CN103329892B - Suspending agent of thifluzamide and tebuconazole composite pesticide and preparation method of suspending agent - Google Patents
Suspending agent of thifluzamide and tebuconazole composite pesticide and preparation method of suspending agent Download PDFInfo
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- CN103329892B CN103329892B CN201310292000.9A CN201310292000A CN103329892B CN 103329892 B CN103329892 B CN 103329892B CN 201310292000 A CN201310292000 A CN 201310292000A CN 103329892 B CN103329892 B CN 103329892B
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Abstract
The invention relates to the technical field of pesticide for controlling rice sheath blight diseases and false smut, in particular to a suspending agent of thifluzamide and tebuconazole composite pesticide and a preparation method of the suspending agent. The suspending agent is prepared by the following ingredients in parts by weight: 20 parts of thifluzamide, 32 parts of tebuconazole, 18 parts of emolsifier and 30 parts of solvent. The prepared suspending agent is obviously superior to products prepared according to other proportions in suspensibility, persistent foamability, wet sieving test, thermal stability and the like. Experiments verify that the cotoxicity coefficient of the suspending agent reaches 154.19, the suspending agent falls in an obvious synergistic action scope, and preparations mixed in other proportions cannot reach the obvious synergistic action scope. In addition, the actual toxicity of different proportions is not raised with theoretical toxicity, and no change law exists between the actual toxicity and the theoretical toxicity. The suspending agent of the thifluzamide and tebuconazole composite pesticide is suitable for controlling the rice sheath blight diseases and the false smut, and has good popularization and application values.
Description
Technical field
The present invention relates to rice sheath blight disease, false smut is prevented and treated technical field of pesticide, specifically relates to suspending agent of a kind of thifluzamide and Tebuconazole composite pesticide and preparation method thereof.
Background technology
At present, existing for preventing and treating the agricultural chemicals of rice sheath blight disease, false smut, for example Chinese patent " CN102630680 A " discloses a kind of " having microbicide compositions of synergistic effect and preparation method thereof ", wherein the weight ratio of thifluzamide and Tebuconazole is 15～40%:3～30%, and makes the various formulations that are suitable for spraying.Meanwhile, the weight ratio of the preferred thifluzamide of this composition pesticide and Tebuconazole is 5:1, makes its synergistic effect reach best.
Inventor is through long term test checking, and this composition pesticide exists following defect:
1), by disclosed several concrete proportionings in said composition are tested, find cannot play good control efficiency to the control of rice sheath blight disease, false smut.
2), for the disclosed several formulations of said composition, find all to exist the defect of different problems through verification experimental verification.For example, wetting powder easily causes and product bonding is difficult for dispersion suspension in water, or stops up shower nozzle, and the phenomenon such as reason precipitation in sprayer causes and sprays irregularly, easily makes that plant is local produces poisoning.
3), composite problem, measure and find by the disclosed several concrete proportionings of this composition pesticide being carried out to the test of virulence test, heat storage stability and mixture co-toxicity coefficient, cannot reach the notable synergistic effect of two kinds of medicaments.
Summary of the invention
One of object of the present invention is to provide the suspending agent of a kind of thifluzamide and Tebuconazole composite pesticide, and this suspending agent dosage form design is reasonable, good to rice sheath blight disease, false smut control efficiency, and can realize the notable synergistic effect of thifluzamide and Tebuconazole.
For achieving the above object, the present invention has adopted following technical scheme:
A suspending agent for thifluzamide and Tebuconazole composite pesticide, this suspending agent is made up of following component according to weight portion:
Thifluzamide: 20 parts;
Tebuconazole: 32 parts;
Emulsifier: 18 parts;
Solvent: 30 parts.
Meanwhile, the present invention can also be able to further realization by the following technical programs:
Preferably, described emulsifier is that calcium dodecyl benzene sulfonate, phenethyl phenol polyoxyethylene poly-oxygen propylene aether and alkyl phenol formaldehyde resin polyoxyethylene ether are that 3:8:7 is mixed according to weight ratio.
