CN103202290B - Cyhalofop-butyl suspending agent and preparation method thereof - Google Patents
Cyhalofop-butyl suspending agent and preparation method thereof Download PDFInfo
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- CN103202290B CN103202290B CN201310162699.7A CN201310162699A CN103202290B CN 103202290 B CN103202290 B CN 103202290B CN 201310162699 A CN201310162699 A CN 201310162699A CN 103202290 B CN103202290 B CN 103202290B
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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 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 suction conductivity low toxicity herbicide, is only kind paddy rice to tight security in fragrant phenoxy phenoxy propionic acid 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, 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 cyhalofop-butyl active compound and is dissolved in organic solvent, can prevent that former medicine is because variations in temperature is separated out.Although cyhalofop-butyl is water insoluble, can make suspending agent, it is inconvenient being made suspending agent, and this is that former medicine is easily separated out formation oil droplet due to when suspending agent carries out heating storage, and this variation is irreversible.As long as analyse oily problem while having solved the storage of cyhalofop-butyl suspending agent heat, just can make suspending agent and use.
Summary of the invention
The object 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.
Object of the present invention is achieved through the following technical solutions:
A cyhalofop-butyl suspending agent, in it is characterized in that filling a prescription, each component and mass percent thereof are: cyhalofop-butyl active compound 1.0% ~ 40.0%, 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), alkylphenol polyoxyethylene carboxylate, alkylphenol polyoxyethylene sulfuric ester, aryl phenol APEO (for example agriculture breast 601), aryl phenol polyoxyethylene ether phosphate (for example agriculture breast 601P), (for example agriculture breast 1601 for aryl phenol polyoxyethylene poly-oxygen propylene aether, 1602), aryl phenol polyoxyethylene poly-oxygen propylene aether phosphate (for example agriculture breast 1601P), polyol fatty acid ester and ethylene oxide adduct thereof (Span60 for example, Tween80), alkylbenzenesulfonate (for example agriculture 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 penetrant t, described antifreezing agent is one or more combinations in mineral salt, urea, ethylene glycol, glycerine, propane diols, diethylene glycol (DEG), described thickener is one or more combinations in aluminium-magnesium silicate, xanthans, gelatin, gum Arabic, sodium alginate, 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 formula, load weighted cyhalofop-butyl active compound, emulsifying dispersant are added in high shear reactor, be heated to 50 ℃ ~ 70 ℃, the oil phase that the system of being stirred to is homogeneous;
(2) by the water in formula, be heated to 50 ℃ ~ 70 ℃, under high speed shear stirs, slowly join in above-mentioned oil phase, after adding, continue again high speed shear and stir 5min ~ 30min, obtain uniform emulsion;
(3) be cooled to room temperature, remaining antifreezing agent and thickener are joined in system, stir.
The present invention has utilized the low-melting feature of cyhalofop-butyl active compound, under the existence higher than melting temperature, emulsifying dispersant and water, can form emulsion, after cooling, former medicine becomes the solid-state suspension system that forms from liquid state, the feature of this technology is: (1) is higher than under melting temperature, System forming emulsion, emulsifying dispersant can be good at former cartridge bag to wrap up in dispersion, has solved and 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, has analysed oily problem; (2) this preparation method has reduced the secondary sand milling step in traditional suspending agent preparation technology, has only increased heating steps, and the comprehensive equipment investment that reduced, has reduced the loss of material, has improved production efficiency.
It should be noted that, because the use storage temperature of agricultural chemicals is generally all lower than 40 ℃, according to the definition of suspending agent and aqueous emulsion, cyhalofop-butyl preparation prepared by the method is called suspending agent, because below 40 ℃ time, the cyhalofop-butyl in preparation is solid-state rather than liquid; The pesticidal preparations term of validity is generally 2 years, in order to investigate the long storage stability of preparation, when research and development preparation, in order to simulate long storage stability, generally preparation sealing is placed in to 54 ℃ of heat storages two weeks, at this temperature, the former medicine in preparation is gradually from the solid-state liquid state that becomes, the system status of system between suspending agent and aqueous emulsion.
Suspending agent prepared by the method, has generality, and the former medicines of other low melting points such as the former medicine of the organic phosphors such as chlopyrifos and chrysanthemum ester class can be prepared into suspending agent by this method.
Embodiment
In order to understand better the present invention, below in conjunction with embodiment, the invention will be further described.But the scope of protection of present invention is not limited to the scope that embodiment indicates.Remove without specified otherwise " % " representative " mass percent " in following embodiment.
embodiment 1 10.0% cyhalofop-butyl suspending agent
97.0% cyhalofop-butyl active compound 10.4%, 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 104kg 97% cyhalofop-butyl active compound, 10kg alkylphenol polyoxyethylene, 40kg aryl phenol polyoxyethylene ether phosphate in high shear reactor, is heated to 55 ℃, the oil phase that the system of being stirred to is homogeneous; (2) 744kg water is heated to 55 ℃, under high speed shear stirs, slowly joins in above-mentioned oil phase, after adding, continue again high speed shear and stir 10min, obtain uniform emulsion; (3) be cooled to room temperature, by 50kg urea, 50kg 4.0% xanthans hydrogel, 2kg aluminium-magnesium silicate join in system, stir.
