CN113875764A - Emamectin benzoate soluble solution, preparation method and application thereof - Google Patents
Emamectin benzoate soluble solution, preparation method and application thereof Download PDFInfo
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- CN113875764A CN113875764A CN202111281694.7A CN202111281694A CN113875764A CN 113875764 A CN113875764 A CN 113875764A CN 202111281694 A CN202111281694 A CN 202111281694A CN 113875764 A CN113875764 A CN 113875764A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
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Abstract
The invention discloses an emamectin benzoate soluble solution, a preparation method and application thereof, wherein the soluble solution comprises the following components in percentage by weight: 21-30% of emamectin benzoate, 10-12% of emulsifier, 2-5% of fat dissolving agent, 20-30% of cosolvent and 25-42.25% of solvent. The soluble liquid has high content, low consumption, low cost, simple use, no limitation of tree height and harmful parts, and environmental friendliness.
Description
Technical Field
The invention relates to the technical field of production and application of pesticides, in particular to an emamectin benzoate soluble solution, a preparation method and application thereof.
Background
Bursaphelenchus xylophilus is a devastating disease of pine trees, known as cancer of pine trees. Once the pine tree is infected with the disease, the pine tree can die in about 40 days at the fastest, and if manual intervention is not carried out, the pine tree can be destroyed into pine forest in 3-5 years.
In order to control the spread of the disease, China invests a large amount of financial resources, firstly, the longhorn beetles serving as the spread media are prevented and killed, secondly, the pine trees died of the disease are eliminated, and the application range of the pine trees is strictly controlled. Many domestic institutions also develop researches for preventing and treating the disease, and the main research direction is to screen and prepare high-efficiency medicament varieties and dosage forms for punching and injecting medicaments. However, the existing injection medicine has a fatal weakness, and must be used at the temperature below 10 ℃ in winter, because the dosage of the current common low-content emamectin benzoate preparations such as 1-5.7% emamectin benzoate microemulsion and other products is large, generally about 30-50 ml, the dosage must be that after the medicine bottle is inserted after drilling and is injected with water, the medicine bottle is manually pulled out at least about 7 days, and the medicine injection hole is plugged by a wooden plug, vaseline or a healing agent.
Aiming at the defects of the existing injection agent in practical application, the inventor carries out improvement research, utilizes a high-content emamectin benzoate preparation and fully utilizes the characteristics of high activity and systemic property of emamectin benzoate to develop a 22.75% emamectin benzoate soluble solution, can effectively prevent and treat the pine wilt disease, simultaneously, the injection agent only needs 5-8 ml, a wooden plug is used for plugging a medicine injection hole after the medicine injection is finished, the prevention and treatment can be completed at one time, and the complicated steps that the medicine bottle is manually pulled out after the medicine injection is injected for at least 7 days at the temperature below 10 ℃ in winter according to the existing injection technology, and the medicine injection hole is plugged by the wooden plug, vaseline or a consolidant are avoided.
The patent with publication number CN109197882A discloses an emamectin benzoate B2a/B2B emulsion, which comprises an active component of emamectin benzoate B2a/B2B benzoate, a solvent, a cosolvent, an emulsifier, an anti-photolysis agent and the like. The methylamino abamectin B2a/B2B benzoate emulsion prepared by the patent has the advantages of large content range, high stability, low decomposition rate, light irradiation resistance and the like, but the dosage form of the patent is microemulsion or missible oil, and the absorption and utilization of active ingredients are influenced because a fat dissolving agent aiming at pine oil is lacked in the formula.
