CN102907436A - Ternary complex emulsifiable solution as well as preparation method and application thereof - Google Patents
Ternary complex emulsifiable solution as well as preparation method and application thereof Download PDFInfo
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- CN102907436A CN102907436A CN2012104519530A CN201210451953A CN102907436A CN 102907436 A CN102907436 A CN 102907436A CN 2012104519530 A CN2012104519530 A CN 2012104519530A CN 201210451953 A CN201210451953 A CN 201210451953A CN 102907436 A CN102907436 A CN 102907436A
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- Prior art keywords
- missible oil
- ternary built
- difenoconazole
- propiconazole
- tebuconazole
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000005760 Difenoconazole Substances 0.000 claims abstract description 50
- BQYJATMQXGBDHF-UHFFFAOYSA-N difenoconazole Chemical compound O1C(C)COC1(C=1C(=CC(OC=2C=CC(Cl)=CC=2)=CC=1)Cl)CN1N=CN=C1 BQYJATMQXGBDHF-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000005822 Propiconazole Substances 0.000 claims abstract description 49
- STJLVHWMYQXCPB-UHFFFAOYSA-N propiconazole Chemical compound O1C(CCC)COC1(C=1C(=CC(Cl)=CC=1)Cl)CN1N=CN=C1 STJLVHWMYQXCPB-UHFFFAOYSA-N 0.000 claims abstract description 49
- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000005839 Tebuconazole Substances 0.000 claims abstract description 45
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 18
- 235000009754 Vitis X bourquina Nutrition 0.000 claims abstract description 15
- 235000012333 Vitis X labruscana Nutrition 0.000 claims abstract description 15
- 235000014787 Vitis vinifera Nutrition 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 240000006365 Vitis vinifera Species 0.000 claims abstract 2
- 239000003795 chemical substances by application Substances 0.000 claims description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- 230000000740 bleeding effect Effects 0.000 claims description 16
- 235000013399 edible fruits Nutrition 0.000 claims description 13
- 150000001412 amines Chemical class 0.000 claims description 9
- 229920002521 macromolecule Polymers 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 5
- 208000019300 CLIPPERS Diseases 0.000 claims description 4
- 208000021930 chronic lymphocytic inflammation with pontine perivascular enhancement responsive to steroids Diseases 0.000 claims description 4
- 238000004945 emulsification Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000002528 anti-freeze Effects 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000010008 shearing Methods 0.000 abstract 1
- 241000219095 Vitis Species 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- 239000003814 drug Substances 0.000 description 8
- 201000010099 disease Diseases 0.000 description 7
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 7
- 230000032683 aging Effects 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 230000003449 preventive effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 241000221785 Erysiphales Species 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000004495 emulsifiable concentrate Substances 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 230000002045 lasting effect Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 206010039509 Scab Diseases 0.000 description 2
- 241000209140 Triticum Species 0.000 description 2
- 235000021307 Triticum Nutrition 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000035613 defoliation Effects 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000855 fungicidal effect Effects 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 241001530056 Athelia rolfsii Species 0.000 description 1
- 240000008790 Musa x paradisiaca Species 0.000 description 1
- 235000018290 Musa x paradisiaca Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000014443 Pyrus communis Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- -1 polyoxy ethyl ether Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a ternary complex emulsifiable solution, as well as a preparation method and application of the ternary complex emulsifiable solution. According to the ternary complex emulsifiable solution, environment-friendly solvent oil serves as the solvent; the solutes are as follows: 100 to 150g/L of difenoconazole, 100 to 150g/L of tebuconazole, 10 to 50g/L of propiconazole, 5 to 20g/L of an emulsifying agent, 1 to 5g/L of a penetrant, and 0.5 to 1g/L of an antifreeze, according to mass-volume concentration. The preparation method comprises the following steps of: (1) adding the environment-friendly solvent oil to a preparing kettle, and starting an agitator; (2) heating to reach temperature more than 60 DEG C, then sequentially adding difenoconazole, tebuconazole and propiconazole; (3) agitating for 0.5 hour, then sequentially adding the emulsifying agent, the penetrant and the antifreeze, and starting a shearing machine to shear and emulsify, and finally stopping agitating; and (4) standing for more than 2 hours, and filtering to obtain the ternary complex emulsifiable solution. The ternary complex emulsifiable solution can effectively control grape white rot, and is safe to use, and simple in preparation technology.
