CN104770376A - Tetramycin and azoxystrobin containing sterilizing aqueous emulsion and preparation method thereof - Google Patents

Tetramycin and azoxystrobin containing sterilizing aqueous emulsion and preparation method thereof Download PDF

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Publication number
CN104770376A
CN104770376A CN201510199137.9A CN201510199137A CN104770376A CN 104770376 A CN104770376 A CN 104770376A CN 201510199137 A CN201510199137 A CN 201510199137A CN 104770376 A CN104770376 A CN 104770376A
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tetramycin
aqueous emulsion
fluoxastrobin
parts
bactericidal
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胡剑锋
沈学锋
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ZHEJIANG SHIJIA TECHNOLOGY CO LTD
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ZHEJIANG SHIJIA TECHNOLOGY CO LTD
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Abstract

The invention relates to the technical field of pesticide compounding and particularly relates to a tetramycin and azoxystrobin containing sterilizing aqueous emulsion and a preparation method thereof. According to the tetramycin and azoxystrobin containing sterilizing aqueous emulsion, effective ingredients of the sterilizing aqueous emulsion consist of tetramycin and azoxystrobin which are subjected to binary compounding; the sterilizing aqueous emulsion contains the following ingredients in parts by mass: 1-50 parts of tetramycin, 1-50 parts of azoxystrobin, 3-30 parts of emulsifying agent, 5-15 parts of solvent, 2-15 parts of stabilizing agent, 1-5 parts of anti-freezing agent, 0.1-8 parts of anti-foaming agent, 0.2-2 parts of thickening agent and the balance of water. The compounded sterilizing agent, which takes tetramycin and azoxystrobin as the effective ingredients, disclosed by the invention has an obvious synergistic effect, so that the generation of key drug resistance is retarded, the production cost and use cost are reduced, and thus, the compounded sterilizing agent can be applied to control on resistance diseases.

