CN102948422A - Sterilization composition containing pyraoxystrobin and pyrimethanil - Google Patents

Sterilization composition containing pyraoxystrobin and pyrimethanil Download PDF

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Publication number
CN102948422A
CN102948422A CN2012104376965A CN201210437696A CN102948422A CN 102948422 A CN102948422 A CN 102948422A CN 2012104376965 A CN2012104376965 A CN 2012104376965A CN 201210437696 A CN201210437696 A CN 201210437696A CN 102948422 A CN102948422 A CN 102948422A
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azoles bacterium
bacterium ester
phonetic mould
mould amine
pyrimethanil
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葛大鹏
陈鹏
韩先正
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Hailir Pesticides and Chemicals Group Co Ltd
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Hailir Pesticides and Chemicals Group Co Ltd
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Abstract

The present invention relates to a sterilization composition containing pyraoxystrobin and pyrimethanil, wherein an active ingredient is obtained by compounding pyraoxystrobin and pyrimethanil, a mass ratio of the pyraoxystrobin to the pyrimethanil is 1-80:80-1, the total mass of the pyraoxystrobin and the pyrimethanil is 1-80% of the total mass of the whole preparation, and the balance is a pesticide acceptable auxiliary component. The sterilization composition can be made into pesticide formulations such as emulsifiable concentrate, a suspension, wettable powder, water dispersible granule, water emulsion and micro-emulsion, is mainly provided for preventions and controls of botrytis cinerea, fusarium wilt, downy mildew of crops such as cucumber, tomato, grape, strawberry, pea, leek and the like, and scab of cucurbits and alternaria mali roberts of fruit trees, and provides excellent prevention and control effects for tomato late blight, cucumber anthracnose, and powdery mildew leaves.