Description
Technical field
The present invention relates to a kind of agricultural bactericidal agent formulation and its preparation method and application, specifically relate to a kind of missible oil that is formed by Difenoconazole, propiconazole and Tebuconazole ternary built and its preparation method and application.
Background technology
Difenoconazole, Tebuconazole and propiconazole are triazole bactericidal agent, the sterilization wide spectrum, can effectively prevent and treat powdery mildew, loose kernel smut, rust, the root rot of wheat, the banded sclerotial blight of paddy rice, bakanae disease, the leaf spot of banana, the spot defoliation of apple, pear scab, the white rot of grape, anthracnose etc.Yet use separately above-mentioned arbitrary single dose to exist the control target single, easily develop immunity to drugs, and the problem such as the lasting period is short.
Summary of the invention
For solve the chemical control target that prior art exists single, easily develop immunity to drugs, the problem such as the lasting period is short, the invention provides a kind of ternary built missible oil and its preparation method and application, effectively enlarge fungicidal spectrum, delayed crop to the pesticide resistance of medicament, improved the lasting effect of dispenser.
Technical scheme of the present invention is: a kind of ternary built missible oil, and the solvent in described ternary built missible oil is the environment-friendly type solvent, solute is Difenoconazole, Tebuconazole, propiconazole, emulsifier, bleeding agent and antifreezing agent; Quality-the volumetric concentration of described each solute is as follows: Difenoconazole: 100~150 g/L, Tebuconazole: 100~150 g/L, propiconazole: 10~50 g/L, emulsifier: 5~20g/L, bleeding agent: 1~5g/L, antifreezing agent: 0.5~1g/L.
Preferred version is: the quality-volumetric concentration of described each solute is as follows: Difenoconazole: 140~150 g/L, Tebuconazole: 140~150 g/L, propiconazole: 30~50 g/L, emulsifier: 5~20g/L, bleeding agent: 1~5g/L, antifreezing agent: 0.5~1g/L.
Described bleeding agent is poly-trisiloxanes, is digested by Guangzhou West that work technology Co., Ltd produces, and its model is the poly-trisiloxanes of 810c.
Described antifreezing agent is ethylene glycol.
Described environment-friendly type solvent naphtha is JEFFSOL AG1730 macromolecule organic amine, by system river, Shanghai Chemical Manufacture.
Described emulsifier is APEO, is to be produced by the agricultural chemical industry of Heze City, Shandong Province Co., Ltd.
A kind of preparation method who prepares the above-mentioned ternary built missible oil of claim, its preparation process is as follows:
(1) add the environment-friendly type solvent naphtha that measures in the preparation still, start agitator;
(2) more than temperature raising to 60 ℃, beginning adds Difenoconazole, Tebuconazole and the propiconazole that measures successively;
(3) stir after 0.5 hour, add successively emulsifier, bleeding agent, antifreezing agent starts clipper and carries out emulsification pretreatment and stop after two hours stirring;
(4) standing filtration more than 2 hours, namely get ternary built missible oil.
Described ternary built the missible oil application in preventing and treating fruit white rot of grape, particularly 350g/L(Difenoconazole 150g/L, propiconazole 50g/L, Tebuconazole 150g/L) ternary built missible oil is remarkable for the fruit white rot of grape control efficiency.
Beneficial effect:
The ternary built missible oil drug effect that the present invention makes is high, production cost is low, use safety, and preparation technology is simple, and its control efficiency that is applied to fruit white rot of grape is remarkable, saves cost, and environmental contamination reduction has significant Social benefit and economic benefit.
Embodiment
The invention will be further described by embodiment, but protection scope of the present invention is not limited to this.
A kind of ternary built wetting powder, the solvent in its ternary built missible oil is the environment-friendly type solvent, solute is Difenoconazole, Tebuconazole, propiconazole, emulsifier, bleeding agent and antifreezing agent; Quality-the volumetric concentration of described each solute is as follows: Difenoconazole: 100~150 g/L, Tebuconazole: 100~150 g/L, propiconazole: 10~50 g/L, emulsifier: 5~20g/L, bleeding agent: 1~5g/L, antifreezing agent: 0.5~1g/L.