Described solvent is dimethylbenzene.
The suspending agent of thifluzamide of the present invention and Tebuconazole composite pesticide, its beneficial effect shows:
1) suspending agent that, prepared by the present invention is all obviously better than the prepared product of other proportionings at aspects such as suspensibility, lasting foaming characteristic, wet screening test etc. and heat storage stabilities.
2), by experiment checking, the co-toxicity coefficient when mixed with 1:1.6 proportioning with thifluzamide and Tebuconazole reaches 154.19, belong to notable synergistic sphere of action, and the mixed preparation of other proportioning all cannot reach notable synergistic sphere of action.Meanwhile, the actual toxicity of different proportionings does not promote along with the enhancing of theoretical toxicity, between actual toxicity and theoretical toxicity, there is no regular variation.
3), thifluzamide of the present invention and Tebuconazole composite pesticide suspending agent, can suitablely prevent and treat rice sheath blight disease, false smut, there is good application value.The dispenser phase should rest in rice sheath blight disease, false smut their early stage, to the even foliar spray of water; When dispenser, do not require water in field, dispenser after dew is dry; Strong wind sky or estimate rainfall in 1 hour, please don't dispenser.78 grams～109 grams/ha of its active ingredients of recommendation, or 10～14 grams/acre of dosings prevent and treat rice sheath blight disease, under recommended dose, occur without poisoning.Prevent and treat and use 3 times at most in rice sheath blight disease per season on paddy rice, the safety interval using on paddy rice is 25 days.
Another object of the present invention is to the preparation method of the suspending agent that a kind of thifluzamide and Tebuconazole composite pesticide are provided, by even to thifluzamide, Tebuconazole, emulsifier and solvent, rough lapping in colloid mill, again through sand mill fine lapping, filter, and control suspensibility >=90%, 75 μ m testing sieve percent of pass >=98%.
The preparation method of the suspending agent of thifluzamide of the present invention and Tebuconazole composite pesticide, preparation technology is comparatively easy, is easy to suitability for industrialized production.
Embodiment
Below optimal way of the present invention is described in further detail.
One, the selection of raw material
1., the former medicine of thifluzamide, Zhejiang Boshida Crop Technology Co., Ltd. provides, registration card number: PD20121866, former medicine content >=95%.
No. CAS: 130000-40-7, chemical name: 2', the bromo-2-methyl-4'-of 6'-bis-trifluoromethoxy-4-Trifluoromethyl-1,3-thiadiazoles-5-hydroxyl anilide, molecular weight: 528.06.Biologically active: sterilization, toxicity rank: belong to the low poison that waits.
Toxicity: rat acute per os LD
50>5000mg/kg, rat acute is through skin LD
50>5000mg/kg, rat acute sucks LC
50>5000mg/L air.There is moderate to stimulate to lagophthalmos eyeball, rabbit skin is had to minimal irritation.Salmonella reversion test feminine gender, micronucleus test showed negative.
Environment: quail, wild duck LC
50>5620mg/L (96h), giant sunfish LC
501.2mg/L (96h), carp 2.9mg/L (96h), rainbow trout 1.3mg/L (96h), water flea LC
502.9mg/L (48h).
Chemical property: sterling is white powdery solid, m.p.177.9～178.6 ℃, 20 ℃ time, in water, solvability is 1.6mg/L, distribution coefficient 4.1, pH value is to stablize for 5～9 o'clock.
2., Original Tebuconazole, Jiangsu Jiannong Agrochemical Co., Ltd. provides, registration card number: PD20082414, former medicine content 96%.
The key technical indexes, impurity title and content: mass fraction: >=96.0%, pH value: 4.5～7.0, dry loss of weight :≤2.0%, acetone insoluble matter :≤0.2%.
No. CAS: 107534-96-3, chemical name: (RS)-1-(4-chlorphenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-yl methyl) penta-3-alcohol, molecular weight: 307.8.
Biologically active: sterilization, toxicity rank: belong to low toxicity.
