CN112741083A - Trifluralin missible oil - Google Patents
Trifluralin missible oil Download PDFInfo
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- CN112741083A CN112741083A CN201911050732.0A CN201911050732A CN112741083A CN 112741083 A CN112741083 A CN 112741083A CN 201911050732 A CN201911050732 A CN 201911050732A CN 112741083 A CN112741083 A CN 112741083A
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- trifluralin
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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
-
- 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
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention relates to trifluralin missible oil which comprises trifluralin, an emulsifier and a solvent, and is characterized in that: the solvent comprises N, N-dimethylacetamide and heavy aromatic solvent oil in a feeding mass ratio of 1: 0.5-3. The invention aims at the characteristics of trifluralin and combines an emulsifiable solution system formed by a specific solvent to realize the preparation of the trifluralin emulsifiable solution with high content and low temperature stability. Compared with the existing trifluralin missible oil, the trifluralin missible oil provided by the invention has the advantages that the safety and the environmental protection performance are obviously improved, and meanwhile, the low-temperature stability is realized, and the trifluralin missible oil is not separated out.
Description
Technical Field
The invention belongs to the technical field of pesticide preparations, and particularly relates to trifluralin missible oil.
Background
Trifluralin belongs to dinitroaniline selective and pre-emergence soil treatment herbicides, and is suitable for preventing and killing annual gramineous weeds and part of broad-leaved weeds in crops such as cotton, soybeans, rapes, peanuts, potatoes, sunflowers, carrots, sugarcanes, tomatoes, cauliflowers, orchards, mulberry gardens and the like. Trifluralin belongs to orange crystalBulk drug, molecular formula: c13H16F3N3O4Relative molecular mass 335.279, density 1.337g/cm3Melting point: 48.5 ℃, flash point: solubility in water at 177 ℃, 25 ℃: 0.184g/L at the pH value of 5, easy to dissolve in organic solvent, more than 1000g/L of dissolubility in acetone, chloroform, toluene and ethyl acetate, 33-40g/L of methanol, 50-67g/L of hexane, 240g/L and 480g/L of missible oil, 5 percent and 50 percent of granules, wherein the missible oil is the main preparation for a long time, wherein the 480g/L of the trifluralin missible oil accounts for more than 95 percent of the market of the trifluralin products, the toluene and the xylene are mainly used as solvents, and the dosage of each mu of the preparation is about 100-150 g. Toluene and xylene which are used in a large amount in the existing trifluralin missible oil have low flash points, and have unsafe and non-environment-friendly factors such as easy combustion, easy explosion, toxicity and the like, so that the development of a safe and environment-friendly novel trifluralin missible oil is urgently needed. In addition, the problem that the trifluralin emulsifiable concentrate is generally separated out at low temperature of 0 ℃ and is unqualified in storage in winter is to be solved.
CN107836461A discloses an environment-friendly pesticide emulsifiable concentrate, which comprises an active component, a solvent and a surfactant, wherein the solvent is ethylene glycol diacetate and/or ethylene glycol monoacetate. The patent mainly improves the safety by adopting ethylene glycol diacetate and/or ethylene glycol monoacetate as a solvent to replace the traditional toluene and xylene solvent. Although the method can improve the safety to a certain extent, the ethylene glycol diacetate and/or the ethylene glycol monoacetate are only suitable for preparing low-content (such as 1.8-250 g/L) missible oil, and the low-content missible oil has large field dosage, high solvent dosage, large packaging dosage and great influence on the environment and can not meet the requirement of environmental protection.
Disclosure of Invention
The invention aims to provide trifluralin missible oil which is safe, environment-friendly and good in low-temperature stability.
In order to solve the technical problems, the invention adopts the following technical scheme:
the trifluralin emulsifiable solution comprises trifluralin, an emulsifier and a solvent, wherein the solvent comprises N, N-dimethylacetamide and heavy aromatic solvent oil in a feeding mass ratio of 1: 0.5-3.
According to the invention, through optimization of the solvent, the content of the trifluralin in the trifluralin emulsifiable solution can be improved, and meanwhile, the low-temperature stability of the trifluralin emulsifiable solution is good, so that the production cost is reduced, the transportation is convenient, the field consumption is small, the use amount of the solvent is reduced, and the method is safe and environment-friendly.