This preparation is placed in to 54 ℃ of heat storages 2 weeks, does not analyse oil, heat storage stability is qualified.
embodiment 2 20% cyhalofop-butyl suspending agents
97% cyhalofop-butyl active compound 20.7%, 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 207kg 97% cyhalofop-butyl active compound, 15kg polyol fatty acid ester, 40kg aryl phenol polyoxyethylene poly-oxygen propylene aether phosphate in high shear reactor, be heated to 60 ℃, the oil phase that the system of being stirred to is homogeneous; (2) 666kg water is heated to 60 ℃, under high speed shear stirs, slowly joins in above-mentioned oil phase, after adding, continue again high speed shear and stir 10min, obtain uniform emulsion; (3) be cooled to room temperature, by 30kg ethylene glycol, 40kg 4.0% xanthans hydrogel, 2kg aluminium-magnesium silicate join in system, stir.
This preparation is placed in to 54 ℃ of heat storages 2 weeks, does not analyse oil, heat storage stability is qualified.
embodiment 3 30% cyhalofop-butyl suspending agents
97% cyhalofop-butyl active compound 31.0%, 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 by 310kg 97% cyhalofop-butyl active compound, 10kg alkylbenzenesulfonate, 20kg fatty alcohol polyoxyethylene ether sulfate, 30kg alkylphenol polyoxyethylene carboxylate, adds in high shear reactor, be heated to 65 ℃, the oil phase that the system of being stirred to is homogeneous; (2) 587kg water is heated to 65 ℃, under high speed shear stirs, slowly joins in above-mentioned oil phase, after adding, continue again high speed shear and stir 10min, obtain uniform emulsion; (3) be cooled to room temperature, by 20kg glycerine, 20kg 4.0% xanthans hydrogel, 3kg aluminium-magnesium silicate join in system, stir.
This preparation is placed in to 54 ℃ of heat storages 2 weeks, does not analyse oil, heat storage stability is qualified.
Cyhalofop-butyl suspending agent of the present invention is used for preventing and treating moleplant seed, and efficacy test is as follows:
The drug effect of cyhalofop-butyl suspending agent prepared by the present invention approaches the drug effect of missible oil product.
Claims (3)
1. one kind for preventing and treating the preparation method of 10% cyhalofop-butyl suspending agent of moleplant seed, it is characterized in that the method comprises the steps: that (1) adds 104kg 97% cyhalofop-butyl active compound, 10kg alkylphenol polyoxyethylene, 40kg aryl phenol polyoxyethylene ether phosphate in high shear reactor, be heated to 55 ℃, the oil phase that the system of being stirred to is homogeneous; (2) 744kg water is heated to 55 ℃, under high speed shear stirs, slowly joins in above-mentioned oil phase, after adding, continue again high speed shear and stir 10min, obtain uniform emulsion; (3) be cooled to room temperature, by 50kg urea, 50kg 4.0% xanthans hydrogel, 2kg aluminium-magnesium silicate join in system, stir.
2. one kind for preventing and treating the preparation method of 20% cyhalofop-butyl suspending agent of moleplant seed, it is characterized in that the method comprises the steps: that (1) adds 207kg 97% cyhalofop-butyl active compound, 15kg polyol fatty acid ester, 40kg aryl phenol polyoxyethylene poly-oxygen propylene aether phosphate in high shear reactor, be heated to 60 ℃, the oil phase that the system of being stirred to is homogeneous; (2) 666kg water is heated to 60 ℃, under high speed shear stirs, slowly joins in above-mentioned oil phase, after adding, continue again high speed shear and stir 10min, obtain uniform emulsion; (3) be cooled to room temperature, by 30kg ethylene glycol, 40kg 4.0% xanthans hydrogel, 2kg aluminium-magnesium silicate join in system, stir.
3. one kind for preventing and treating the preparation method of 30% cyhalofop-butyl suspending agent of moleplant seed, it is characterized in that the method comprises the steps: that (1) is by 310kg 97% cyhalofop-butyl active compound, 10kg alkylbenzenesulfonate, 20kg fatty alcohol polyoxyethylene ether sulfate, 30kg alkylphenol polyoxyethylene carboxylate, add in high shear reactor, be heated to 65 ℃, the oil phase that the system of being stirred to is homogeneous; (2) 587kg water is heated to 65 ℃, under high speed shear stirs, slowly joins in above-mentioned oil phase, after adding, continue again high speed shear and stir 10min, obtain uniform emulsion; (3) be cooled to room temperature, by 20kg glycerine, 20kg 4.0% xanthans hydrogel, 3kg aluminium-magnesium silicate join in system, stir.
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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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| CN101773122A (en) * | 2009-12-30 | 2010-07-14 | 西南大学 | Cyhalofop-butyl water suspending agent and preparation method thereof |
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