Description

A kind of bactericidal composition that contains azoles bacterium ester and phonetic mould amine
Technical field
The present invention relates to the agriculture chemical compounding technical field, be specifically related to a kind of bactericidal composition that contains azoles bacterium ester and phonetic mould amine.
Background technology
Azoles bacterium ester is the strobilurin fungicide that Shenyang Chemical Engineering Inst develops.Azoles bacterium ester fungicidal spectrum is wide, bactericidal activity is high, and relatively more outstanding stripped bactericidal activity is arranged, and cucumber downy mildew, downy mildew of garpe, tomato late blight, cucumber anthracnose, powdery mildew of cucumber are had excellent control efficiency.Azoles bacterium esterification formal name used at school is called (E)-2-(2-((3-(4-chlorphenyl)-1-methyl isophthalic acid H-pyrazoles-5-oxygen base) methyl) phenyl)-3-methoxy-methyl acrylate.
Phonetic mould amine claims again methylpyrimidine amine, diformazan pyrilamine to belong to the pyrimidine fungicides bactericide, and gray mold is had special efficacy.Its bactericidal action mechanism is unique, thereby stops infection process by the secretion that suppresses the infection process enzyme, and kill pathogens.Have protection and therapeutic action, have simultaneously interior suction and fumigation action, be mainly used in preventing and treating cucumber, tomato, grape, strawberry, pea, leek, etc. crop gray mold, fusarium wilt and black spot of fruit tree, spot defoliation etc.The chemical name of phonetic mould amine is N-(4,6-dimethyl pyrimidine-2-yl) aniline, its chemical structural formula is
Figure 572872DEST_PATH_IMAGE001
Using chemical agent is the most effectively means of controlling plant diseases.But long-term use single chemical bactericide continuously high dose, cause easily the problems such as residual, the environmental pollution of medicament and anti-pesticide resistance fungi development.Reasonably chemical bactericide is composite or be mixed and have the expansion fungicidal spectrum, improve control efficiency, prolong the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay Antifungal resistance and the positive characteristics such as drug-fast generation and development, bactericide compounded is the most one of the effective method that addresses the above problem.Exploitation new product bactericide price is constantly soaring, and by contrast, exploitation is efficient with research, low toxicity, low-residual composite be mixed have small investment, the lead time is short and be subject to domestic and international attention, the numerous and confused dynamics that develops that strengthens.We filter out azoles bacterium ester and phonetic mould amine and carry out compositely on the basis of lab screening and field trial, have obvious synergistic effect.And about the composite bactericidal composition of azoles bacterium ester and phonetic mould amine and use and there is no at present the people and reported.
Summary of the invention
Based on above situation, the object of the invention is to provide a kind of new and effective pesticide sterilizing composite.Be mainly used in preventing and treating cucumber, tomato, grape, strawberry, pea, leek, etc. crop gray mold, fusarium wilt, downy mildew and black spot of fruit tree, spot defoliation, tomato late blight, cucumber anthracnose, powdery mildew leaf are had excellent control efficiency.
Technical scheme of the present invention realizes by following measures:
A kind of bactericidal composition that contains azoles bacterium ester and phonetic mould amine, active ingredient azoles bacterium ester and two yuan of the phonetic mould amine of this bactericidal composition are composite, and all the other are auxiliary element.The mass ratio of active ingredient azoles bacterium ester and phonetic mould amine is 1~80: 80~1 in the wherein said Pesticidal combination, and described bactericidal composition of the present invention is through the toxicity test experimental verification, and the mass ratio of azoles bacterium ester and phonetic mould amine is 1~40: 40~1 o'clock, and synergistic effect is better.
The formulations of pesticide that described bactericidal composition of the present invention can be prepared are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion.Wherein active ingredient azoles bacterium ester and the gross mass of phonetic mould amine in preparation account for 1%~80% of the whole quality of the pharmaceutical preparations, when wherein accounting for 5%-50%, and toxicity and the residual preferably balance that reaches, cost is also lower.
The specific embodiments of the formulations of pesticide that bactericidal composition of the present invention is mixed with is as follows:
Described bactericidal composition is cream preparation, and the mass fraction of component is: azoles bacterium ester 1~80; 1~80 part of phonetic mould amine; 10~30 parts of conventional emulsifiers; 20~50 parts of conventional solvents; 1~5 part of conventional synergist.
The concrete production stage of this cream preparation adds emulsifier, the synergist rear oily liquids that becomes transparent and homogeneous that stirs after dissolving fully in the solvent again for first active ingredient azoles bacterium ester and phonetic mould amine being added, can namely can be made into the cream preparation of the present composition.
Described bactericidal composition is suspending agent, and the mass fraction of component is: 1~80 part of azoles bacterium ester; 1~80 part of phonetic mould amine; 5~20 parts of dispersants; 1~5 part of antifreezing agent; 0.1~2 part of thickener; 0.1~0.8 part of defoamer; 0~10 part of penetrating agent; 0.1~5 part of pH value conditioning agent; Water, surplus.
The concrete production stage of this suspending agent is for mixing other auxiliary agents first, mix through high speed shear, add active ingredient azoles bacterium ester and phonetic mould amine, abrading-ball is 2~3 hours in ball crusher, make a diameter all below 5mm, namely can be made into the suspending agent preparation of the present composition.
Described bactericidal composition is wetting powder, and the mass fraction of component is: 1~80 part of azoles bacterium ester; 1~80 part of phonetic mould amine; 3~10 parts of dispersants; 1~5 part of wetting agent; Filler, surplus.
The concrete production stage of this wetting powder is: by above-mentioned prescription active ingredient azoles bacterium ester is mixed with phonetic mould amine and dispersant, wetting agent and filler, uniform stirring in stirred tank, behind airslide disintegrating mill, mixing, namely can be made into the wetting powder of the present composition.
