 10.4% of 97.0% cyhalofop-butyl, alkylphenol polyoxyethylene 1.0%, aryl phenol polyoxyethylene ether phosphate 4.0%, urea 5.0%, 4.0% xanthans hydrogel 5.0%, aluminium-magnesium silicate 0.2%, water 74.4%.
The preparation method of this suspending agent is: (1) adds the former medicine of 104kg 97% cyhalofop-butyl, 10kg alkylphenol polyoxyethylene, 40kg aryl phenol polyoxyethylene ether phosphate in the high shear reactor, is heated to 55 ℃, and the system of being stirred to is the oil phase of homogeneous; (2) 744kg water is heated to 55 ℃, under high speed shear stirs, slowly joins in the above-mentioned oil phase, continue high speed shear again after adding finishes and stir 10min, obtain uniform emulsion; (3) be cooled to room temperature, with 50kg urea, 50kg 4.0% xanthans hydrogel, 2kg aluminium-magnesium silicate join in the system, stir.
This preparation is placed 54 ℃ of heat 2 weeks of storage, do not analyse oil, heat storage stability is qualified.
Embodiment 2 20% cyhalofop-butyl suspending agents
The former medicine 20.7% of 97% cyhalofop-butyl, polyol fatty acid ester 1.5%, aryl phenol polyoxyethylene poly-oxygen propylene aether phosphate 4.0%, ethylene glycol 3.0%, 4.0% xanthans hydrogel 4.0%, aluminium-magnesium silicate 0.2%, water 66.6%.
The preparation method of this suspending agent is: (1) adds the former medicine of 207kg 97% cyhalofop-butyl, 15kg polyol fatty acid ester, 40kg aryl phenol polyoxyethylene poly-oxygen propylene aether phosphate in the high shear reactor, be heated to 60 ℃, the system of being stirred to is the oil phase of homogeneous; (2) 666kg water is heated to 60 ℃, under high speed shear stirs, slowly joins in the above-mentioned oil phase, continue high speed shear again after adding finishes and stir 10min, obtain uniform emulsion; (3) be cooled to room temperature, with 30kg ethylene glycol, 40kg 4.0% xanthans hydrogel, 2kg aluminium-magnesium silicate join in the system, stir.
This preparation is placed 54 ℃ of heat 2 weeks of storage, do not analyse oil, heat storage stability is qualified.
Embodiment 3 30% cyhalofop-butyl suspending agents
The former medicine 31.0% of 97% cyhalofop-butyl, alkylbenzenesulfonate 1.0%, fatty alcohol polyoxyethylene ether sulfate 2.0%, alkylphenol polyoxyethylene carboxylate 3.0%, glycerine 2.0%, 4.0% xanthans hydrogel 2.0%, aluminium-magnesium silicate 0.3%, water 58.7%.
The preparation method of this suspending agent is: (1) is with the former medicine of 310kg 97% cyhalofop-butyl, 10kg alkylbenzenesulfonate, the 20kg fatty alcohol polyoxyethylene ether sulfate, 30kg alkylphenol polyoxyethylene carboxylate adds in the high shear reactor, be heated to 65 ℃, the system of being stirred to is the oil phase of homogeneous; (2) 587kg water is heated to 65 ℃, under high speed shear stirs, slowly joins in the above-mentioned oil phase, continue high speed shear again after adding finishes and stir 10min, obtain uniform emulsion; (3) be cooled to room temperature, with the 20kg glycerine, 20kg 4.0% xanthans hydrogel, 3kg aluminium-magnesium silicate join in the system, stir.
This preparation is placed 54 ℃ of heat 2 weeks of storage, do not analyse oil, heat storage stability is qualified.
Cyhalofop-butyl suspending agent of the present invention is used for the control moleplant seed, and the indoor harmacological effect experiment is as follows:
The drug effect of the cyhalofop-butyl suspending agent of the present invention's preparation is near the drug effect of missible oil product.
Claims (2)
1. the cyhalofop-butyl suspending agent of phase conversion emulsifying preparation, each component and mass percent thereof are in it is characterized in that filling a prescription: the former medicine 1.0% ~ 40.0% of cyhalofop-butyl, emulsifying dispersant 1.0% ~ 15.0%, antifreezing agent 1.0% ~ 8.0%, thickener 0% ~ 3.0%, surplus are water; Described emulsifying dispersant is alkylphenol polyoxyethylene, the alkylphenol polyoxyethylene phosphate, the alkylphenol polyoxyethylene carboxylate, the alkylphenol polyoxyethylene sulfuric ester, the aryl phenol APEO, the aryl phenol polyoxyethylene ether phosphate, the aryl phenol polyoxyethylene poly-oxygen propylene aether, aryl phenol polyoxyethylene poly-oxygen propylene aether phosphate, polyol fatty acid ester and ethylene oxide adduct thereof, alkylbenzenesulfonate, castor oil polyoxyethylene ether, sulfated castor oil, fatty alcohol polyoxyethylene ether sulfate, one or more combinations in the penetrant t; Described antifreezing agent is one or more combinations in mineral salt, urea, ethylene glycol, glycerine, propane diols, the diethylene glycol (DEG); Described thickener is one or more combinations in aluminium-magnesium silicate, xanthans, gelatin, gum Arabic, sodium alginate, the polyacrylate.
2. phase conversion emulsifying according to claim 1, it is characterized in that this method may further comprise the steps: (1) is according to the proportioning in the prescription, the former medicine of load weighted cyhalofop-butyl, emulsifying dispersant are added in the high shear reactor, be heated to 50 ℃ ~ 70 ℃, the system of being stirred to is the oil phase of homogeneous; (2) water in will filling a prescription is heated to 50 ℃ ~ 70 ℃, under high speed shear stirs, slowly joins in the above-mentioned oil phase, adds to continue high speed shear again after finishing and stir 5min ~ 30min, obtains uniform emulsion; (3) be cooled to room temperature, remaining antifreezing agent and thickener are joined in the system, stir.
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| CN201310162699.7A CN103202290B (en) | 2013-05-07 | 2013-05-07 | Cyhalofop-butyl suspending agent and preparation method thereof |
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| CN201310162699.7A CN103202290B (en) | 2013-05-07 | 2013-05-07 | Cyhalofop-butyl suspending agent and preparation method thereof |
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| CN103202290B CN103202290B (en) | 2014-04-16 |
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| CN105724400A (en) * | 2016-04-13 | 2016-07-06 | 安徽美兰农业发展股份有限公司 | Penoxsulam and cyhalofop-butyl compounded dispersible oil suspending agent and preparation method thereof |
| CN113575582A (en) * | 2021-08-27 | 2021-11-02 | 安徽省圣丹生物化工有限公司 | Synergistic herbicide containing cyhalofop-butyl |
| CN115152749A (en) * | 2022-06-01 | 2022-10-11 | 佳化化学科技发展（上海）有限公司 | Aqueous suspension and preparation method thereof |
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| CN113575582A (en) * | 2021-08-27 | 2021-11-02 | 安徽省圣丹生物化工有限公司 | Synergistic herbicide containing cyhalofop-butyl |
| CN115152749A (en) * | 2022-06-01 | 2022-10-11 | 佳化化学科技发展（上海）有限公司 | Aqueous suspension and preparation method thereof |
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