CN101836626A - Fluazinam-containing pesticide suspension concentrate and preparation method thereof - Google Patents
Fluazinam-containing pesticide suspension concentrate and preparation method thereof Download PDFInfo
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- CN101836626A CN101836626A CN 201010173065 CN201010173065A CN101836626A CN 101836626 A CN101836626 A CN 101836626A CN 201010173065 CN201010173065 CN 201010173065 CN 201010173065 A CN201010173065 A CN 201010173065A CN 101836626 A CN101836626 A CN 101836626A
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- fluazinam
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Abstract
The invention discloses a fluazinam-containing pesticide suspension concentrate and a preparation method thereof. The fluazinam-containing pesticide suspension concentrate mainly comprises the following components by weight percent: 50.0% of fluazinam, 3.5% of alkyl aryl polyoxyethylene ether phosphate, 0.15% of thickening agent WJZ-04, 3% of defoamer 8431, 6.0% of antifreeze ethylene glycol and the balance of water. Through the lower temperature and thermal storage stability test, the appearance of the suspension concentrate has no obvious layering, the dispersion in water is good, and each index reaches the related standards of the suspension concentrate. The suspension concentrate takes water as a dispersion medium, and the problems of flammability and injury generated by an organic solvent do not occur. The suspension concentrate has better dispersion and spread performance, high suspension rate, strong adhesion capacity to the surfaces of plants, and rain erosion resistance, and thereby, the drug effect is more obvious and durable compared with the wet powder, and is simultaneously more favorable for protecting natural environment so as to reduce the damage to the environment.
Description
Technical field
The invention belongs to the organic agricultural chemicals applied technical field, relate to the formulations of pesticide that contain fluazinam, especially a kind of pesticide suspension concentrate that contains fluazinam and preparation method thereof and application.
Background technology
21st century, the use of agricultural chemicals is still one of human main means of struggling with disease pest and weed in agricultural production.A large amount of uses along with agricultural chemicals, a large amount of organic solvents have caused pollution to environment, continuous enhancing along with people's environmental consciousness and security knowledge, at present, the formulations of pesticide develop towards the direction of water baseization, spheroidizing, slow release, multi-functional, laborsavingization and environment-friendly type, and particularly the formulation of aqueous suspension agent more and more is subjected to making a pet of of people and payes attention to.Pesticide suspension concentrate (Suspension Concentrate, SC) be a kind of be the environment amenable environment-protection pesticide formulation of medium with water, be by some auxiliary agent by the solid pesticide that is insoluble to or is slightly soluble in water, adopt the wet method ultramicro grinding to be scattered in more equably in the water, form the very thin higher suspension of a kind of particle diameter, can flow, stable liquid-solid attitude preparation.Because pesticide suspension concentrate has good Environmental compatibility, drug effect height, cost is low and it is safe in utilization to process, and shows one's talent in water base property preparation, has very big development potentiality.
External at present existing hundreds of suspending agent exploitations are put into production, but in China, conventional dosage forms such as missible oil, wetting powder, pulvis still have comparative advantage, aqueous suspension agent is less, and have stable inadequately problem mostly, the made pesticide suspension concentrate that contains fluazinam of the present invention is through low temperature and heat storage stability experiment, and outward appearance does not have obvious layering, favorable dispersibility in the water, every index meets the suspending agent relevant criterion.The present invention will play certain impetus to the development of China's formulations of pesticide, and the application of its invention also can bring good economic benefits to enterprise.
The fluazinam chemical name is 3-chloro-N-(3-chloro-5-trifluoromethyl-2-pyridine radicals)-α, α, α-three fluoro-2,6-dinitro-para-totuidine.Fluazinam has the bactericidal activity of wide spectrum.To interlink spore genus, Botrytis, Phytophthora, Plasmopara, Sclerotinia with black to cultivate the Pseudomonas bacterium very effective, Botrytis cinerea to anti-benzimidazole type and dicarboximide class biocide agent also has good result, have the effect of good control phytophagous mites concurrently, the crucifer club root also there is remarkable preventive effect, to good preventive effect also being arranged by the microbial paddy rice damping off of head mold.Its molecular formula is: C
13H
4Cl
2F
6N
4O
4, structural formula is as follows:
Summary of the invention
An object of the present invention is to provide a kind of pesticide suspension concentrate that contains fluazinam.