Described bactericidal composition is water dispersible granules, and the mass fraction of component is: 1~80 part of azoles bacterium ester; 1~80 part of phonetic mould amine; 3~10 parts of dispersants; 1~10 part of wetting agent; 1~5 part of disintegrant; The filler surplus.
The concrete production stage of this water dispersible granules is: by above-mentioned prescription active ingredient azoles bacterium ester and phonetic mould amine and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, then add and carry out granulation, drying, screening in the fluidized bed prilling dryer by sample analysis, namely can be made into the water dispersible granules of the present composition.
Described bactericidal composition is aqueous emulsion, and the mass fraction of component is: 1~80 part of azoles bacterium ester; 1~80 part of phonetic mould amine; 3~30 parts of emulsifier; 5~15 parts of solvents; 2~15 parts of stabilizing agents; 1~5 part of antifreezing agent; 0.1~8 part of defoamer; 0.2~2 part of thickener; Water surplus.
The concrete production stage of this aqueous emulsion is: at first azoles bacterium ester and phonetic mould amine, solvent and emulsifier, cosolvent are added together, make and be dissolved into uniform oil phase; With part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added water, slowly add water until reach the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear approximately half an hour, form the aqueous emulsion of oil-in-water type, namely can be made into the aqueous emulsion of the present composition.
Wherein above-described emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, the alkylphenol polyoxyethylene sulfosuccinate, styrylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, any or more than one any mixtures than forming in the polyoxyethylene aliphatic alcohol ether.
Described solvent is dimethylbenzene or biodiesel, toluene, and diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine oil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in the water equal solvent are arbitrarily than the mixture that forms.
Described dispersant is selected from polycarboxylate, lignosulfonates, alkylphenol polyoxyethylene methyl ether condensate sulfate, the alkylsulfonate calcium salt, the naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, one or more in the fatty acid glyceride APEO.
Described wetting agent is selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, and Nekal BX, moistening bleeding agent F, alkylbenzenesulfonate polyoxyethylene triphen is phosphenylic acid salt dimly, spaonin powder, silkworm excrement, one or more in the soapberry powder.
Described disintegrant is selected from bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, one or more in the sodium bicarbonate.
Described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, in the polyvinyl alcohol one or more.
Described stabilizing agent is selected from sodium citrate, a kind of in the resorcinol.
Described antifreezing agent is selected from ethylene glycol, propane diols, one or more in the glycerine.
Described defoamer is selected from silicone oil, silicone compound, C 10-20The saturated fat acid compounds, C 8-10One or more of fatty alcohol.
Described filler is selected from kaolin, diatomite, bentonite, attapulgite, white carbon, starch, one or more in the precipitated calcium carbonate.
The composite bactericide of the present invention take azoles bacterium ester and phonetic mould amine as active ingredient has obvious synergistic effect, delays the drug-fast generation in key, and reduced to become to produce cost and use cost, can be used for the improvement of resistance disease.Be mainly used in preventing and treating cucumber, tomato, grape, strawberry, pea, leek, etc. crop gray mold, fusarium wilt, downy mildew and black spot of fruit tree, spot defoliation, tomato late blight, cucumber anthracnose, powdery mildew leaf are had excellent control efficiency.
Embodiment
For making technical scheme of the present invention, purpose and advantage are clearer, and the present invention describes with following specific embodiment, but the present invention is not limited to these examples.The mode that effect experiment of the present invention adopts indoor biometrics and field trial to combine, if no special instructions, the ratio of below mentioning all is ratio of quality and the number of copies.
Embodiment: the different proportioning co-toxicity experiments from phonetic mould amine of azoles bacterium ester.
1.1 reagent agent
The former medicine of 95.5% azoles bacterium ester, the former medicine of 98% phonetic mould amine, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
Never executing azoles bacterium ester and phonetic mould amine and cucumber of the same type from the Shandong Pingdu gathers potted plantly and separates.Cucumber variety: middle peasant No. 13.
1.3 test method
1.3.1 medicament preparation
Use first the former medicine of acetone solution, according to the result of preliminary experiment two an amount of former medicines are made into 5 different proportionings, with acetone each is processed again that to be diluted to respectively 5 concentration gradients stand-by, and with clear water in contrast.
1.3.2 chemicals treatment
With the former medicine of 95.5% azoles bacterium ester, the former medicinal acetone of 98% phonetic mould amine is solvent dilution, is made into the 10000ug/ml mother liquor, saves backup under 4 ℃ of conditions.
To infect No. 13 residences of cucumber variety middle peasant and fit in the seedling-growing container, and place the greenhouse to cultivate, plant grows to three to four leaf after dates, gathers the blade of identical leaf age, is used for mensuration and the cultivation of cucumber downy mildew.
Cucumber downy mildew adopts the plants method at 20 ℃, cultivates under the condition of 12h alternation of light and darkness, turns culture once in per 30 days.With the conidium on the sterile water wash-out incidence of leaf, being configured to concentration is 1 * 10 during inoculation 6The spore suspension of individual/ml.
1.3.3 for examination strain sensitivity testing
Adopt leaf dish moisturizing method to carry out toxicity test.First the blade that gathers is prepared into the leaf dish that diameter is 1.5cm, test is with the blank that is treated to of adding medicine not, after soaking end, leaf faces up and puts on the wetting blotting paper of same concentrations liquid, and the liquid on the leaf dish is blotted, and the spore suspension 10L that configures is inoculated in leaf dish central authorities, after room temperature is placed 5min, place under 20 ℃, the condition of 12h alternation of light and darkness and cultivate, measure the onset area on the leaf dish behind the 10d, calculate EC 50.
The percentage that accounts for the leaf disc area according to lesion area is divided sick level