Preferred scheme is that the quality-volumetric concentration of described each solute is as follows: Difenoconazole: 140~150 g/L, Tebuconazole: 140~150 g/L, propiconazole: 30~50 g/L, emulsifier: 5~20g/L, bleeding agent: 1~5g/L, antifreezing agent: 0.5~1g/L.
Described bleeding agent is poly-trisiloxanes, digests work technology Co., Ltd by Guangzhou West and produces, and its model is the poly-trisiloxanes of 810c.
Described antifreezing agent is ethylene glycol.
Described environment-friendly type solvent naphtha is JEFFSOL AG1730 macromolecule organic amine, by system river, Shanghai Chemical Manufacture.
Described emulsifier is the polyoxy ethyl ether, is to be produced by the agricultural chemical industry of Heze City, Shandong Province Co., Ltd.
A kind of preparation method who prepares the above-mentioned ternary built missible oil of claim, its preparation process is as follows:
(1) add the environment-friendly type solvent naphtha that measures in the preparation still, start agitator;
(2) more than temperature raising to 60 ℃, beginning adds Difenoconazole, Tebuconazole and the propiconazole that measures successively;
(3) stir after 0.5 hour, add successively emulsifier, bleeding agent, antifreezing agent starts clipper and carries out emulsification pretreatment and stop after two hours stirring;
(4) standing filtration more than 2 hours, namely get ternary built missible oil.
This preparation method's technique is simple, easy to implement.
Described ternary built missible oil is remarkable at the effect of preventing and treating fruit white rot of grape, particularly 350g/L(Difenoconazole 150g/L, propiconazole 50g/L, Tebuconazole 150g/L) ternary built missible oil is remarkable for the fruit white rot of grape control efficiency.
Embodiment 1:
Ternary built missible oil of the present invention, solvent in its ternary built missible oil is JEFFSOL AG1730 macromolecule organic amine, and the quality-volumetric concentration of each solute is as follows: the poly-trisiloxanes of 150g/L Difenoconazole, 50g/L propiconazole, 150g/L Tebuconazole, 10g/L APEO, 5g/L, 0.5g/L ethylene glycol.The preparation method of this ternary built missible oil is:
(1) add the environment-friendly type solvent naphtha that measures in the preparation still, start agitator;
(2) temperature raising to 60 ℃ beginning adds Difenoconazole, Tebuconazole and the propiconazole that measures successively;
(3) stir after 0.5 hour, add successively emulsifier, bleeding agent, antifreezing agent starts clipper and carries out emulsification pretreatment and stop after two hours stirring;
(4) filtered in standing 2 hours, namely get ternary built missible oil.
This 350g/L(Difenoconazole 150g/L, propiconazole 50g/L, Tebuconazole 150g/L after testing) ternary built missible oil; Its pH value: 7.5, moisture 0.3%, outward appearance: orange transparent, dispersiveness: meet missible oil standard, hot cold storage qualified stability, ageing stability is qualified.
Embodiment 2:
Ternary built missible oil of the present invention, solvent in its ternary built missible oil is JEFFSOL AG1730 macromolecule organic amine, and the quality-volumetric concentration of each solute is as follows: the poly-trisiloxanes of 100g/L Difenoconazole, 50g/L propiconazole, 100g/L Tebuconazole, 5g/L APEO, 2g/L, 0.5g/L ethylene glycol.The preparation method of this ternary built missible oil is identical with step in embodiment 1.
This 250g/L(Difenoconazole 100g/L, propiconazole 50g/L, Tebuconazole 100g/L after testing) ternary built missible oil, its pH value: 8.5, moisture: 0.4%, outward appearance: orange transparent, dispersed: meet missible oil standard, hot cold storage qualified stability, ageing stability qualified.
Embodiment 3:
Ternary built missible oil of the present invention, solvent in its ternary built missible oil is JEFFSOL AG1730 macromolecule organic amine, and the quality-volumetric concentration of each solute is as follows: the poly-trisiloxanes of 140g/L Difenoconazole, 50g/L propiconazole, 140g/L Tebuconazole, 20g/L APEO, 1g/L, 1g/L ethylene glycol.The preparation method of this ternary built missible oil is identical with step in embodiment 1.