Another object of the present invention provides a kind of the contain preparation method of fluazinam pesticide suspension concentrate and the application of controlling plant diseases aspect thereof.For achieving the above object, technology contents disclosed by the invention is as follows:
A kind of pesticide suspension concentrate that contains fluazinam is characterized in that it is made up of following raw material:
Fluazinam 40～50%,
Wetting dispersing agent 1～10%,
Stabilizing agent 0.01～0.06%,
Antifreezing agent 1～8%,
Thickener 0.1～1%,
Defoamer 0.1～1%,
Water complements to 100%;
The pesticide suspension concentrate that the present invention is more preferably is made up of following raw material: 50.0% fluazinam, 10% neopelex, 0.06% stabilizing agent sodium sorbate, 0.2% thickener modification xanthans, 0.1% defoamer, 8431,6.0% antifreeze glycols, water complements to 100%.Wherein suspend particle diameter at 2～5 μ m.
Pesticide suspension concentrate of the present invention, wetting dispersing agent wherein are alkylaryl polychloroprene APEO, calcium dodecyl benzene sulfonate, nonyl phenol formaldehyde resin APEO, calcium lignosulfonate, polyoxyethylene nonylphenol ether or alkylaryl polyoxyethylene ether phosphate.
Stabilizing agent wherein is sodium sorbate, potassium sorbate or calcium sorbate; Thickener is xanthans XG, WJZ-04 or CMC.
Antifreezing agent wherein is glycerine or ethylene glycol; Defoamer is a silicone 8431.
The preparation method of pesticide suspension concentrate of the present invention is characterized in that being undertaken by following step
(1) according to the prescription requirement, former medicine fluazinam, stabilizing agent, wetting dispersing agent, antifreezing agent, defoamer and water mixing are sized mixing, pre-dispersed with high-shear emulsion machine;
(2) the gained slurry is moved into the sand milling jar, feeds cooling water and carry out sand milling, sand milling to the suspension particle diameter of material after 2～5 μ m reach 98% or more, filtration, slurry is standby;
(3) thickener is mixed with the aqueous solution (1～2%) of different proportion, joins in the slurry after the filtration, the qualified finished product that is is detected in the debugging back.
Screening process to fluazinam suspending agent prescription of the present invention is described in further detail below:
1 experiment material and method
1.1 experiment material
The former medicine of fluazinam: yellow crystal powder, effective component content 95%.
Wetting dispersing agent: alkylaryl polychloroprene APEO, calcium dodecyl benzene sulfonate, nonyl phenol formaldehyde resin APEO, calcium lignosulfonate, polyoxyethylene nonylphenol ether, alkylaryl polyoxyethylene ether phosphate.
Thickener: xanthans XG, WJZ-04, CMC.
Antifreezing agent: glycerine, ethylene glycol.
Defoamer: 8431.
1.2 experimental instrument
Sand mill (0.1L, 0.3L, 1.5L), laboratory high speed shear mulser, NDJ-1 viscosimeter, PH meter, laboratory centrifuge, laser granulometry.
1.3 experimental technique
Adopt wet method sand milling ultramicro grinding.According to the prescription requirement, former medicine, auxiliary agent and water mixed sizes mixing, with high-shear emulsion machine pre-dispersed after, slurry is moved into the sand milling jar, feed cooling water and carry out sand milling, sand milling to the particle diameter of material qualified after, filter, standby.Thickener is mixed with the aqueous solution of different proportion, joins in the slurry after the filtration, the qualified finished product that is is detected in the debugging back.
1.4 the mensuration of aqueous suspension agent physicochemical property
The assay method of the dispersiveness of aqueous suspension agent, centrifugal stability, viscosity, pH value, pourability, suspensibility, cold storage stability, heat storage stability all carries out with reference to the suspending agent quality standard and the method for inspection in " formulations of pesticide processing book series " (third edition), and the fluazinam content analysis adopts liquid chromatography.
2 prescription screenings
2.1 the selection of wetting dispersing agent
The suspension system of pesticide suspension concentrate comes from a kind of thermodynamic unstable system between colloidal dispersion system and rough segmentation are loose.The particle diameter of aqueous suspension agent generally has several microns sizes, because particle diameter is very little, the surface free energy of particle is very big, easy adsorption-condensation between particle.In order to increase the stability of aqueous suspension agent; usually must add a certain amount of wetting dispersing agent; around dispersed phase particles, form firm diaphragm; or formation electric double layer; make the pesticide granules surface charging; mutually repel between charged particle and dispersion is tended towards stability, make it in storage process, not take place cohesion and knot end phenomenon.Even a small amount of layering is arranged, can become stable suspension system through shaking gently still, and have good in dispersiveness.