Description

A kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin and preparation method thereof
Technical field
The present invention relates to technical field of pesticide combination, particularly relate to a kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin and preparation method thereof.
Background technology
The fermentating metabolism product that tetramycin (tetramycin) is S. ahygroscopicus Wuzhou subspecies, fungicidal spectrum is wide, all has extremely strong killing action to three main kind of 26 kinds of known disease funguses such as mastigomycetes, sac fungi and Deuteromycotina fungies.Be suitable for the multiple fungi of various crop, the control of bacteriosis.Especially to fruit tree putrefaction disease spot defoliation; Rice blast; Root rot; Cucurbits fusarium wilt; Cotton verticillium wilt; Jujube tree rust; Fruit white rot of grape; Panax pseudoginseng black spot; Tealeaves tea gall, the fungal disease special efficacys such as forest rot, canker, gummosis, defoliation, woods seedling blight.
Fluoxastrobin is a kind of efficient, wide spectrum, new type bactericide; there is the multiple actions such as Uptake and translocation, prevention, protection, treatment; sprouting and the generation of nearly all mycota (Ascomycotina, Basidiomycotina, Mastigomycotina and Deuteromycotina) germ spore can be suppressed, also can control mycelial growth.And Spores can be suppressed to invade; there is good prolection; effectively control the various fungal diseases of the plants such as vegetables, fruit tree, flowers, as powdery mildew, downy mildew, scab, anthracnose, rust, epidemic disease, glume blight, net blotch, rice blast etc. comprehensively.Especially to powdery mildew of strawberry, melon powdery mildew, powdery mildew of cucumber, pear scab special efficacy.
In the real process of agricultural production, using chemical agent is the most effective means of control plant pest, but is the generation of disease drug resistance by the problem that chemical control disease the most easily produces.In the chemical control of bacteriosis, years of researches are carried out both at home and abroad, although some antibacterium medicaments have started to enter practical stage, but the medicament of chemosynthesis has cycle long, the shortcoming such as cost is high, toxicity is large, environmental pollution is serious, can not meet the requirement of agricultural sustainable development far away.And long-term use single pesticidal preparations continuously high dose, easily cause the problems such as the remaining of medicament, environmental pollution and resistance to pesticide resistance fungi development.And by contrast, exploitation is efficient with research, low toxicity, low-residual composite and mixture has small investment, the lead time is short and be subject to domestic and international attention, numerous and confused increasing develops dynamics.We are on the basis of lab screening and field trial, filter out tetramycin and Fluoxastrobin carries out composite, have obvious synergistic effect.And about tetramycin and Fluoxastrobin composite composition pesticide and apply and there is no people at present and reported.
Summary of the invention
Based on above situation, the object of the invention is to provide a kind of new and effective composition pesticide and preparation thereof, to powdery mildew of cucumber, downy mildew and fruit tree putrefaction disease spot defoliation; Rice blast; Root rot; Cucurbits fusarium wilt; Cotton verticillium wilt; Jujube tree rust; Fruit white rot of grape; Panax pseudoginseng black spot; Tealeaves tea gall, the fungal disease special efficacys such as forest rot, canker, gummosis, defoliation, woods seedling blight.
Technical scheme of the present invention is realized by following measures:
Contain a bactericidal aqueous emulsion for tetramycin and Fluoxastrobin, the active ingredient of this bactericidal aqueous emulsion is tetramycin and Fluoxastrobin binary built, comprises following component by mass fraction: tetramycin 1 ~ 50 part; Fluoxastrobin 1 ~ 50 part; Emulsifier 3 ~ 30 parts; Solvent 5 ~ 15 parts; Stabilizing agent 2 ~ 15 parts; Antifreezing agent 1 ~ 5 part; Defoamer 0.1 ~ 8 part; Thickener 0.2 ~ 2 part; Water, surplus.
As preferably, the mass ratio of tetramycin and Fluoxastrobin is 1 ~ 10: 50 ~ 1.
As preferably, the mass ratio of tetramycin and Fluoxastrobin is 1:10 ~ 10:1.
As preferably, emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, alkylphenol polyoxyethylene sulfosuccinate, styrylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, any one in polyoxyethylene aliphatic alcohol ether or more than one any mixtures than composition.
As preferably, described solvent is dimethylbenzene or biodiesel, toluene, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine-based vegetable oil code name is ND-45, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in water equal solvent are arbitrarily than the mixture of composition.
As preferably, described stabilizing agent is selected from sodium citrate, the one in resorcinol.
As preferably, described antifreezing agent is selected from ethylene glycol, propane diols, one or more in glycerine.
As preferably, described defoamer is selected from silicone oil, silicone compound, C10-20 saturated fat acid compounds, one or more of C8-10 fatty alcohol.
As preferably, described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, in polyvinyl alcohol one or more.