Chemical property: fusing point: approximately 102.4 ℃, vapour pressure (20 ℃): 0.013mPa, solvability (20 ℃): 32mg/L in water, carrene is greater than 200g/L, and hexane is less than 100mg/L, 50g/L～100g/L in isopropyl alcohol, toluene, stability: be 4～9,22 ℃ of hydrolysis DT in pH value
50be greater than 1 year.
3., calcium dodecyl benzene sulfonate, phenethyl phenol polyoxyethylene poly-oxygen propylene aether and alkyl phenol formaldehyde resin polyoxyethylene ether, Nanjing Teva-Chem. Co., Ltd. provides.Dimethylbenzene, Tianjin Supure Science and Technology Co., Ltd. provides.
Testing result, the heat storage stability result of the test of all technical of the prepared suspending agent of two, the preparation of the suspending agent of thifluzamide and Tebuconazole composite pesticide, and each embodiment.
Embodiment 1
Thifluzamide tebuconazole suspension concentrates, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Thifluzamide | 20 |
| Tebuconazole | 32 |
| Calcium dodecyl benzene sulfonate | 3 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 8 |
| Alkyl phenol formaldehyde resin polyoxyethylene ether | 7 |
| Dimethylbenzene | 30 |
Preparation method: thifluzamide, Tebuconazole, calcium dodecyl benzene sulfonate, phenethyl phenol polyoxyethylene poly-oxygen propylene aether, alkyl phenol formaldehyde resin polyoxyethylene ether and dimethylbenzene are mixed, rough lapping in colloid mill, then through sand mill fine lapping, filter.
Embodiment 2
Thifluzamide tebuconazole suspension concentrates, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Thifluzamide | 20.2 |
| Tebuconazole | 32.3 |
| Calcium dodecyl benzene sulfonate | 3.2 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 7.8 |
| Alkyl phenol formaldehyde resin polyoxyethylene ether | 6.7 |
| Dimethylbenzene | 29.8 |
Preparation method is with embodiment 1.
Embodiment 3
Thifluzamide tebuconazole suspension concentrates, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Thifluzamide | 20.5 |
| Tebuconazole | 31.6 |
| Calcium dodecyl benzene sulfonate | 2.7 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 8.3 |
| Alkyl phenol formaldehyde resin polyoxyethylene ether | 7.4 |
| Dimethylbenzene | 29.5 |
Preparation method is with embodiment 1.
Embodiment 4
Thifluzamide tebuconazole suspension concentrates, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Thifluzamide | 19.5 |
| Tebuconazole | 32.5 |
| Calcium dodecyl benzene sulfonate | 2.7 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 7.9 |
| Alkyl phenol formaldehyde resin polyoxyethylene ether | 7.3 |
| Dimethylbenzene | 30.1 |
Preparation method is with embodiment 1.
Embodiment 5
Thifluzamide tebuconazole suspension concentrates, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Thifluzamide | 19.7 |
| Tebuconazole | 31.8 |
| Calcium dodecyl benzene sulfonate | 3.3 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 8.2 |
| Alkyl phenol formaldehyde resin polyoxyethylene ether | 6.5 |
| Dimethylbenzene | 30.5 |
Preparation method is with embodiment 1.
The thifluzamide tebuconazole suspension concentrates that embodiment 1～5 is prepared, the testing result of product all technical is as shown in table 1, and product heat storage stability result of the test is as shown in table 2.
The testing result of a table 15 embodiment preparing product all technical
A table 25 embodiment preparing product heat storage stability result of the test
Can find out by table 1 and 2, product prepared by embodiment 1 is all obviously better than the prepared product of other embodiment at aspects such as suspensibility, lasting foaming characteristic, wet screening test etc. and heat storage stabilities.
Three, toxicological information
Thifluzamide Tebuconazole composite pesticide suspending agent, female/male 1467.3mg/kgBW, the 1710.7mg/kgBW of being respectively of rat acute per os; Acutely be greater than 2000mg/kg through skin; Rat acute sucks the female male 2000mg/m that is all greater than
3; In rabbit eyes irritant test, after eye drip, do not wash eye and present slight excitant, after eye drip, wash eye and all present slight excitant; Cavy acute skin irritation test is presented to nonirritant; To guinea pig skin sensitization rate (%)=0, belong to weak sensitizer.