According to the physical and chemical performance of fluazinam and the research experience of similar products processing thereof, we select different nonionics and anion wetting dispersing agent to carry out screening (table 1)
Table 1 wetting dispersing agent is selected test (unit: %)
| Project % | ??1# | ??2# | ??3# | ??4# | ??5# | ??6# | ??7# | ??8# |
| Fluazinam % | ??50.5 | ??50.5 | ??50.5 | ??50.5 | ??50.5 | ??50.5 | ??50.5 | ??50.5 |
| Calcium lignosulfonate | ??7 | ??5.5 | ??4.0 | ??3 | ||||
| Polyoxyethylene nonylphenol ether | ??8.0 | |||||||
| The alkylaryl polyoxyethylene ether phosphate | ??3.5 | |||||||
| Calcium dodecyl benzene sulfonate | ??1.5 | ??2.5 | ??2.0 | ??1.5 | ??1.0 | |||
| Alkylaryl polyoxyethylene polyoxypropylene ether | ??2.5 | ??2.5 | ??4.0 | ??2.5 | ||||
| The nonyl phenol formaldehyde resin APEO | ??2.5 | ??3.5 | ??3.5 | ??2.5 | ||||
| Suspensibility | ??75 | ??83 | ??91 | ??72 | ??92 | ??88 | ??96 | ??91 |
| Dispersed | Can | Can | Can | Can | Can | Can | Very | Can |
| Centrifugal stability | Bad | Very | Bad | Bad | Bad | Bad | Very | Very |
| Heat storage stability | Difference | Difference | Difference | Difference | Difference | Difference | Can | Can |
2.2 the selection of thickener
The viscosity of suspending agent is a key factor that influences the product bin stability.Viscosity is too little, product easily layering after placement a period of time, easy caking; Viscosity is too big, and it is serious that product is difficult for toppling over wall built-up, brings difficulty for processing and use.In order to improve the pourability of product, improve suspensibility and bin stability, must make product that a suitable viscosity is arranged.For this reason, according to the experience of developing suspending agent in the past, on the basis of 7# prescription, we screen several thickeners and have carried out stability test, find to select for use WJZ-04 thickener effect better, and it the results are shown in Table 2.
The centrifugal stability of preparation is best during from The selection result as can be known, with XG (0.4%) and WJZ-04.But preparation viscosity is higher when adding 0.4%XG, is difficult for flowing and sticking wall; When adding WJ-04, formulation flows is better, so the final thickener of determining WJZ-04 as 50% fluazinam SC, its consumption is 0.2%.
Table 2 thickener is selected test
| The thickener kind | Consumption | Viscosity (mpa.s) | Centrifugal stability |
| ??XG | ??0.15 | ??275 | Bad |
| ??XG | ??0.4 | ??1350 | Excellent |
| ??WJZ-04 | ??0.10 | ??650 | Bad |
| ??WJZ-04 | ??0.15 | ??1050 | Excellent |
| ??WJZ-04 | ??0.18 | ??1300 | Bad |
| ??CMC | ??2.2 | ??375 | Bad |
| ??CMC | ??5.0 | ??750 | Very |
2.3 the selection of antifreezing agent
With water is the pesticide suspension concentrate of medium, and its prescription not only will be suitable for storing under the southern high-temperature condition and using, and will be suitable for storage and use under northern area cold.The former can add antifreezing agent less, and the latter must add an amount of antifreezing agent, to guarantee normal result of use.
We have done comparative trial to ethylene glycol, glycerine commonly used, and both consumptions are even to be 6.0%.When test found to make antifreezing agent with glycerine, though aqueous suspension agent outward appearance no change during cold storage mobilely obviously descends, and there was not this situation in ethylene glycol.Therefore, this formulation selection ethylene glycol is as antifreezing agent, and its consumption is 6.0%.
2.4 the selection of defoamer
The production technology of agricultural chemicals suspension agent adopts the multistage sand milling superfine grinding of wet method more, and a large amount of air is brought and be dispersed into to the dispersion impeller of high speed rotating into atomic little bubble, and the suspending agent volume is expanded rapidly.These micro-bubbles not only can influence viscosity (mobile variation), metering and packing, and will reduce production efficiency significantly.If can not froth breaking, this may make the creeping type become dilatant fluid.So, in pharmaceutical formulation, add a certain amount of defoamer, and require defoamer good intermiscibility to be arranged with each component of preparation.This prescription is characterized in that with 8431 defoaming effect is good, and good with each component intermiscibility of preparation, consumption is few, dosage 3.0%, and price is low.
