CN101530082A - Preparation method of cyhalofop-butyl microemulsion - Google Patents
Preparation method of cyhalofop-butyl microemulsion Download PDFInfo
- Publication number
- CN101530082A CN101530082A CN200810101937A CN200810101937A CN101530082A CN 101530082 A CN101530082 A CN 101530082A CN 200810101937 A CN200810101937 A CN 200810101937A CN 200810101937 A CN200810101937 A CN 200810101937A CN 101530082 A CN101530082 A CN 101530082A
- Authority
- CN
- China
- Prior art keywords
- cyhalofop
- butyl
- microemulsion
- water
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a pesticide preparation, in particular to a preparation method of cyhalofop-butyl microemulsion. As to exterior appearance, the cyhalofop-butyl microemulsion is transparent and homogeneous liquid and consists of following ingredients with composition ratios by weight: 2 to 20 percent of technical product of cyhalofop-butyl, 5 to 30 percent of organic solvent, 5 to 30 percent of surface active agent, and the balance of de-ionized water. The organic solvent is cyclohexanone, ethyl alcohol, methyl alcohol, DMF, toluol or dimethylbenzene; the surface active agent is Polyoxyethylene nonyl phenyl ether, calcium dodecyl benzene sulfonate and the like. The cyhalofop-butyl microemulsion is primrose yellow transparency liquid in exterior appearance which does not change when stored in subzero 5 DEG C to 60 DEG C. The agricultural chemical particles of microemulsion are micronized into about 0.1 to 0.01mu m, thus having strong penetrability to plants and pest epidermis and raising the activity of desinsection and chlordimeform.
Description
Technical field
The present invention relates to a kind of pesticide herbicide, relate to a kind of preparation method of cyhalofop-butyl microemulsion specifically.
Technical background
Cyhalofop-butyl, other title: alkynes oxalic acid, a thousand pieces of gold, eternal lasting, crin autumn, Clincher.Physicochemical property: this product is a white crystalline solid, 50 ℃ of fusing points, vapour pressure 120mPa (20 ℃).Solvability (20 ℃): 0.7mg/L in the water (pH7), 60.7% (percentage by weight) in the dimethylbenzene 47.7%, in the acetone.Stable under pH4, slowly hydrolysis under pH7 is decomposed the fastest when pH1.2 or pH9.
The present invention is that a kind of selectivity inner sucting conduction type cauline leaf is handled weed killer herbicide.Handle as cauline leaf, the stem, the leaf that can be plant absorb, and are transmitted to growing point and meristematic tissue, and the fatty acid that suppresses weeds by the inhibition to acetyl-CoA carboxylase is synthetic, suppresses weed growth, stopped growing in several days by the medicine weeds, and be withered gradually later on.This medicine is to rice safety.Mainly prevent and kill off the barnyard grass grass, grassy weeds such as moleplant seed.Scope of application paddy field.Using method rice direct seeding field amount of formulation 495-750 milliliter/hectare,, former medicine rat acute per os LD50 in grassy weed 2-3 leaf phase dispenser〉5000 milligrams/kilogram, rat acute is through skin LD50〉2000 milligrams/kilogram.Skin is had no stimulation, eyes are had minimal irritation.No carcinogenic, teratogenesis, mutagenesis.Formulation 10% missible oil.
Along with being extensive use of of chemical pesticide, how to reduce the pollution of environment and, more and more paid close attention to by people to people and animals' murder by poisoning, therefore, reduce toxicity, the raising drug effect is the inexorable trend that agricultural chemicals develops.Researching and developing the purpose that realizes reducing toxicity, improves drug effect by formulation is a kind of comparatively economy mode efficiently for former medicine research and development.At present, China is relatively backward aspect formulations of pesticide research and development, and basically based on missible oil and wetting powder, its consumption accounts for the 70-80% of total amount of formulation; And formulation is more single, and the ratio of former medicine and preparation is 1:6, the then about 1:30 of developed country, and both fall far short.Obviously, this can not adapt to current agricultural production development, especially agricultural product structural adjustment far away to the variation of agricultural chemicals demand, and can influence the marketing and the service life of Pesticidal products to a great extent.Simultaneously, the single operation technique that also can cause of the formulations of pesticide falls behind.Pay attention to the transformation of existing formulation, develop the novel form that meets production and environmental requirement, not only adapt to the requirement of sustainable development, also can remedy the deficiency of former medicine development ability simultaneously.