Patent publication No. CN101199280A discloses a soluble liquid agent prepared by mixing emamectin benzoate and nereistoxin. The soluble liquid agent comprises the following raw materials in percentage by weight: 0.1-10 wt% of emamectin benzoate, 10-50 wt% of nereistoxin, 1-30 wt% of emulsifier, 5-30 wt% of cosolvent, 0.2-20 wt% of stabilizer, 0.1-10 wt% of synergist, 5-70 wt% of solvent, 0.1-10 wt% of penetrating agent and 0.01-5 wt% of pH value regulator. The synergistic effect of emamectin benzoate and nereistoxin is utilized to improve the drug effect, enlarge the application range and delay the resistance. The mixed pesticide is particularly suitable for preventing and treating various pests with serious resistance on rice, vegetables and fruit trees, but the patent relates to a compound pesticide form, has low emamectin benzoate content and is different from the application field of the application.
Patent publication No. CN101449680A discloses a methylamino abamectin benzoate microemulsion, which consists of raw pesticide, solvent, cosolvent, emulsifier and water, and the weight percentages of the components are as follows: 0.5-5% of emamectin benzoate, 5-20% of solvent, 1-10% of cosolvent, 5-30% of emulsifier, 0.1-3% of synergist, 0.1-3% of stabilizer and the balance of water to 100%. Dissolving the raw materials with solvent and cosolvent, adding emulsifier, mixing, and adding water under stirring to obtain homogeneous transparent product. The product replaces part of organic solvent with water, is environment-friendly and safe for users, and improves the drug effect, but the product of the patent has low content, is a water-containing preparation and is far different from the injection drying agent of the application.
The patent with the publication number of CN101933509A discloses an agricultural insecticide emamectin benzoate microemulsion and a preparation method thereof, wherein the emamectin benzoate microemulsion comprises, by weight, 0.5-10% of emamectin benzoate, 5-20% of a solvent, 1-15% of a cosolvent, 5-40% of an emulsifier, 0.1-3% of a stabilizer and water which is supplemented to 100%; the preparation method comprises the steps of firstly stirring and mixing the solvent, the cosolvent and the emamectin benzoate uniformly at a rotating speed of 40-100 revolutions per minute in proportion, then adding the emulsifier and the stabilizer in proportion, stirring uniformly, finally adding water to supplement 100%, and continuously stirring for 1-2 hours to obtain a uniform transparent solution product, wherein the environmental pollution is reduced, water is used for replacing part of the solvent, and the using amount of the aromatic organic solvent is reduced; the pesticide effect is improved, the penetration capacity and the spreading uniformity of the emamectin benzoate to insects and plants are improved, the control effect and the effective utilization rate of the pesticide are improved, but the pesticide is low in product content, is a microemulsion and is far different from the drying injection of the pesticide.
The patent with publication number CN1795720A discloses a group of new soluble liquid pesticide formulations using propoxur as raw material for preventing and controlling crop pests and sanitary pests such as cotton, vegetables and fruit trees. Is prepared from benzene-free assistant, benzene-free solvent, emulsifier and synergist. Has the characteristics of high efficiency, lasting effect, safety for producers and users, environmental protection and the like. The composition content (by weight percentage) of the propoxur-emamectin benzoate soluble solvent comprises 1-20% of propoxur, 0.1-5% of emamectin benzoate, 0-30% of cosolvent, 1-35% of emulsifier, 0-15% of penetrant, 0-5% of synergist and 0.1-1% of antioxidant, but the content of emamectin benzoate related to the product is low, and the propoxur is a typical insecticide and is far different from the dry injection agent.
The patent with publication number CN1788562A discloses a new formulation of emamectin benzoate soluble liquid for controlling crop pests such as vegetables, fruit trees and the like. Prepared by benzene-free cosolvent, solvent, emulsifier and synergist, has the characteristics of high efficiency, lasting effect, safety for producers and users, environmental protection and the like. According to the composition content (in weight percentage) of the emamectin benzoate soluble liquid, the emamectin benzoate is 0.05-20%, the cosolvent is 0-30%, the emulsifier is 1-35%, the penetrant is 0-15%, the synergist is 0-5%, and the antioxidant is 0.1-1%.