Preferably, the feeding mass ratio of the N, N-dimethylacetamide to the heavy aromatic solvent oil is 1: 0.7-2.
Preferably, the content of the N, N-dimethylacetamide is 100-230 g/L.
More preferably, the content of the N, N-dimethylacetamide is 150-230 g/L.
Preferably, the heavy aromatic solvent oil is one or more of No. 100 solvent oil, No. 150 solvent oil and No. 200 solvent oil.
Table 1 below shows the relevant performance parameters for each solvent.
TABLE 1
| Solvent(s) | Distillation range, boiling point/° c | Solubility in water | Volatility | Flash point (closed, DEG C) |
| NN-dimethyl acetamide | 164-166 | Good taste | Is low in | 66℃ |
| No. 100 solvent oil | 158-193 | Good taste | Is low in | 52 |
| No. 150 solvent oil | 175-208 | Good taste | Is low in | 62 |
| No. 200 solvent oil | 200-240 | Good taste | Is low in | 82 |
Preferably, the content of the trifluralin is 200-700 g/L.
More preferably, the content of the trifluralin is 280-700 g/L.
More preferably, the content of the trifluralin is 450-650 g/L.
More preferably, the content of the trifluralin is 500-600 g/L.
According to a specific and preferred embodiment, the trifluralin emulsifiable concentrate consists of trifluralin, an emulsifier and a solvent, wherein the content of the trifluralin is 600g/L, the content of the N, N-dimethylacetamide is 150-230 g/L, and the content of the heavy aromatic solvent oil is 180-265 g/L.
Compared with 480g/L trifluralin emulsifiable concentrate in the prior art, the specific and preferred embodiment has the advantages that the content of the trifluralin is increased by 120g/L, so that the using amount of a solvent in the trifluralin emulsifiable concentrate is reduced, and the using amount of the solvent in a field is reduced due to the increase of the content of the trifluralin in the emulsifiable concentrate, so that the using amount of the solvent in the using process is reduced.
The emulsifier of the emulsifiable concentrate of the invention can be any emulsifier commonly used in the art, such as: alkylphenol polyoxyethylene ether polyoxypropylene ether, polyoxyethylene polyoxypropylene block copolymer, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty amine, epoxy hexane adduct of fatty amide, ester type nonionic emulsifier, hydroxyl-terminated nonionic emulsifier, alkylphenol, aryl phenol, alkylphenol or polyoxyethylene ether or polyoxyethylene polyoxypropylene ether formaldehyde condensate, alkyl polyglucoside, sulfonates, sulfates, phosphate ester and phosphite ester emulsifiers and the like.
The preparation method of the trifluralin emulsifiable concentrate comprises the following steps:
(1) adding trifluralin and an emulsifier into a solvent, controlling the temperature to be more than or equal to 30 ℃, and stirring, mixing and dissolving;
(2) standing and filtering to obtain the trifluralin missible oil.
The other preparation method of the trifluralin missible oil comprises the following steps:
(1) heating the solvent to more than or equal to 50 ℃, adding the emulsifier, and stirring and mixing;
(2) adding trifluralin into the solvent and the emulsifier in the step (1), and stirring until the trifluralin is dissolved;
(3) standing and filtering to obtain the trifluralin missible oil.
Preferably, in the step (1), the temperature is controlled to be 60-70 ℃.
The preparation method has the advantages of simple process, high safety factor, no generation of three wastes and reduction of the field use amount and the solvent use amount of the product.
Due to the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:
the invention aims at the characteristics of trifluralin and combines an emulsifiable solution system formed by a specific solvent to realize the preparation of the trifluralin emulsifiable solution with high content and low temperature stability. Compared with the existing trifluralin missible oil, the trifluralin missible oil provided by the invention has the advantages that the safety and the environmental protection performance are obviously improved, and meanwhile, the low-temperature stability is realized, and the trifluralin missible oil is not separated out.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that these embodiments are provided to illustrate the basic principles, essential features and advantages of the present invention, and the present invention is not limited by the following embodiments. The implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not specified are generally the conditions in routine experiments.