This 330g/L(Difenoconazole 140g/L, propiconazole 50g/L, Tebuconazole 140g/L after testing) ternary built missible oil, its pH value: 8.2, moisture: 0.5%, outward appearance: orange transparent, dispersed: meet missible oil standard, hot cold storage qualified stability, ageing stability qualified.
Embodiment 4:
Ternary built missible oil of the present invention, solvent in its ternary built missible oil is JEFFSOL AG1730 macromolecule organic amine, and the quality-volumetric concentration of each solute is as follows: the poly-trisiloxanes of 120g/L Difenoconazole, 50g/L propiconazole, 120g/L Tebuconazole, 20g/L APEO, 1g/L, 1g/L ethylene glycol.The preparation method of this ternary built missible oil is identical with step in embodiment 1.
This 290g/L(Difenoconazole 120g/L, propiconazole 50g/L, Tebuconazole 120g/L after testing) ternary built missible oil, its pH value: 8.3, moisture: 0.5%, outward appearance: orange transparent, dispersed: meet missible oil standard, hot cold storage qualified stability, ageing stability qualified.
Embodiment 5:
Ternary built missible oil of the present invention, solvent in its ternary built missible oil is JEFFSOL AG1730 macromolecule organic amine, and the quality-volumetric concentration of each solute is as follows: the poly-trisiloxanes of 100g/L Difenoconazole, 40g/L propiconazole, 140g/L Tebuconazole, 20g/L APEO, 1g/L, 1g/L ethylene glycol.The preparation method of this ternary built missible oil is identical with step in embodiment 1.
This 280g/L(Difenoconazole 100g/L, propiconazole 40g/L, Tebuconazole 140g/L after testing) ternary built missible oil, its pH value: 7.8, moisture: 0.5%, outward appearance: orange transparent, dispersed: meet missible oil standard, hot cold storage qualified stability, ageing stability qualified.
Embodiment 6:
Ternary built missible oil of the present invention, solvent in its ternary built missible oil is JEFFSOL AG1730 macromolecule organic amine, and the quality-volumetric concentration of each solute is as follows: the poly-trisiloxanes of 140g/L Difenoconazole, 30g/L propiconazole, 140g/L Tebuconazole, 20g/L APEO, 1g/L, 1g/L ethylene glycol.The preparation method of this ternary built missible oil is identical with step in embodiment 1.
This 310g/L(Difenoconazole 140g/L, propiconazole 30g/L, Tebuconazole 140g/L after testing) ternary built missible oil, its pH value: 8.3, moisture: 0.5%, outward appearance: orange transparent, dispersed: meet missible oil standard, hot cold storage qualified stability, ageing stability qualified.
This ternary built missible oil can be used for preventing and treating powdery mildew, root rot, the rust of wheat, disease, particularly 350g/L(Difenoconazole 150g/L, propiconazole 50g/L, the Tebuconazole 150g/L such as the spot defoliation of the anthracnose on vegetables, powdery mildew and fruit tree, scab, rust, anthracnose, white rot) ternary built missible oil is remarkable for the fruit white rot of grape control efficiency.
Below that ternary built missible oil of the present invention is used for preventing and treating the field control effectiveness test of fruit white rot of grape.
1, test medicine: get 350g/L ternary built missible oil, 250g/L ternary built missible oil, 330g/L ternary built missible oil that embodiment 1,2,3 makes;
2, contrast medicament: 250g/L Difenoconazole missible oil
The 250g/L propiconazole emulsifiable concentrate
3, for studying thing: grape;
4, controlling object: white rot;
5, experimental scheme:
(1) 350g/L Difenoconazole propiconazole Tebuconazole missible oil;
(2) 250g/L Difenoconazole propiconazole Tebuconazole missible oil;
(3) 330g/L Difenoconazole propiconazole Tebuconazole missible oil;
(4) 250g/L Difenoconazole missible oil;
(5) 250g/L propiconazole emulsifiable concentrate;
(6) contrast sprays clear water.
6, application method
Adopt the spraying of BP-16 type knapsack manual sprayer, every mu is watered 50Kg;
Control efficiency adopts following disease index to calculate, and the test data Analysis of variance is with the significance of difference of LSR method check control efficiency.