Prepare a preparation method for described bactericidal aqueous emulsion, first tetramycin and Fluoxastrobin, solvent, emulsifier are added together, make to be dissolved into uniform oil phase; By part water, antifreeze, defoamer, thickener, mix uniformly aqueous phase; While high-speed stirred, oil phase is added aqueous phase in a kettle., slowly add water until reach phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear about half an hour, form the aqueous emulsion of oil-in-water type, namely can be made into the aqueous emulsion of the present composition.
The composite bactericide that the present invention is active ingredient with tetramycin and Fluoxastrobin has obvious synergistic effect, delays the drug-fast generation in key, and reduces into product cost and use cost, can be used for the improvement of resistance disease.To powdery mildew of cucumber, downy mildew and fruit tree putrefaction disease spot defoliation; Rice blast; Root rot; Cucurbits fusarium wilt; Cotton verticillium wilt; Jujube tree rust; Fruit white rot of grape; Panax pseudoginseng black spot; Tealeaves tea gall, the fungal disease special efficacys such as forest rot, canker, gummosis, defoliation, woods seedling blight.
Embodiment
For making technical scheme of the present invention, object and advantage are clearly understood, the following specific embodiment of the present invention is described, but the present invention is not limited to these examples.The mode that effect experimental of the present invention adopts indoor biometrics and field trial to combine, if no special instructions, the ratio below mentioned is all ratio of quality and the number of copies.
Embodiment 1:
Contain a bactericidal aqueous emulsion for tetramycin and Fluoxastrobin, the active ingredient of this bactericidal aqueous emulsion is tetramycin and Fluoxastrobin binary built, tetramycin 10 parts; Fluoxastrobin 5 parts; Calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether 10 parts; Toluene 10 parts; Sodium citrate 5 parts; Ethylene glycol 3 parts; Silicone oil 2 parts; Xanthans 1 part; Water, surplus.
First tetramycin and Fluoxastrobin, solvent, emulsifier are added together, make to be dissolved into uniform oil phase; By part water, antifreeze, defoamer, thickener, mix uniformly aqueous phase; While high-speed stirred, oil phase is added aqueous phase in a kettle., slowly add water until reach phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear about half an hour, form the aqueous emulsion of oil-in-water type, namely can be made into the aqueous emulsion of the present composition.
Embodiment 2: tetramycin and Fluoxastrobin different ratio co-toxicity are tested.
1.1 test targets
From Taizhou of Zhejiang never executed tetramycin and Fluoxastrobin and cucumber of the same type potted plant gather and be separated, for examination cucumber variety: Chang Chun Mi Ci.
1.2 test method
By susceptible cucumber variety Chang Chun Mi Ci cultivation in pot for growing seedlings, be placed in greenhouse and cultivate, plant grows to three to four leaf after dates, gathers the blade of identical leaf age, for cultivation and the mensuration of cucumber powdery mildew's pathogen.
1.2.1 the cultivation of cucumber powdery mildew's pathogen and the preparation of spore suspension
Cucumber powdery mildew's pathogen adopt plants method 20 DEG C, cultivate under the condition of 12h alternation of light and darkness, every 30 d turn culture 1 time.With the conidium on sterile water wash-out incidence of leaf during inoculation, be mixed with the suspension that spore concentration is l × 106/mL.
1.2.2 strains tested sensitivity testing
Leaf dish moisturizing method is adopted to carry out toxicity test.First the blade of collection is prepared into the leaf dish that diameter is 1.5cm, random mixing, be placed in the series concentration liquid configured respectively and soak lh, each concentration 50 leaf dishes, test with the process of not adding medicine as blank, after immersion terminates, leaf faces up and puts on the blotting paper that identical liquor strength is wetting, liquid on leaf dish is blotted, the spore suspension l0L prepared is inoculated in leaf dish central authorities, after room temperature places 5 min, be placed in 20 DEG C, cultivate under the condition of 12h alternation of light and darkness, the onset area on leaf dish is measured after 10d, calculate EC50.
On the basis of preliminary experiment, carry out toxicity test respectively in order to upper method to single dose tetramycin and Fluoxastrobin, the two EC50 value is respectively 13.6574 ㎎/l and 10.2147 ㎎/l.
The percentage accounting for leaf disc area according to lesion area divides disease level
0 grade: anosis;
1 grade: sorus area accounts for less than 5% of whole leaf area;
3 grades: sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: sorus area accounts for more than 50% of whole leaf area.
1.2.3 mixture toxicity test and interpretation of result
Carry out the toxicity test of mixture according to mixed ratio by single dose toxicity test method.
If contrast lethality <5%, does not correct, contrast lethality, between 5%-20%, corrects by formula 2, and contrast lethality >20%, test need be reformed.
Be independent variable x with the logarithm value of drug concentration (mg/L), with the probability value of corrected mortality for dependent variable y, set up virulence regression equation formula respectively, the EC50 adopting DPS software to calculate single dose and each proportioning mixture calculates co-toxicity coefficient (CTC) according to the abundant method of Sun Yun.Co-toxicity coefficient CTC, computing formula is as follows: (take tetramycin as standard agent, its toxicity index is 100):
EC50 × 100 of the EC50/ Fluoxastrobin of toxicity index (the TI)=tetramycin of Fluoxastrobin
EC50 × 100 of the EC50/M of true toxicity index (the ATI)=tetramycin of M