In numerous formulations of pesticide, comparatively convenient and general use is a liquid formulation, and wherein using maximum formulations for a long time is missible oil.Missible oil needs to use a large amount of organic solvents in process, as benzene,toluene,xylene or the like, the use of a large amount of organic solvents not only causes the waste of industrial chemicals, and since the combustibility of solvent on transportation, storage and container selection, also be restricted.Simultaneously, brought very big murder by poisoning for environment and human health, economic development and environment for human survival that will crisis country.Developed country limits or forbids using in a large number the pesticide new variety registration of harmful organic solvent preparations such as benzene,toluene,xylene from sustainable development target.Therefore, develop novel liquid formulation, become the trend of the times of agricultural chemicals development to reduce or eliminate these virulent organic solvents.Wherein, Water-borne modification is exactly one of dominant direction of formulations of pesticide development.And, the new architecture of agricultural chemicals also can increase new feature to agricultural chemicals, more can give full play to the action characteristic of former medicine self, overcome and remedy the deficiency of the original formulation of agricultural chemicals, toxicity and excitant that the people is held are all lower, and can alleviate the poisoning to crop, improve physico chemistry and biological property, enlarge range of application, prolong the service life of medicament etc.
Microemulsion (Microemulsion) is one of novel form that meets the agricultural chemicals developing direction, and international code name: the ME of formulation is that water, water-insoluble and water-soluble substance are formed, and former medicine is with the microparticulate preparation wherein of 0.01-0.1u.He is a stable homogeneous phase on the thermodynamics, the solubility system.Outward appearance is transparence, and microcosmic is to be the limiting condition that aqueous emulsion fully disperses for the big micellar dispersion that expands.Its physics, chemical stability are good, strong to plant and insect tissue cell permeability, the absorption ratio height, and preventive effect is good, simultaneously, has production, storing and safe in utilization, and environmental pollution is little, helps the improvement of ecotope.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of cyhalofop-butyl microemulsion.
Another object of the present invention is to adopt easy processing technology, and less equipment prepares that a kind of long-term storage is stable, can evenly disperse in the water, the O/W type cyhalofop-butyl liquid formulation-microemulsion of good fluidity.Microemulsion is the dispersion that a kind of water-oil-surfactant is formed, different with general emulsion is that its outward appearance is transparent or approximate transparent homogeneous liquid, disperse phase is dispersed in the water with ultrafine particle (being generally 0.1-0.01um), and belonging to heating power needs stabilising system.O/W type microemulsion be with oil-soluble agricultural chemicals as disperse phase, water is made the microemulsion system of continuous phase.The preparation of microemulsion and selected pesticide species relation are very big, stable and the required surfactant of different cultivars agricultural chemicals in aqueous medium is not exclusively the same, therefore, the problem that is run into during preparation is also different, the method more complicated of dealing with problems must be solved at the specific question of each kind.The present invention utilizes micro-emulsion technology, the kind and the compatibility thereof of different surfaces activating agent have been studied, and to low temperature crystallization that this system produced caking and frozen glue, problems such as active ingredient cyhalofop-butyl decomposition of heat storage back and the distinctive transparency temperature range size of microemulsion are furtherd investigate, finally select suitable formula combination, cyhalofop-butyl, solvent, surfactant and water have been made stable cyhalofop-butyl microemulsion of storage period.The present invention is achieved in that the composition of this agricultural chemicals cyhalofop-butyl microemulsion comprises: with the cyhalofop-butyl is active component, is equipped with organic solvent, surfactant and water, and its outward appearance is transparent homogeneous liquid, forms proportioning and comprises:
The former medicine 2-20% of cyhalofop-butyl (weight)
Organic solvent 5-30% (weight)
Surfactant 5-30% (weight)
Water is supplied
Organic solvent among the present invention is: the compound use of one or two or more kinds in methyl alcohol, ethanol, dimethyl formamide, dimethyl sulfoxide (DMSO), N-Methyl pyrrolidone, cyclohexanone, toluene, dimethylbenzene, the benzene.Described surfactant is one or more the compound uses in alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy polyethenoxy ether, castor oil ethylene oxide adduct, alkylphenol polyoxyethylene formaldehyde condensation products, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyethenoxy ether phosphate, calcium dodecyl benzene sulfonate, the neopelex.Described water is natural water, running water, demineralized water or distilled water.
The bleeding agent maleic acid di-sec-octyl sodium sulfonate that can add 0-10% (weight) in the cyhalofop-butyl microemulsion of the present invention, sodium sulfonic acid succinic acid dialkyl.
The thickener that can add 0-10% (weight) in the cyhalofop-butyl microemulsion of the present invention, thickener are sodium cellulose glycolate, sodium carboxymethyl starch, polyvinylpyrrolidone, polyvinyl alcohol.
The cosurfactant that can add 0-10% (weight) in the cyhalofop-butyl microemulsion of the present invention, cosurfactant are C
3-C
10Alcohols, comprise n-butanol, n-amyl alcohol, isoamyl alcohol, propyl alcohol.