Disclosure of Invention
In view of the above, the invention aims to provide a high-content emamectin benzoate soluble solution which is low in dosage, low in cost, simple to use, capable of being used all the year round, free of limitation of tree height, harm parts and the like, and green and environment-friendly.
In order to achieve the above purpose, the invention provides the following technical scheme:
the emamectin benzoate soluble solution comprises the following components in percentage by weight: 21-30% of emamectin benzoate, 10-12% of emulsifier, 2-5% of fat dissolving agent, 20-30% of cosolvent and 25-42.25% of solvent.
When the weight percentage of the emamectin benzoate is in the range, the absorption is over 80 percent.
The preferable weight percentage of the emamectin benzoate is 22.75%.
When the weight percentage of the emamectin benzoate is about 22.75 percent, the absorption reaches the maximum value.
The emulsifier is preferably at least one selected from triphenylethylphenol polyoxyethylene polyoxypropylene ether, triphenylethylphenol polyoxyethylene ether, diphenylethylphenol formaldehyde condensation compound polyoxyethylene ether, castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether sulfate, fatty amine polyoxyethylene ether and alkyl glycoside.
The fat dissolving agent is preferably at least one of isooctanol polyoxyethylene ether, agricultural organic silicon, sulfonated dioctyl sodium succinate, synergistic ether, azone and fatty alcohol-polyoxyethylene ether.
The cosolvent is preferably at least one of cyclohexanone, acetone, dimethyl sulfoxide, ethylene glycol monomethyl ether and xylene.
The compound auxiliary agent with the HLB value of more than 12 is preferred, and has better solubilizing and synergistic effects on a soluble agent.
The solvent is preferably at least one selected from methanol, ethylene glycol, diethylene glycol, dimethylformamide, ethanol, isopropanol, and N-methylpyrrolidone.
The invention also provides a preparation method of the emamectin benzoate soluble solution, which comprises the following steps:
a. weighing cosolvent, pouring two-thirds to three-fourths of the cosolvent into a container, and stirring;
b. and weighing the emulsifier, the emamectin benzoate and the fat dissolving agent in sequence, pouring the mixture into a container, flushing the measuring cup with the residual solvent, pouring the mixture into the container, continuously stirring, observing the material to be clear and transparent, and stopping stirring to obtain the composition.
The invention further provides application of the emamectin benzoate soluble solution in preventing and treating pine wilt disease.
When in use, the emamectin benzoate accounts for 22.75 percent by weight, and the injection amount is 5ml to 8 ml.
The invention has the following main beneficial effects:
1. the emamectin benzoate soluble solution with high content (22.75%) is prepared by adopting proper solvent, cosolvent, emulsifier and fat dissolving agent, has super strong affinity to pine wood and pine oil, can be quickly absorbed when being injected into pine tree bodies, and has simple preparation method.
2. The dose is only required to be 5-8 ml per time, and the active ingredients can reach 1g per time.
3. The method is not limited by the height and the damage parts of the trees, and the pest control of the upper pests, the root pests, the hidden sap sucking pests with wax shell protection, the boring pests, the vascular bundle diseases and other pests which are difficult to effectively control by the conventional pesticide application method of tall trees becomes simple and feasible.
4. The method is not limited by rainfall, and chemical control can be implemented under the conditions of continuous raininess or severe drought and water shortage.
5. Is not limited by temperature, and can be used for chemical prevention and treatment all the year round.
6. The medicine injection and the medicine hole plugging are completed at one time, the medicine bottle is prevented from being pulled up and the medicine hole is prevented from being plugged by a wood plug at the second time, and the labor cost for medicine application is effectively reduced.
7. The utilization rate of the pesticide irrigation can be greatly improved, the prevention and treatment cost is saved, the losses of ineffective waste, leaching loss, soil fixation of a soil application method and the like of the spraying method are avoided, and all pesticide liquid is sent into the target tree body to be fully utilized.