The environment-friendly safe novel missible oil has the following two advantages: firstly, an environment-friendly and safe solvent combination with high flash point and low volatility is used, a higher-content trifluralin missible oil variety is developed, the using amount of pesticide field usage and the using amount of organic solvent are reduced, and the environment safety is improved; and secondly, developing a trifluralin emulsifiable concentrate variety with higher content, dissolving more effective components by using less organic solvent, reducing production and packaging use, and having higher economic benefit. Specifically, the invention enables the content of trifluralin in emulsifiable concentrate to be obviously improved through the integral formula design of solvent combination, thereby enabling the using amount of fields to be small, improving the production and use safety of products, reducing the using amount of solvents, lowering the formula cost and the packaging cost by more than 20%, and simultaneously having good low-temperature stability and meeting the production and storage requirements below 0 ℃.
The heavy aromatic solvent oil in the invention can be a kettle substrate obtained after lower boiling point substances such as benzene, toluene and xylene are extracted by petroleum refining and reforming. The N, N-dimethylacetamide has the advantages of high flash point, strong dissolving capacity, low cost and easy obtainment.
According to some specific and preferred aspects of the present invention, the heavy aromatic mineral spirits are a combination of one or more selected from the group consisting of mineral spirits No. 100, 150, 200.
Example 1
A600 g/L trifluralin emulsifiable concentrate has a specific gravity of 1.13g/mL, and its formula components and proportion are shown in Table 2, flash point, low-temperature stability, field dosage of preparation, and solvent dosage are shown in Table 3.
TABLE 2
The preparation method comprises the following steps: heating the solvent to 65 ℃, adding the required emulsifier, and starting to stir uniformly. And (3) putting the trifluralin solid raw medicine into the heated solvent, starting stirring until the trifluralin raw medicine is completely dissolved, and obtaining liquid with uniform components. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 3
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50－75℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | No separation of raw medicine |
| Low temperature stability (-5 ℃ for 30 days) | No separation of raw medicine |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 33.2 |
Example 2
A600 g/L trifluralin emulsifiable concentrate is calculated by the specific gravity of 1.13g/mL, the components and the proportion of the formula are shown in table 4, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in table 5.
TABLE 4
The preparation method comprises the following steps: heating the solvent to 65 ℃, adding the required emulsifier, and starting to stir uniformly. And (3) putting the trifluralin solid raw medicine into the heated solvent, starting stirring until the trifluralin raw medicine is completely dissolved, and obtaining liquid with uniform components. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 5
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50－75℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | No separation of raw medicine |
| Low temperature stability (-5 ℃ for 30 days) | No separation of raw medicine |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 32.4 |
Example 3
A600 g/L trifluralin emulsifiable concentrate is prepared from the components and proportion shown in Table 6, flash point, low-temp stability, field dosage and solvent dosage shown in Table 7, wherein the specific gravity is 1.13 g/mL.
TABLE 6
The preparation method comprises the following steps: heating the solvent to 50 deg.C, adding the required emulsifier, and stirring. And (3) putting the trifluralin solid raw medicine into the heated solvent, starting stirring until the trifluralin raw medicine is completely dissolved, and obtaining liquid with uniform components. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 7
Example 4
A600 g/L trifluralin emulsifiable concentrate, calculated by specific gravity of 1.13g/mL, has the formula components and the mixture ratio shown in Table 8, and has the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent shown in Table 9.
TABLE 8
The preparation method comprises the following steps: heating the solvent to 55 deg.C, adding the required emulsifier, and stirring. And (3) putting the trifluralin solid raw medicine into the heated solvent, starting stirring until the trifluralin raw medicine is completely dissolved, and obtaining liquid with uniform components. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 9
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50－75℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | No separation of raw medicine |
| Low temperature stability (-5 ℃ for 30 days) | No separation of raw medicine |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 32.4 |
Example 5
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13mg/L, the formula components and the proportion are shown in table 10, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in table 11.