The preparation method of cyhalofop-butyl microemulsion of the present invention makes cyhalofop-butyl solution with the former medicinal organic solvent dissolving of cyhalofop-butyl, add surfactant and water again, dispersed with stirring is even, or with surfactant and water mixed dissolution, generate water, again that cyhalofop-butyl solution adding water dispersed with stirring is even.
Equipment of the present invention can be selected enamel reaction still, stainless steel mixing kettle or homogeneous mixer etc., and preparation technology is very simple, convenient.
The prepared cyhalofop-butyl microemulsion outward appearance of the present invention is a light yellow transparent liquid, and when-5-60 ℃ of storage, outward appearance is constant, and said preparation can disperse the transparent homogeneous liquid of formation naturally in water.Because the agricultural chemicals particle miniaturization of microemulsion is generally 0.1-0.01um, so the plant of plant is had stronger permeability.
Embodiment
With embodiment content of the present invention is further described below.
Table 1. instantiation
Pertinence pipette method and result
(1) mensuration of transparency temperature scope:
The appearance transparent of microemulsion is relevant with temperature, and the transparency temperature scope is the temperature range when indicating preparation and can keep pellucidity.This interval should meet product storage, the temperature condition when using.And the transparency temperature range size is directly relevant with the prescription composition with interval position, so these performance indications also are to weigh the importance of preparation product quality.
Assay method: get cyhalofop-butyl microemulsion 30mL in the 50mL vial, place ice bath, cooling gradually under agitation, the temperature T when the record sample is white in color muddy shape
1, slowly heating up with 2 ℃/minute speed again, sample becomes transparence, continues to heat up the temperature T when the record sample is white in color muddy shape once more
2, T then
1-T
2The interval be the transparency temperature scope.Measurement result is listed in the table 2.
(2) heat storage stability test:
Sample thief 10ml is sealed in the ampoule bottle, deposits 14 days in 54 ± 2 ℃ of constant temperature ovens, takes out.
1. observe appearance change; 2. the content of cyhalofop-butyl in the working sample, and with original content contrast, calculate resolution ratio.Measurement result is listed in the table 2.
(3) low-temperature test;
Sample was preserved 24 hours in 0-5 ℃.Observe appearance change, the results are shown in Table 2.
(4) dispersed mensuration:
Sample thief 1ml adds and to fill in the 50ml342PPM hard water color-comparison tube, observes dispersion phenomenon, and fluctuates after 15 times, places 30min in 30 ℃, observes the stable case of dispersion liquid, and measurement result is listed in the table 2.
The cyhalofop-butyl microemulsion of above presentation of results gained of the present invention all can keep the outward appearance homogeneous transparent at-5-60 ℃, good dispersion in water, and storage-stable has reached purpose of the present invention.
Table 2: performance measurement result
Claims (7)
1, a kind of preparation method of cyhalofop-butyl microemulsion, it is characterized in that composition comprises: with the cyhalofop-butyl is active component, is equipped with organic solvent, surfactant and water, its outward appearance is transparent homogeneous liquid, forms proportioning to be:
Cyhalofop-butyl 2-20% (weight)
Organic solvent 5-30% (weight)
Surfactant 5-30% (weight)
Water is supplied (weight).
2, cyhalofop-butyl microemulsion according to claim 1 is characterized in that: described organic solvent is one or two or more kinds the compound use in methyl alcohol, ethanol, dimethyl formamide, dimethyl sulfoxide (DMSO), N-Methyl pyrrolidone, cyclohexanone, toluene, dimethylbenzene, the benzene.Described surfactant is one or more the compound uses in alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy polyethenoxy ether, castor oil ethylene oxide adduct, alkylphenol polyoxyethylene formaldehyde condensation products, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyethenoxy ether phosphate, calcium dodecyl benzene sulfonate, the neopelex.Described water is natural water, running water, demineralized water or distilled water.
3, cyhalofop-butyl microemulsion according to claim 1 and 2, it is characterized in that: add the antifreezing agent of 2-10% (weight) in microemulsion, antifreezing agent is for choosing any one kind of them from ethylene glycol, propane diols, glycerine, polyethylene glycol, isopropyl alcohol, urea or several.
4, cyhalofop-butyl microemulsion according to claim 1 and 2 is characterized in that: add the bleeding agent maleic acid di-sec-octyl sodium sulfonate of 0-10% (weight) in microemulsion, sodium sulfonic acid succinic acid dialkyl.
5, cyhalofop-butyl microemulsion according to claim 1 and 2 is characterized in that: add the thickener of 0-10% (weight) in microemulsion, thickener is sodium cellulose glycolate, sodium carboxymethyl starch, polyvinylpyrrolidone, polyvinyl alcohol.
6, cyhalofop-butyl microemulsion according to claim 1 and 2 is characterized in that: add the cosurfactant of 0-10% (weight) in microemulsion, cosurfactant is C
3-C
10Alcohols, comprise n-butanol, n-amyl alcohol, isoamyl alcohol, propyl alcohol.