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area;
1.3.4 mixture toxicity test and interpretation of result
Carry out the toxicity test of mixture according to mixed ratio with single dose toxicity test method.According to the toxicity test result of single dose, be 24% ratio of quality and the number of copies azoles bacterium ester by active ingredient: phonetic mould amine is 4: 36,6: 34, and 8: 32,10:30,12:28.
Adopt said method to carry out toxicity test, if contrast lethality<5% is not proofreaied and correct, the contrast lethality by formula 2 is proofreaied and correct between 5%-20%, the contrast lethality〉20%, test need be reformed.
Take the logarithm value of drug concentration (mg/L) as independent variable x, take the probability value of corrected mortality as dependent variable y, set up respectively the virulence regression equation formula, adopt DPS software to calculate the LC of single dose and each proportioning mixture 50Calculate co-toxicity coefficient (CTC) according to the abundant method of Sun Yun.Co-toxicity coefficient CTC, computing formula is as follows: (take azoles bacterium ester as the standard medicament, its toxicity index is 100):
The LC of the toxicity index of phonetic mould amine (TI)=azoles bacterium ester 50The LC of phonetic mould amine 50* 100
The LC of the true toxicity index (ATI) of M=azoles bacterium ester 50The LC of/M 50* 100
The phonetic mould amine of TI * P of the TI of the theoretical toxicity index (TTI) of M=azoles bacterium ester * P azoles bacterium ester+phonetic mould amine
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100
In the formula:
M is the mixture of azoles bacterium ester and the different proportionings of phonetic mould amine
P azoles bacterium ester is azoles bacterium ester shared ratio in mixture
The phonetic mould amine of P is phonetic mould amine shared ratio in mixture
2.1 toxicity test result
Table 1 azoles bacterium ester and phonetic mould amine are to the toxicity test of cucumber downy mildew
Figure 427696DEST_PATH_IMAGE002
As can be seen from the table, in different proportionings, be 4: 36 in the active ingredient ratio, 6: 34,8: 32, when 10:30,12:28 dilute respectively, all show stronger synergistic effect, its co-toxicity coefficient is all greater than 120, show certain synergistic effect, wherein the mass ratio of azoles bacterium ester and phonetic mould amine is that 8: 32 synergistic effect is the most obvious, and co-toxicity coefficient is 167.74.Suggestion is carried out further field control effectiveness test to 8: 32 left and right sides mixture preparations of suitable proportion, to estimate its field practical application effect.
3, field trial control cucumber downy mildew, the experimental result of gray mold
3.1 field trial control cucumber downy mildew
3.1.1 test method
Test is on Shandong Pingdu City cucumber ground, and 4 points of every residential quarter investigation are investigated 2 strains at every, put down in writing occurring degree with staging, and grade scale is as follows:
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area;
3.1.2 control time and number of times
Test is investigated 4 times altogether, investigates in 15 days behind 3 days, 7 days and the medicine behind radix investigation, the medicine before the medicine.
3.1.3 drug effect computational methods
Sick leaf rate (the %)=sick number of sheets/investigate total number of sheets * 100
Disease index=∑ (the sick numbers of sheets at different levels * relative level numerical value)/(investigating total number of sheets * 9) * 100
Control efficiency (%)=(disease index behind disease index before the 1-(blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100
3.1.4 poisoning investigation method
Whether continuous 7d range estimation medicament has poisoning to crop after the dispenser.
3.1.5 result of the test and analysis
Each processes the effect (table 2) of control cucumber downy mildew
Each processes the effect of control cucumber downy mildew table 2
Figure 400243DEST_PATH_IMAGE003
The Mixed Pharmacy of different proportion is tested by different consumptions as can be seen from Table 2, and its control to cucumber downy mildew all is better than contrasting medicament behind the medicine, and 15 days bactericidal effect is respectively 90.35,91.41 behind medicine, and 92.62.Bactericidal effect increases progressively with the increase of dosage.According to the field range estimation, in the test dose scope, 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.Advise that the bactericide different from the mechanism of action mixes use to delay the drug-fast generation of germ.
4.1 field trial control gray mold of cucumber
4.1.1 test method
Test is on Shandong Pingdu City cucumber ground, and 4 points of every residential quarter investigation are investigated 2 strains at every, put down in writing occurring degree with staging, and grade scale is as follows:
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area.
4.1.2 control time and number of times
Test is investigated 4 times altogether, radix investigation before the medicine, for the first time behind the medicine 7 days, investigated in 14 days and 21 days behind the medicine for the second time.
4.1.3 drug effect computational methods
Sick leaf rate (the %)=sick number of sheets/investigate total number of sheets * 100
Disease index=∑ (the sick numbers of sheets at different levels * relative level numerical value)/(investigating total number of sheets * 9) * 100
Control efficiency (%)=(disease index behind disease index before the 1-(blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100
4.1.4 poisoning investigation method
Continuous Observation after the dispenser, whether the range estimation medicament has poisoning to crop.
4.1.5 result of the test and analysis
Each processes the effect (table 3) of control gray mold of cucumber
Each processes the effect of control gray mold of cucumber table 3
Figure 733135DEST_PATH_IMAGE004
As can be seen from Table 3, the phonetic mould amine of 40% azoles bacterium ester is very remarkable with the effect of 8:32 proportioning control gray mold of cucumber.The effect of complex preparation is significantly higher than single dose, its instant effect, and the lasting period is also better, is the desirable medicament of preventing and treating gray mold, and to cucumber safety, can effectively delays the drug-fast generation of germ.
In sum, the present invention contains the bactericidal composition of azoles bacterium ester and phonetic mould amine, powdery mildew of cucumber and gray mold are had good control efficiency, and it is to the target crop safety.Complex preparation has not only improved preventive effect, and has enlarged fungicidal spectrum, so this compounded combination tool in production practices is of great significance.