According to China's pesticide toxicity grading criteria, thifluzamide Tebuconazole composite pesticide suspending agent belongs to hypotoxicity agricultural chemicals.
Four, the thifluzamide of different proportionings and the Tebuconazole action effect comparative trial to rice sheath blight disease
1, formula Design
According to weight ratios different between thifluzamide and Tebuconazole, be divided into successively totally 5 groups of 1:0.8,1:1.2,1:1.6,1:2,1:2.4.
2, assay method
1., pastille medium preparation
Treatment agent acetone solution, is mixed with mother liquor.Will test medicament and contrast medicament according to certain concentration gradient, add respectively through sterilizing and be cooled in the medium of 45 ℃ of left and right to mix, pour plate into, make pastille flat board.
2., Toxicological testing
Adopt mycelial growth rate method.At pastille, dull and stereotyped central authorities connect a bacterium dish, and mycelia down.25 ℃ of medium to blank bacterium colonies are covered with culture dish 2/3 when above, measure the colony diameter of each processing.Each bacterium colony is sent out and is measured 2 times by right-angled intersection, represents the size of bacterium colony with its mean.Calculate the inhibition of medicament to mycelial growth rate.
3., evaluation method:
The content (%) of toxicity index × B of content (the %)+B of toxicity index × A of theoretical toxicity index TTI=A in mixture in mixture
Co-toxicity coefficient is greater than 120, and showing has synergistic effect; Co-toxicity coefficient is greater than 150, shows to have notable synergistic effect; Be less than 80 and show there is antagonism; Between 80～120, show to have summation action.
3, measurement result
1., the thifluzamide toxicity test to rice sheath blight disease mixed with Tebuconazole the results are shown in Table 3.
Table 3 thifluzamide toxicity test result to rice sheath blight disease mixed with Tebuconazole
Can find out by table 3, in each determined different proportionings, the highest with the virulence of 1:1.6 proportioning, EC
50value is 0.0685 μ g/ml, EC
90value is 1.9159 μ g/ml, and bacteriostatic activity is obviously better than other proportioning groups, in addition, known by table 3, and along with the lifting of Tebuconazole relative amount, the comprehensive virulence of its mixture also has no regular variation.
2., the thifluzamide synergy reaction mixed with Tebuconazole
Co-toxicity coefficient is greater than 120, and showing has synergistic effect; Co-toxicity coefficient is greater than 150, shows to have notable synergistic effect; Be less than 80 and show there is antagonism; Between 80～120, show to have summation action.Its testing result is in table 4.
The synergy reaction that table 4 thifluzamide is mixed with Tebuconazole
Can find out by table 4, in 5 kinds of determined mixed preparations, the co-toxicity coefficient when mixed with 1:1.6 proportioning with thifluzamide and Tebuconazole reaches 154.19, belongs to notable synergistic sphere of action, and the mixed preparation of other proportioning all cannot reach notable synergistic sphere of action., can also draw by table 4, the actual toxicity of different proportionings does not promote along with the enhancing of theoretical toxicity meanwhile, between actual toxicity and theoretical toxicity, there is no regular variation.
Five, the control of rice sheath blight disease, false smut
Thifluzamide Tebuconazole composite pesticide suspending agent of the present invention, can suitablely prevent and treat rice sheath blight disease, false smut, has good application value.The dispenser phase should rest in rice sheath blight disease, false smut their early stage, to the even foliar spray of water; When dispenser, do not require water in field, dispenser after dew is dry; Strong wind sky or estimate rainfall in 1 hour, please don't dispenser.78 grams～109 grams/ha of its active ingredients of recommendation, or 10～14 grams/acre of dosings prevent and treat rice sheath blight disease, under recommended dose, occur without poisoning.Prevent and treat and use 3 times at most in rice sheath blight disease per season on paddy rice, the safety interval using on paddy rice is 25 days.