7, a kind of preparation method of agricultural chemicals cyhalofop-butyl, it is characterized in that: the former medicinal organic solvent dissolving of cyhalofop-butyl is made cyhalofop-butyl solution, add surfactant and water again, dispersed with stirring is even, or with surfactant and water mixed dissolution, generate water, again that cyhalofop-butyl solution adding water dispersed with stirring is even.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810101937A CN101530082A (en) | 2008-03-14 | 2008-03-14 | Preparation method of cyhalofop-butyl microemulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810101937A CN101530082A (en) | 2008-03-14 | 2008-03-14 | Preparation method of cyhalofop-butyl microemulsion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101530082A true CN101530082A (en) | 2009-09-16 |
Family
ID=41101099
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810101937A Pending CN101530082A (en) | 2008-03-14 | 2008-03-14 | Preparation method of cyhalofop-butyl microemulsion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101530082A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102726420A (en) * | 2012-07-12 | 2012-10-17 | 安徽美兰农业发展股份有限公司 | Cyhalofop-butyl-fenoxaprop-p-ethyl microemulsion and preparation method thereof |
| CN105360113A (en) * | 2015-12-04 | 2016-03-02 | 兰州交通大学 | Preparation method for synergistic pesticide microemulsion |
| CN107787964A (en) * | 2017-04-25 | 2018-03-13 | 惠州市银农科技股份有限公司 | It is a kind of using cyhalofop-butyl as microemulsion of active ingredient and preparation method thereof |
-
2008
- 2008-03-14 CN CN200810101937A patent/CN101530082A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102726420A (en) * | 2012-07-12 | 2012-10-17 | 安徽美兰农业发展股份有限公司 | Cyhalofop-butyl-fenoxaprop-p-ethyl microemulsion and preparation method thereof |
| CN105360113A (en) * | 2015-12-04 | 2016-03-02 | 兰州交通大学 | Preparation method for synergistic pesticide microemulsion |
| CN107787964A (en) * | 2017-04-25 | 2018-03-13 | 惠州市银农科技股份有限公司 | It is a kind of using cyhalofop-butyl as microemulsion of active ingredient and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102027900B (en) | Synergist and synergist-containing diquat aqueous solution | |
| CN104115848B (en) | Compound pesticide composition containing florasulam and picloram or its salt, preparation and application | |
| CN103283778A (en) | Weeding composition comprising glufosinate and saflufenacil | |
| CN102318632A (en) | Synergistic weeding composition containing fluroxypyr | |
| CN105230652A (en) | Weed-killing composition containing haloxyfop-P-methyl and glyphosate | |
| CN103783076B (en) | A kind of mixed herbicide containing glyphosate, two careless ether and methoxone and application thereof | |
| CN103609582A (en) | Topramezone and halosulfuron-methyl containing phytocidal composition | |
| CN100562252C (en) | A kind of herbicidal composition | |
| CN104542645A (en) | Weeding composition containing pyroxsulam, chodinafop-propargyl and fluroxypyr | |
| CN103250722B (en) | A kind of composition pesticide containing bromoxynil octanoate | |
| CN101530082A (en) | Preparation method of cyhalofop-butyl microemulsion | |
| CN102027929B (en) | Herbicidal composition containing haloxyfop-R-methyl and quizalofop-p-ethyl and application thereof | |
| CN101336632B (en) | Composite synergistic herbicide for controlling weeds in cornfield | |
| CN102204559A (en) | Agricultural chemical composite herbicide containing cyhalofopbutyl | |
| CN103109848A (en) | Glyphosate-containing weeding composition | |
| CN103300008B (en) | A kind of Synergistic herbicide compositions of containing chlorine fluorine pyrrole fluoroacetic acid | |
| CN103229773B (en) | Complex herbicidal composition | |
| CN102077834A (en) | Microcapsule suspension concentrate for preventing and removing rice paddy weed and preparation method thereof | |
| CN103238607B (en) | The Herbicidal combinations of a kind of Han isoxazole humulone and fluroxypyr | |
| CN103371158B (en) | A kind of Herbicidal combinations containing AC322140 | |
| CN104920396A (en) | Weeding composition containing pinoxaden and pyraflufen-ethyl | |
| CN104304278A (en) | Mixed herbicide containing cloransulam-methyl and bentazone and preparation method thereof | |
| CN105076146A (en) | Weeding composition containing haloxyfop-R-methyl and saflufenacil | |
| CN102396463A (en) | Weeding combination containing pyraflufen-ethyl and diphenyl ether compound | |
| CN104304273A (en) | Mixed herbicide containing cloransulam-methyl and metolachlor and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20090916 |