Watch 10
The preparation method comprises the following steps: heating the solvent to 70 ℃, adding the required emulsifier, and starting and stirring uniformly. And (3) putting the trifluralin solid raw medicine into the heated solvent, starting stirring until the trifluralin raw medicine is completely dissolved, and obtaining liquid with uniform components. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 11
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50－75℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stableQualitative (30 days at 0 degree C) | No separation of raw medicine |
| Low temperature stability (-5 ℃ for 30 days) | No separation of raw medicine |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 33.2 |
Example 6
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 12, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 13.
TABLE 12
The preparation method comprises the following steps: heating the solvent to 70 ℃, adding the required emulsifier, and starting and stirring uniformly. And (3) putting the trifluralin solid raw medicine into the heated solvent, starting stirring until the trifluralin raw medicine is completely dissolved, and obtaining liquid with uniform components. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 13
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50－75℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | No separation of raw medicine |
| Low temperature stability (-5 ℃ for 30 days) | No separation of raw medicine |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 32.8 |
Example 7
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 14, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 15.
TABLE 14
The preparation method comprises the following steps: heating the solvent to 70 ℃, adding the required emulsifier, and starting and stirring uniformly. And (3) putting the trifluralin solid raw medicine into the heated solvent, starting stirring until the trifluralin raw medicine is completely dissolved, and obtaining liquid with uniform components. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 15
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50－75℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | No separation of raw medicine |
| Low temperature stability (-5 ℃ for 30 days) | No separation of raw medicine |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 32.8 |
Example 8
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 16, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 17.
TABLE 16
The preparation method comprises the following steps: heating the solvent to 70 ℃, adding the required emulsifier, and starting and stirring uniformly. And (3) putting the trifluralin solid raw medicine into the heated solvent, starting stirring until the trifluralin raw medicine is completely dissolved, and obtaining liquid with uniform components. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 17
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50－75℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | No separation of raw medicine |
| Low temperature stability (-5 ℃ for 30 days) | No separation of raw medicine |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 32.8 |
Example 9
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 18, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 19.
Watch 18
The preparation method comprises the following steps: heating the solvent to 70 ℃, adding the required emulsifier, and starting and stirring uniformly. And (3) putting the trifluralin solid raw medicine into the heated solvent, starting stirring until the trifluralin raw medicine is completely dissolved, and obtaining liquid with uniform components. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 19
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50－75℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | No separation of raw medicine |
| Low temperature stability (-5 ℃ for 30 days) | No separation of raw medicine |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 32.8 |
Comparative example 1
A480 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.05g/mL, the formula components and the mixture ratio are shown in Table 20, and the flash point, the low-temperature stability, the field dosage of the preparation and the solvent dosage are shown in Table 21.
Watch 20
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 21
Comparative example 2
A480 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.05g/mL, the formula components and the mixture ratio are shown in Table 22, and the flash point, the low-temperature stability, the field dosage of the preparation and the solvent dosage are shown in Table 23.
TABLE 22
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 23
| Project index | The result of the detection |
| Flash point (closed) deg.C | 60℃ |
| Low temperature stability (0 ℃ for 7 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (-5 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 100 |
| Solvent usage amount (g/mu) | 48 |
Comparative example 3
The specific gravity of the 480g/L trifluralin emulsifiable solution is calculated by 1.05g/mL, the components and the proportion of the formula are shown in a table 24, and the flash point and the low-temperature stability are shown in a table 25.
Watch 24
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 25
| Project index | The result of the detection |
| Flash point (closed) deg.C | 58℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (-5 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 100 |
| Solvent usage amount (g/mu) | 48.5 |
Comparative example 4
A480 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.05g/mL, the formula components and the proportion are shown in Table 26, and the flash point, the low-temperature stability, the field dosage of the preparation and the solvent dosage are shown in Table 27.
Watch 26
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 27
| Project index | The result of the detection |
| Flash point (closed) deg.C | 38℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | No separation of raw medicine |
| Low temperature stability (-5 ℃ for 30 days) | No separation of raw medicine |
| Dosage (mL/mu) for formulation used in field | 100 |
| Solvent usage amount (g/mu) | 46 |
Comparative example 5
A480 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.05g/mL, the formula components and the mixture ratio are shown in Table 28, and the flash point, the low-temperature stability, the field dosage of the preparation and the solvent dosage are shown in Table 29.