TI × P Fluoxastrobin of TI × P tetramycin+Fluoxastrobin of theoretical toxicity index (the TTI)=tetramycin of M
TTI × 100 of the ATI/M of co-toxicity coefficient (the CTC)=M of M
In formula:
M is the mixture of tetramycin and Fluoxastrobin different ratio
P tetramycin is the ratio of tetramycin shared by mixture
P Fluoxastrobin is the ratio of Fluoxastrobin shared by mixture.
2.1 toxicity test results
Table 1 tetramycin and Fluoxastrobin are to the toxicity test of powdery mildew of cucumber
As can be seen from the table, the result of the test of different proportion proportioning shows, dilute respectively in active ingredient ratio and all show stronger synergistic effect, wherein with tetramycin: time Fluoxastrobin is 1:20 ~ 20:1, synergistic effect is best, suggestion carries out further field control effectiveness test to suitable proportion about 1:20 ~ 20:1 mixture preparation, to evaluate its field practical application effect.
3 field trials prevent and treat the experimental result of powdery mildew of cucumber, cucumber bacterial angular leaf spot
3.1 field trials prevent and treat powdery mildew of cucumber
3.1.1 test method
Test on Zhejiang Jiaxing city cucumber ground, 4 points are investigated in every community, and often some investigation 2 strains, record occurring degree by staging,
Grade scale is as follows:
0 grade: anosis;
1 grade: sorus area accounts for less than 5% of whole leaf area;
3 grades: sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: sorus area accounts for more than 50% of whole leaf area.
3.1.2 control time and number of times
Test altogether investigate 4 times, before medicine radix investigation, first time medicine after 7 days, second time 7 days and medicine after within 15 days, investigate.
3.1.3 drug effect computational methods
Sick leaf rate (%)=sick number of sheets/investigate the total number of sheets × 100
Disease index=Σ (the sick number of sheets × relative level numerical value at different levels)/(investigating the total number of sheets × 9) × 100
Control efficiency (%)=(before 1-(blank district medicine after disease index × treatment region medicine disease index)/(after blank district medicine before disease index × treatment region medicine disease index)) × 100.
3.1.4 poisoning investigation method
Whether after dispenser, continuous 15d estimates medicament has poisoning to crop.
3.1.5 result of the test and analysis
Each process prevents and treats the effect of powdery mildew of cucumber.(table 2)
The effect of powdery mildew of cucumber prevented and treated by table 2 respectively process
Control successful higher than tetramycin and Fluoxastrobin single dose with 24:24 ratio composite bactericide for powdery mildew of cucumber by known 48% tetramycin of table 2 and Fluoxastrobin, bactericidal effect increases progressively with the increase of dosage.According to field range estimation, within the scope of test dose, plant growth is normal, and the poisoning phenomenon to cucumber does not all appear in each treatment agent, illustrates that it is safe to cucumber, significant for agricultural produce, is worthy to be popularized.
3.2 field trial control cucumber bacterial angular leaf spots
3.2.1 test method
Test on Zhejiang Jiaxing cucumber ground, test kind is middle peasant No. 8, and often process 4 times and repeat, every community double diagonal line investigates 5 points, often some investigation 3 strain cucumber, and record occurring degree by staging, grade scale is as follows:
0 grade: anosis;
1 grade: scab heap area accounts for less than 5% of whole leaf area;
3 grades: scab heap area accounts for below the 6%-10% of whole leaf area;
5 grades: scab heap area accounts for below the 11%-20% of whole leaf area;
7 grades: scab heap area accounts for below the 21%-50% of whole leaf area;
9 grades: scab heap area accounts for more than 50% of whole leaf area.
3.2.2 control time and number of times
Test altogether investigate 4 times, before medicine radix investigation, first time medicine after 7 days, second time 7 days and medicine after within 15 days, investigate.
3.2.3 drug effect computational methods
Sick leaf rate (%)=sick number of sheets/investigate the total number of sheets × 100
Disease index=Σ (the sick number of sheets × relative level numerical value at different levels)/(investigating the total number of sheets × 9) × 100
Control efficiency (%)=(before 1-(blank district medicine after disease index × treatment region medicine disease index)/(blank
Disease index before disease index after district's medicine × treatment region medicine)) × 100.
3.2.4 poisoning investigation method
Whether after dispenser, continuous 15d estimates medicament has poisoning to crop.
3.2.5 result of the test and analysis
Table 3 different disposal prevents and treats measurement result to cucumber bacterial angular leaf spot
Shown by above field experiment, tetramycin and azoxystrobin compound preparation are obviously better than single dose for the preventive effect of cucumber bacterial angular leaf spot, and bactericidal effect increases progressively with the increase of dosage.According to field range estimation, within the scope of test dose, plant growth is normal, occurs without poisoning situation, significant for agricultural produce, is worthy to be popularized.
In sum, the present invention contains the bactericidal composition of tetramycin and Fluoxastrobin, has good control efficiency to powdery mildew of cucumber and cucumber bacterial angular leaf spot, and it is to Target crops safety.Complex preparation not only increases preventive effect, and expands the control to bacterium, so this compounded combination tool in production practices is of great significance.