Determining and checking of 3 optimization formulas
The technical indicator of 3.150% fluazinam aqueous suspension agent
Table 3 technical indicator
| Project | Index |
| Outward appearance | White, can flow, thick liquid. |
| Fluazinam content, % | 50.0 ± 2.5 |
| Suspensibility, % | 〉=90 |
| The pH value | 5.0～8.0 |
| Particle diameter (3～5 μ m) | 〉=90% |
| Pourability | Qualified |
| Heat storage stability | Qualified |
| Cold storage stability | Qualified |
3.2 preferential prescription is by intersection screening and heat storage stability test to former steps, obtained preferential prescription, its prescription is as follows: 50.0% fluazinam, 3.5% alkylaryl polyoxyethylene ether phosphate, 0.15% thickener WJZ-04,3% defoamer, 8431,6.0% antifreeze glycols, water complements to 100%.
Sample by preferential formulated detects its every technical indicator, its result such as table 4
Table 4 sample detection result
| Sequence number | The pH value | Suspensibility (%) | Particle diameter (μ m) | Pourability | Dispersed | Cold storage stability | Heat storage stability |
| ??1 | ??6.3 | ??96.2 | ??4.51 | Very | Very | Qualified | Qualified |
| ??2 | ??6.8 | ??96.7 | ??4.73 | Very | Very | Qualified | Qualified |
| ??3 | ??6.7 | ??95.9 | ??3.97 | Very | Very | Qualified | Qualified |
| ??4 | ??6.5 | ??95.4 | ??4.22 | Very | Very | Qualified | Qualified |
4. result
(1) it is as follows originally to have determined preferential prescription:
50.0% fluazinam, 3.5% alkylaryl polyoxyethylene ether phosphate, 0.15% thickener WJZ-04,3% defoamer, 8431,6.0% antifreeze glycols, water complements to 100%.
(2) this prescription detection effect is as follows:
Preparation is through low temperature and heat storage stability experiment, and outward appearance does not have obvious layering, favorable dispersibility in the water, and every index meets the suspending agent relevant criterion.
The good effect that contains the pesticide suspension concentrate of fluazinam provided by the invention is:
(1) formulation of change fluazinam is a suspending agent, and during use, no dust harzard is to operator and Environmental security.
(2) formulation of change fluazinam can make the peasant more convenient when using this product, and is quick.
(3) suspending agent is dispersion medium with water, and the inflammable and drug injury problem that is produced by organic solvent can not take place.
(4) dispersiveness of suspending agent and plate-out ability are all relatively good, the suspensibility height, and the ability that sticks to the plant corpus surface is more intense, resistance of rainwater washing against, thereby drug effect significantly and also compares lastingly than wetting powder.
(5) change the fluazinam formulation, help the conservation of nature environment, alleviate the destruction that environment is caused.
It is as shown in the table to change fluazinam pesticide suspension concentrate correlation technique index:
Description of drawings
Fig. 1 is pesticide suspension concentrate preparation flow figure.
Embodiment
In order to explain enforcement of the present invention more fully, provide following preparation method's embodiment.These embodiments only are to explain rather than limit the scope of the invention, raw materials used all have commercially available.
Embodiment 1-4
Embodiment 5
The preparation method of embodiment 1-4
(1) by the requirement of above-mentioned photograph prescription, former medicine 40～50% fluazinams, stabilizing agent, wetting dispersing agent, antifreezing agent, defoamer and water mixing are sized mixing, pre-dispersed with high-shear emulsion machine;
(2) the gained slurry is moved into the sand milling jar, feeds cooling water and carry out sand milling, sand milling to the suspension particle diameter of material after 2～5 μ m reach 98% or more, filtration, slurry is standby;
(3) thickener is mixed with the aqueous solution (1～2%) of different proportion, joins in the slurry after the filtration, the qualified finished product that is is detected in the debugging back.
Embodiment 6
The dispenser parameter:
The dispenser result:
| Title | 50% fluazinam | Blade | Stem | The potato piece |
| Potato | 27-33 milliliter/mu | The green and brown color spot point of water soaking mode disappears | The brown streak disappears | The potato piece is good |
| Potato | ??0 | The green and brown color spot point of water soaking mode | The brown streak | Puce bulk scab |
The present invention is after the preferred embodiment that describes in detail, being familiar with this technology personage can be well understood to, can carry out various variations and modification not breaking away under above-mentioned claim and the spirit, all foundations technical spirit of the present invention all belongs to the scope of technical solution of the present invention to any simple modification, equivalent variations and modification that above embodiment did.And the embodiment that the present invention also is not subject in the specification to be given an actual example.
Claims (8)
1. pesticide suspension concentrate that contains fluazinam is characterized in that it is made up of following raw material:
Fluazinam 40～50%,
Wetting dispersing agent 1～10%,
Stabilizing agent 0.01～0.06%,
Antifreezing agent 1～8%,
Thickener 0.1～1%,
Defoamer 0.1～1%,
Water complements to 100%; Wherein suspend particle diameter at 2～5 μ m.