8. Is safe for predation, parasitic natural enemies, people and livestock.
9. Has no residue in water, soil and air, no environmental pollution, no phytotoxicity to crops, and safety to fish, bee and other aquatic organisms.
The soluble solution meets the following technical requirements:
1. the appearance is transparent uniform liquid, and the liquid is still uniform and transparent after being diluted by water.
2. After the product is stored for 7 days at 0 +/-2 ℃, the volume of solid precipitate and/or liquid is not more than 0.3 ml; the content of the original drug is not less than the specified amount after being stored for 14 days at 54 +/-2 ℃.
3. The solution is diluted by 342mg/L standard hard water by 20 times at 30 +/-2 ℃ for 1 hour, and the diluted solution is uniform and has no precipitate.
4. The product is stored at normal temperature, the liquid is not layered and does not deteriorate, and the original physical and chemical properties are still maintained to ensure the exertion of the drug effect.
Drawings
FIG. 1 is a graph showing the absorption of emamectin benzoate soluble solution at different concentrations by punching holes and injecting drugs.
Detailed Description
Example 1
The preparation method comprises the following steps:
a. weighing cyclohexanone and two-thirds to three-fourths of dimethylformamide, pouring into a container, and stirring;
b. and weighing the triphenyl phenol polyoxyethylene polyoxypropylene ether, the triphenyl phenol polyoxyethylene ether, the emamectin benzoate and the isooctyl alcohol polyoxyethylene ether in sequence, pouring into a container, finally flushing the measuring cup with the residual dimethyl formamide, pouring into the container, continuing stirring, observing that the material is clear and transparent, and stopping stirring to obtain the composition.
Example 2
The preparation method comprises the following steps:
a. weighing cyclohexanone and two-thirds to three-fourths of dimethylformamide, pouring into a container, and stirring;
b. and sequentially weighing castor oil polyoxyethylene ether, diphenylethylphenol formaldehyde condensate polyoxyethylene ether, emamectin benzoate and agricultural organic silicon, pouring into a container, finally flushing the measuring cup with the residual dimethylformamide, pouring into the container, continuously stirring, observing the material to be clear and transparent, and stopping stirring to obtain the product.
Example 3
The preparation method comprises the following steps:
a. weighing dimethylbenzene, pouring two-thirds to three-fourths of ethanol into a container, and stirring;
b. and weighing triphenyl ethylphenol polyoxyethylene ether, methylamino abamectin benzoate and sulfonated dioctyl sodium succinate in sequence, pouring the weighed materials into a container, finally flushing the measuring cup with the residual ethanol, pouring the materials into the container, continuously stirring, observing the materials to be clear and transparent, and stopping stirring to obtain the finished product.
Example 4
The preparation method comprises the following steps:
a. weighing dimethyl sulfoxide and two-thirds to three-fourths of isopropanol, pouring into a container, and stirring;
b. and sequentially weighing castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, emamectin benzoate and synergistic ether, pouring into a container, finally flushing the measuring cup with the residual isopropanol, pouring into the container, continuously stirring, observing that the material is clear and transparent, and stopping stirring to obtain the castor oil-polyoxyethylene ether-methyl-amino-abamectin benzoate-synergistic ether-methyl-isopropyl-methyl-ethyl-propyl-methyl-isopropyl-methyl-ethyl-methyl-propyl-methyl-ethyl alcohol measuring and methyl-ethyl-methyl-ethyl alcohol measuring material.
Example 5
The preparation method comprises the following steps:
a. weighing dimethyl sulfoxide and two-thirds to three-fourths of N-methylpyrrolidone, pouring into a container, and stirring;
b. and sequentially weighing castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, emamectin benzoate and isooctanol polyoxyethylene ether, pouring into a container, flushing the measuring cup with the residual N-methyl pyrrolidone, pouring into the container, continuously stirring, observing the material to be clear and transparent, and stopping stirring to obtain the castor oil-based fatty alcohol polyoxyethylene ether.