Disease index=(∑ (the sick numbers of sheets at different levels * relative level numerical value)/investigate total number of sheets * 9) * 100
Control efficiency=((check plot disease index-treatment region disease index)/check plot disease index) * 100
7, result of the test
Result of the test is seen following two forms.
Table 1 (Difenoconazole+propiconazole+Tebuconazole) ternary built EC fruit white rot of grape test effect
Table 2 (Difenoconazole+propiconazole+Tebuconazole) ternary built EC fruit white rot of grape test effect
Result shows: Difenoconazole, propiconazole, three kinds of composite ternary built missible oil of Tebuconazole all have control efficiency preferably to fruit white rot of grape, and its preventive effect is apparently higher than the preventive effect of two kinds of contrast medicaments.Wherein, 350g/L Difenoconazole propiconazole Tebuconazole EC best results, preventive effect is 91.92%.250g/L Difenoconazole propiconazole Tebuconazole missible oil preventive effect is lower slightly, but high than two kinds of contrast pharmacy control efficacies.
Preventive effect is carried out variance analysis:
350g/L Difenoconazole propiconazole Tebuconazole missible oil and 330g/L Difenoconazole propiconazole Tebuconazole missible oil difference are not remarkable, with 250g/L Difenoconazole propiconazole Tebuconazole missible oil significant difference.
250g/L Difenoconazole propiconazole Tebuconazole missible oil and contrast medicament (250g/L Difenoconazole missible oil) significant difference.
Two kinds of contrast medicament differences of 250g/L Difenoconazole missible oil and 250g/L propiconazole emulsifiable concentrate are not remarkable.
Show by above embodiment, the composite missible oil of Difenoconazole of the present invention, propiconazole, Tebuconazole is in technical indicator or field efficacy all has good effect, be better than in the market propiconazole and missible oil and the composition single dose thereof of Difenoconazole.The advantages such as the present invention's bactericidal potency in production application is high, expansion fungicidal spectrum, saving pesticide cost, environmentally safe.Fruit white rot of grape etc. is had good control efficiency, and safety is good, without poisoning.
Claims (8)
1. ternary built missible oil, it is characterized in that: the solvent in described ternary built missible oil is the environment-friendly type solvent naphtha, solute is Difenoconazole, Tebuconazole, propiconazole, emulsifier, bleeding agent and antifreezing agent; Quality-the volumetric concentration of described each solute is as follows: Difenoconazole: 100~150 g/L, Tebuconazole: 100~150 g/L, propiconazole: 10~50 g/L, emulsifier: 5~20g/L, bleeding agent: 1~5g/L, antifreezing agent: 0.5~1g/L.
2. ternary built missible oil according to claim 1, it is characterized in that: the quality-volumetric concentration of described each solute is as follows: Difenoconazole: 140~150 g/L, Tebuconazole: 140~150 g/L, propiconazole: 30~50 g/L, emulsifier: 5~20g/L, bleeding agent: 1~5g/L, antifreezing agent: 0.5~1g/L.
3. ternary built missible oil according to claim 1 and 2 is characterized in that: described bleeding agent is poly-trisiloxanes.
4. ternary built missible oil according to claim 1 and 2, it is characterized in that: described antifreezing agent is ethylene glycol.
5. ternary built missible oil according to claim 1 and 2, it is characterized in that: described environment-friendly type solvent naphtha is macromolecule organic amine.
6. ternary built missible oil according to claim 1 and 2, it is characterized in that: described emulsifier is APEO.
7. method for preparing the described ternary built missible oil of claim 1 or 2, it is characterized in that: the preparation process of the method is as follows:
(1) add the environment-friendly type solvent naphtha that measures in the preparation still, start agitator;
(2) more than temperature raising to 60 ℃, add successively the Difenoconazole, Tebuconazole and the propiconazole that measure;
(3) stir after 0.5 hour, add successively emulsifier, bleeding agent, antifreezing agent starts clipper and carries out emulsification pretreatment and stop after two hours stirring;
(4) standing filtration more than 2 hours, namely get ternary built missible oil.
8. the application of ternary built missible oil claimed in claim 1 in preventing and treating fruit white rot of grape.
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Application publication date: 20130206 |