2. the described pesticide suspension concentrate of claim 1 is characterized in that it is made up of following raw material:
Fluazinam 45～50%,
Wetting dispersing agent 5～10%,
Stabilizing agent 0.03～0.06%,
Antifreezing agent 6～8%,
Thickener 0.2～1%,
Defoamer 0.1～0.5%,
Water complements to 100%; Wherein suspend particle diameter at 2～5 μ m.
3. claim 1 or 2 described pesticide suspension concentrates, wetting dispersing agent wherein is alkylaryl polychloroprene APEO, calcium dodecyl benzene sulfonate, nonyl phenol formaldehyde resin APEO, calcium lignosulfonate, polyoxyethylene nonylphenol ether or alkylaryl polyoxyethylene ether phosphate.
4. the described pesticide suspension concentrate of claim 1, stabilizing agent wherein is sodium sorbate, potassium sorbate or calcium sorbate; Thickener is xanthans XG, WJZ-04 or CMC.
5. the described pesticide suspension concentrate of claim 1, antifreezing agent wherein is glycerine or ethylene glycol; Defoamer is an organic silicone 8431.
6. pesticide suspension concentrate as claimed in claim 1 or 2, it is characterized in that it is made up of following raw material: 50.0% fluazinam, 10% neopelex, 0.06% stabilizing agent sodium sorbate, 0.2% thickener modification xanthans, 0.1% defoamer, 8431,6.0% antifreeze glycols, water complements to 100%, and wherein particle diameter is at 2～5 μ m.
7. the preparation method of claim 1 or 2 described pesticide suspension concentrates is characterized in that being undertaken by following step
(1) by the requirement of above-mentioned photograph prescription, former medicine fluazinam, stabilizing agent, wetting dispersing agent, antifreezing agent, defoamer and water mixing are sized mixing, pre-dispersed with high-shear emulsion machine;
(2) the gained slurry is moved into the sand milling jar, feeds cooling water and carry out sand milling, sand milling to the suspension particle diameter of material after 2～5 μ m reach 98% or more, filtration, slurry is standby;
(3) thickener is mixed with 1～2% aqueous solution, joins in the slurry after the filtration, the qualified finished product that is is detected in the debugging back.
8. the described application of pesticide suspension concentrate aspect controlling plant diseases that contains fluazinam of claim 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108522512A (en) * | 2018-04-10 | 2018-09-14 | 江阴苏利化学股份有限公司 | A kind of anti-jump type fluazinam suspending agent and preparation method thereof |
| CN108770859A (en) * | 2018-07-04 | 2018-11-09 | 广西南宁益土生物科技有限责任公司 | A kind of bactericidal composition of containing fluazinam and thiram |
| CN117368056A (en) * | 2023-12-06 | 2024-01-09 | 山东则正医药技术有限公司 | Method for testing particle size and particle size distribution of azithromycin medicine |
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| TW440429B (en) * | 1994-08-12 | 2001-06-16 | Bayer Ag | Substituted biphenyloxazolines |
| TWI296619B (en) * | 2001-05-31 | 2008-05-11 | Nihon Nohyaku Co Ltd | |
| CN101380016A (en) * | 2008-08-22 | 2009-03-11 | 张少武 | Bactericidal composition containing fluazinan and thiophonate-methyl |
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2010
- 2010-05-17 CN CN 201010173065 patent/CN101836626A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW440429B (en) * | 1994-08-12 | 2001-06-16 | Bayer Ag | Substituted biphenyloxazolines |
| TWI296619B (en) * | 2001-05-31 | 2008-05-11 | Nihon Nohyaku Co Ltd | |
| CN101380016A (en) * | 2008-08-22 | 2009-03-11 | 张少武 | Bactericidal composition containing fluazinan and thiophonate-methyl |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108522512A (en) * | 2018-04-10 | 2018-09-14 | 江阴苏利化学股份有限公司 | A kind of anti-jump type fluazinam suspending agent and preparation method thereof |
| CN108770859A (en) * | 2018-07-04 | 2018-11-09 | 广西南宁益土生物科技有限责任公司 | A kind of bactericidal composition of containing fluazinam and thiram |
| CN117368056A (en) * | 2023-12-06 | 2024-01-09 | 山东则正医药技术有限公司 | Method for testing particle size and particle size distribution of azithromycin medicine |
| CN117368056B (en) * | 2023-12-06 | 2024-04-12 | 山东则正医药技术有限公司 | Method for testing particle size and particle size distribution of azithromycin medicine |
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Application publication date: 20100922 |