Claims (10)

1. contain a bactericidal aqueous emulsion for tetramycin and Fluoxastrobin, it is characterized in that: the active ingredient of this bactericidal aqueous emulsion is tetramycin and Fluoxastrobin binary built, comprises following component by mass fraction: tetramycin 1 ~ 50 part; Fluoxastrobin 1 ~ 50 part; Emulsifier 3 ~ 30 parts; Solvent 5 ~ 15 parts; Stabilizing agent 2 ~ 15 parts; Antifreezing agent 1 ~ 5 part; Defoamer 0.1 ~ 8 part; Thickener 0.2 ~ 2 part; Water, surplus.
2. a kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin according to claim 1, is characterized in that: the mass ratio of tetramycin and Fluoxastrobin is 1 ~ 10: 50 ~ 1.
3. a kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin according to claim 1, is characterized in that: the mass ratio of tetramycin and Fluoxastrobin is 1:10 ~ 10:1.
4. a kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin according to claim 1, it is characterized in that: emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, alkylphenol polyoxyethylene sulfosuccinate, styrylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, any one in polyoxyethylene aliphatic alcohol ether or more than one any mixtures than composition.
5. a kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin according to claim 1, is characterized in that: described solvent is dimethylbenzene or biodiesel, toluene, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine-based vegetable oil code name is ND-45, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in water equal solvent are arbitrarily than the mixture of composition.
6. a kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin according to claim 1, is characterized in that: described stabilizing agent is selected from sodium citrate, the one in resorcinol.
7. a kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin according to claim 1, is characterized in that: described antifreezing agent is selected from ethylene glycol, propane diols, one or more in glycerine.
8. a kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin according to claim 1, is characterized in that: described defoamer is selected from silicone oil, silicone compound, C10-20 saturated fat acid compounds, one or more of C8-10 fatty alcohol.
9. a kind of bactericidal aqueous emulsion containing tetramycin and Fluoxastrobin according to claim 1, is characterized in that: described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, in polyvinyl alcohol one or more.
10. prepare a preparation method for the bactericidal aqueous emulsion described in claim 1 ~ 9 any one claim, it is characterized in that: first tetramycin and Fluoxastrobin, solvent, emulsifier are added together, make to be dissolved into uniform oil phase; By part water, antifreeze, defoamer, thickener, mix uniformly aqueous phase; While high-speed stirred, oil phase is added aqueous phase in a kettle., slowly add water until reach phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear about half an hour, form the aqueous emulsion of oil-in-water type, namely can be made into the aqueous emulsion of the present composition.
CN201510199137.9A 2015-04-24 2015-04-24 Tetramycin and azoxystrobin containing sterilizing aqueous emulsion and preparation method thereof Pending CN104770376A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105284949A (en) * 2015-12-05 2016-02-03 济南舜昊生物科技有限公司 Compound pesticide used for controlling powdery mildew of cucumbers
CN106577696A (en) * 2016-11-12 2017-04-26 广东中迅农科股份有限公司 Tetramycin-containing pesticidal composition
CN109221100A (en) * 2018-09-13 2019-01-18 绩溪农华生物科技有限公司 A kind of pesticide emulsion in water and preparation method thereof
CN110651784A (en) * 2018-06-28 2020-01-07 江苏龙灯化学有限公司 Preparation method of pesticide emulsion in water, emulsion in water prepared based on method and application of emulsion in water
CN110651782A (en) * 2018-06-28 2020-01-07 江苏龙灯化学有限公司 Pesticide aqueous emulsion and preparation method and application thereof

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US5145856A (en) * 1989-02-10 1992-09-08 Imperial Chemical Industries Plc Fungicides
CN103636623A (en) * 2013-11-28 2014-03-19 北京燕化永乐生物科技股份有限公司 Azoxystrobin-containing bactericidal composition
CN103651421A (en) * 2012-09-12 2014-03-26 青岛星牌作物科学有限公司 Bactericidal composition containing tetramycin and bismerthiazol and application of bactericidal composition
CN103651423A (en) * 2012-09-17 2014-03-26 青岛星牌作物科学有限公司 Bactericidal composition containing tetramycin and Xinjunan and application of bactericidal composition

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5145856A (en) * 1989-02-10 1992-09-08 Imperial Chemical Industries Plc Fungicides
CN103651421A (en) * 2012-09-12 2014-03-26 青岛星牌作物科学有限公司 Bactericidal composition containing tetramycin and bismerthiazol and application of bactericidal composition
CN103651423A (en) * 2012-09-17 2014-03-26 青岛星牌作物科学有限公司 Bactericidal composition containing tetramycin and Xinjunan and application of bactericidal composition
CN103636623A (en) * 2013-11-28 2014-03-19 北京燕化永乐生物科技股份有限公司 Azoxystrobin-containing bactericidal composition

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105284949A (en) * 2015-12-05 2016-02-03 济南舜昊生物科技有限公司 Compound pesticide used for controlling powdery mildew of cucumbers
CN106577696A (en) * 2016-11-12 2017-04-26 广东中迅农科股份有限公司 Tetramycin-containing pesticidal composition
CN110651784A (en) * 2018-06-28 2020-01-07 江苏龙灯化学有限公司 Preparation method of pesticide emulsion in water, emulsion in water prepared based on method and application of emulsion in water
CN110651782A (en) * 2018-06-28 2020-01-07 江苏龙灯化学有限公司 Pesticide aqueous emulsion and preparation method and application thereof
CN109221100A (en) * 2018-09-13 2019-01-18 绩溪农华生物科技有限公司 A kind of pesticide emulsion in water and preparation method thereof

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Application publication date: 20150715