Example 6
The preparation method comprises the following steps:
a. weighing ethylene glycol monomethyl ether, pouring two-thirds to three-fourths of isopropanol into a container, and stirring;
b. and sequentially weighing castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, emamectin benzoate and dioctyl sodium sulfosuccinate, pouring into a container, finally flushing the measuring cup with the residual isopropanol, pouring into the container, continuously stirring, observing the material to be clear and transparent, and stopping stirring to obtain the castor oil polyoxyethylene ether-methyl-amino-abamectin benzoate-sulfonated dioctyl sodium sulfosuccinate.
Test example:
first, example 1 forest dry injection test
The test method comprises the following steps: through batch drilling, the injection dry dosage is 5-8 ml, the absorption conditions of emamectin benzoate with different contents are measured after 24 hours, data are counted, and a curve graph of the content and the absorption conditions is drawn.
The test results are shown in figure 1, and it can be seen from figure 1 that the absorption is higher than 80% at a concentration of 21% to 30%, and the absorption forms a peak at a concentration of about 22.75%.
When the concentration is lower than 21%, due to the fact that the content of active substances is low, partial operation is not in place possibly during batch drilling, sawdust in partial holes is remained, the actual injection dry dose is not 5-8 ml, and after the concentration is higher than 30%, due to the fact that the viscosity of materials is gradually increased, absorption is gradually difficult.
Test of absorption condition of two, 22.75% emamectin benzoate soluble solution
The test method comprises the following steps: in Fuling white Crane forest park, the absorption of 22.75% methylamino abamectin benzoate soluble solution at different time points was examined, and the results are shown in Table 1.
TABLE 122.75% Emamectin benzoate soluble solution punch injection absorption (%)
As can be seen from Table 1, after 1 hour, the emamectin benzoate soluble solution has an average absorption rate of more than 65 percent, a maximum absorption rate of 90 percent and a fast absorption rate, and after 24 hours, most of the emamectin benzoate soluble solution can be absorbed by 98 percent and almost completely absorbed, so that the absorption rate is fast and the permeability is good.
Test for residual quantity of methylamino abamectin benzoate solution of three, 22.75%
The test method comprises the following steps: in Fuling white Crane forest park, the residual quantity of the effective components of the 22.75 percent methylamino abamectin benzoate soluble solution at different time points is examined, and the results are shown in Table 2.
TABLE 222.75 analysis table for residual quantity of effective components in emamectin benzoate soluble solution
From the results of actual measurement data in table 2, it is found that the residual amount of the 22.75% emamectin benzoate soluble solution in the tree body after punching and injection presents a parabola, the peak point is at 3 months to 8 months after punching and injection, then the residual amount gradually decreases, and the residual amount decreases to about 5% of the peak value after two years, but still is far more than the LC95 value of 0.75mg/kg, which indicates that the effective period is more than 2 years.
Test of control effect of emamectin benzoate 22.75% solution
The test conditions are as follows: at Fuling white Crane forest park, the annual inspection is 1 time, and the annual mortality rate of pine trees in perforated injection fields is recorded in detail. The control area was obtained from 2000 pine trees (labeled at the same time) in the same park near the forest. Remarking: the test area carries out the elimination of the epidemic trees every year in autumn.
The control effect in different years is counted by punching 2000 plants of the plant tree with the pesticide and contrasting 2000 plants of the plant tree with the pesticide, and the result is shown in table 3.
TABLE 322.75 statistics table for preventing and treating emamectin benzoate soluble solution in different years
As can be seen from the results in Table 3, the control effect of the 22.75% emamectin benzoate soluble solution is significantly higher than that of the control area.