Six, paddy field residual data, result is as shown in table 5.
Residual quantity data after the dispenser of table 5 each department
Seven, environmental influence
Environmental influence data on paddy rice, particular content is as follows:
1, birds acute oral toxicity (LD
50): quail LD
50(7d)=441.82mg/kg body weight, belongs to high poison.
2, fish acute toxicity (LD
50or TLM): zebra fish (96h): LC
50=1.88mg/L belongs to medium poison.
3, water flea class acute toxicity: Daphnia magna EC
50(48h): 1.70mg/L, belongs to poisoning.
4, Acute Toxicity of Algae silkworm (LD
50or microgram/silkworm): green alga EC
50(96h): 2.10mg/L, belongs to poisoning.
5, honeybee acute oral toxicity (LD
50or microgram/honeybee) natural enemy and beneficial organism (LD
50): honeybee (LD
50or microgram/honeybee): honeybee per os LC
50(48h)=253.09mg/L, belongs to poisoning
6, the acute contact toxicity of bee: LD
50(48h) > 20.0ug/ honeybee, low toxicity.
7, natural enemy oophagous trichogrammae class acute toxicity: oophagous trichogrammae LC
50(24h) 35.58mg/L, risk.
8, silkworm class acute toxicity: LC
50(two ridges)=14.13mg/kg mulberry leaf, belong to high poison.
9, earthworm acute toxicity: Taihu Lake paddy soil LC
50(14d) 63.37mg/kg dry ground, belongs to low toxicity, black soil of Northeast China LC
50(14d) 77.57mg/kg dry ground, belongs to low toxicity.
Above-described embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various distortion and improvement that those of ordinary skills make technical scheme of the present invention, all should fall in the definite protection domain of the claims in the present invention book.
Claims (2)
1. a suspending agent for thifluzamide and Tebuconazole composite pesticide, is characterized in that: this suspending agent is made up of following component according to weight portion:
Thifluzamide: 20 parts;
Tebuconazole: 32 parts;
Emulsifier: 18 parts;
Solvent: 30 parts;
Described emulsifier is that calcium dodecyl benzene sulfonate, phenethyl phenol polyoxyethylene poly-oxygen propylene aether and alkyl phenol formaldehyde resin polyoxyethylene ether are that 3:8:7 is mixed according to weight ratio;
Described solvent is dimethylbenzene.
2. the preparation method of the suspending agent of thifluzamide and Tebuconazole composite pesticide as claimed in claim 1, it is characterized in that: by even to thifluzamide, Tebuconazole, emulsifier and solvent, rough lapping in colloid mill, again through sand mill fine lapping, filter, and control suspensibility >=90%, 75 μ m testing sieve percent of pass >=98%.
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|---|---|---|---|
| CN201310292000.9A CN103329892B (en) | 2013-07-12 | 2013-07-12 | Suspending agent of thifluzamide and tebuconazole composite pesticide and preparation method of suspending agent |
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| CN103329892B true CN103329892B (en) | 2014-05-28 |
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Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101828559B (en) * | 2010-06-02 | 2013-04-10 | 陕西上格之路生物科学有限公司 | Agricultural sterilizing composite containing thifluzamide |
| CN102630680A (en) * | 2012-04-10 | 2012-08-15 | 江苏东宝农药化工有限公司 | Bactericide composition with synergy and preparation method thereof |
| CN102657183A (en) * | 2012-04-12 | 2012-09-12 | 广西田园生化股份有限公司 | Thifluzamide-containing ultra low volume liquid formulation |
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Application publication date: 20131002 Assignee: Meilan innovation (Beijing) Polytron Technologies Inc Assignor: Anhui Meiland Agricultural Development Co., Ltd. Contract record no.: 2014990000327 Denomination of invention: Suspending agent of thifluzamide and tebuconazole composite pesticide and preparation method of suspending agent License type: Exclusive License Record date: 20140521 |
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