Claims (5)

1. bactericidal composition that contains azoles bacterium ester and phonetic mould amine, it is characterized in that: the active ingredient of this bactericidal composition is that azoles bacterium ester and two yuan of phonetic mould amine are composite, and wherein the mass ratio of active ingredient azoles bacterium ester and phonetic mould amine is 1~80: 80~1.
2. bactericidal composition according to claim 1, it is characterized in that: the quality optimization ratio of azoles bacterium ester and phonetic mould amine is 1~40: 40~1.
3. bactericidal composition according to claim 1, it is characterized in that: azoles bacterium ester and phonetic mould amine account for 1%~80% of the whole quality of the pharmaceutical preparations.
4. bactericidal composition according to claim 3, it is characterized in that: azoles bacterium ester and phonetic mould amine account for 5%~50% of the whole quality of the pharmaceutical preparations.
5. according to claim 1 and 2 or 3 or 4 described bactericidal compositions, it is characterized in that: the formulations of pesticide that this bactericidal composition can be prepared into are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion.
CN2012104376965A 2012-11-06 2012-11-06 Sterilization composition containing pyraoxystrobin and pyrimethanil Pending CN102948422A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112794777A (en) * 2021-01-26 2021-05-14 广西壮族自治区农业科学院 Novel fertilizer special for eucalyptus and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102106355A (en) * 2009-12-23 2011-06-29 中国中化股份有限公司 Antifungal composition containing pyraoxystrobin
WO2012031061A2 (en) * 2010-09-01 2012-03-08 E. I. Du Pont De Nemours And Company Fungicidal pyrazoles and their mixtures
CN102696647A (en) * 2012-06-29 2012-10-03 青岛星牌作物科学有限公司 Sterilizing composite containing pyraclostrobin and pyrimethanil and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102106355A (en) * 2009-12-23 2011-06-29 中国中化股份有限公司 Antifungal composition containing pyraoxystrobin
WO2012031061A2 (en) * 2010-09-01 2012-03-08 E. I. Du Pont De Nemours And Company Fungicidal pyrazoles and their mixtures
CN102696647A (en) * 2012-06-29 2012-10-03 青岛星牌作物科学有限公司 Sterilizing composite containing pyraclostrobin and pyrimethanil and application

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112794777A (en) * 2021-01-26 2021-05-14 广西壮族自治区农业科学院 Novel fertilizer special for eucalyptus and preparation method thereof

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Application publication date: 20130306