According to the LC95 value of the effective components of the emamectin benzoate to the pine wood nematodes, the LC95 value is 0.75mg/L, and the water content of pine branches is about 50%. According to the calculation, when the dry weight of the emamectin benzoate in the pine branches contains the effective component amount of the emamectin benzoate more than 0.75mg/kg, the pine has immunity to the pine wilt disease. According to the measured data, after a 22.75% emamectin benzoate soluble solution is used for punching and injecting the pesticide into the pine tree (5 ml of pesticide is injected according to the diameter of 10-20 cm at breast height, 5ml is increased every 10cm at breast height), the concentration of the emamectin benzoate in the branches reaches 5-10 times of the LC95 value of the pine wood nematode 10 days after the pesticide injection, then the concentration of the emamectin benzoate continues to rise, the residual emamectin benzoate reaches the peak value 3-8 months after the pesticide injection, then the residual emamectin benzoate gradually falls, the average value after two years is 10% -20% of the peak value, but still reaches about 7-10 times of the LC 95. According to the analysis of the degradation rule of emamectin benzoate in pine trees, the residue is still more than 0.75mg/kg LC95 after 3 years, so the effective protection can reach three years.
The above embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention.
Claims (9)
1. An emamectin benzoate soluble solution, which is characterized in that: the soluble agent comprises the following components in percentage by weight: 21-30% of emamectin benzoate, 10-12% of emulsifier, 2-5% of fat dissolving agent, 20-30% of cosolvent and 25-42.25% of solvent.
2. A soluble agent according to claim 1, wherein: the weight percentage of the emamectin benzoate soluble solution is 22.75 percent.
3. A soluble agent according to claim 1 or 2, characterized in that: the emulsifier is at least one selected from triphenylethylphenol polyoxyethylene polyoxypropylene ether, triphenylethylphenol polyoxyethylene ether, diphenylethylphenol formaldehyde condensation compound polyoxyethylene ether, castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether sulfate, fatty amine polyoxyethylene ether and alkyl glycoside.
4. A soluble agent according to claim 1 or 2, characterized in that: the fat dissolving agent is selected from at least one of isooctanol polyoxyethylene ether, agricultural organic silicon, sulfonated dioctyl sodium succinate, synergistic ether, azone and fatty alcohol-polyoxyethylene ether.
5. A soluble agent according to claim 1 or 2, characterized in that: the cosolvent is at least one selected from cyclohexanone, acetone, dimethyl sulfoxide, ethylene glycol monomethyl ether and xylene.
6. A soluble agent according to claim 1 or 2, characterized in that: the solvent is at least one selected from methanol, ethylene glycol, diethylene glycol, dimethylformamide, ethanol, isopropanol and N-methylpyrrolidone.
7. A method for preparing emamectin benzoate soluble solution according to any one of claims 1 to 2, which is characterized in that: the method comprises the following steps:
a. weighing cosolvent, pouring two-thirds to three-fourths of the cosolvent into a container, and stirring;
b. and weighing the emulsifier, the emamectin benzoate and the fat dissolving agent in sequence, pouring into a container, flushing the measuring cup with the residual solvent, pouring into the container, continuously stirring, observing that the material is clear and transparent, and stopping stirring to obtain the composition.
8. The application of the emamectin benzoate soluble solution as claimed in any one of claims 1-2 in preventing and treating pine wilt disease.
9. The use of emamectin benzoate soluble solution according to claim 8 for the control of pine wilt disease, characterized in that: when in use, the emamectin benzoate accounts for 22.75 percent by weight, and the injection amount is 5ml to 8 ml.
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CN114600896A (en) * | 2022-01-14 | 2022-06-10 | 杭州益森键生物科技有限公司 | Efficient permeation and conduction type pine trunk injection agent and preparation method thereof |
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CN102007926A (en) * | 2010-12-14 | 2011-04-13 | 杨凌农科大无公害农药研究服务中心 | Liquid formulation containing emamectin benzoate for trunk injection |
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CN114600896A (en) * | 2022-01-14 | 2022-06-10 | 杭州益森键生物科技有限公司 | Efficient permeation and conduction type pine trunk injection agent and preparation method thereof |
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