Watch 28
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 29
| Project index | The result of the detection |
| Flash point (closed) deg.C | 60℃ |
| Low temperature stability (0 ℃ for 7 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | No separation of raw medicine |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 100 |
| Solvent usage amount (g/mu) | 48.5 |
Comparative example 6
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the mixture ratio are shown in Table 30, and the flash point, the low-temperature stability, the field dosage of the preparation and the solvent dosage are shown in Table 31.
Watch 30
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 31
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50-75℃ |
| Low temperature stability (0 ℃ for 7 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 35.2 |
Comparative example 7
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 32, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 33.
Watch 32
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 33
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50-75℃ |
| Low temperature stability (0 ℃ for 7 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 35.2 |
Comparative example 8
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the mixture ratio are shown in Table 34, and the flash point, the low-temperature stability, the field dosage of the preparation and the solvent dosage are shown in Table 35.
Watch 34
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 35
Comparative example 9
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 36, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 37.
Watch 36
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 37
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50-75℃ |
| Low temperature stability (0 ℃ for 7 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Preparation fieldApplication amount (mL/mu) | 80 |
| Solvent usage amount (g/mu) | 33.6 |
Comparative example 10
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 38, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 39.
Watch 38
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 39
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50-75℃ |
| Low temperature stability (0 ℃ for 7 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 33.6 |
Comparative example 11
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 40, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 41.
Watch 40
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Table 41
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50-75℃ |
| Low temperature stability (0 ℃ for 7 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 33.6 |
Comparative example 12
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 42, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 43.
Watch 42
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 43
Comparative example 13
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 44, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 45.
Watch 44
| Component name | Proportioning |
| Trifluralin (96%) | 625 g |
| Emulsifier (alkylphenol polyoxyethylene: calcium dodecylbenzene sulfonate) | (55:30) g |
| N, N-dimethyl acetamide | 70 g |
| Mineral spirit No. 100 or 150 or 200 | 350 g |
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
TABLE 45
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50-75℃ |
| Low temperature stability (0 ℃ for 7 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 33.6 |
Comparative example 14
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 46, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 47.
TABLE 46
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 47
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50-75℃ |
| Low temperature stability (0 ℃ for 7 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 33.6 |
Comparative example 15
A600 g/L trifluralin emulsifiable concentrate, the specific gravity of which is calculated by 1.13g/mL, the formula components and the proportion are shown in Table 48, and the flash point, the low-temperature stability, the field dosage of the preparation and the dosage of the solvent are shown in Table 49.
Watch 48
The preparation method comprises the following steps: the trifluralin is heated to more than 50 ℃, and the trifluralin is dissolved into a flowable liquid for later use. Pumping the melted trifluralin and the emulsifier into a solvent, controlling the temperature at 30 ℃, and stirring until all the components are dissolved and fused to obtain a uniform liquid. Standing to normal temperature, and filtering out impurities through a filter to obtain a finished product of the preparation.
Watch 49
| Project index | The result of the detection |
| Flash point (closed) deg.C | 50-75℃ |
| Low temperature stability (0 ℃ for 7 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Low temperature stability (0 ℃ for 30 days) | Separation of the original drug |
| Dosage (mL/mu) for formulation used in field | 80 |
| Solvent usage amount (g/mu) | 33.6 |
As can be seen from the table above, compared with comparative examples 1-15, the content of the 600g/L trifluralin emulsifiable concentrate in the invention is improved by 120g/L, the dosage of the solvent is obviously reduced by about 33%, meanwhile, the flash point and the low-temperature stability of the 600g/L trifluralin emulsifiable concentrate in the invention are obviously superior to those of the comparative examples, and the dosage of the preparation used in fields and the dosage of the solvent are obviously lower than those of the 480g/L comparative examples.
The above-mentioned embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and to implement the present invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (10)
1. A trifluralin missible oil comprises trifluralin, an emulsifier and a solvent, and is characterized in that: the solvent comprises N, N-dimethylacetamide and heavy aromatic solvent oil in a feeding mass ratio of 1: 0.5-3.
2. A trifluralin emulsifiable concentrate according to claim 1, characterized in that: the feeding mass ratio of the N, N-dimethylacetamide to the heavy aromatic solvent oil is 1: 0.7-2.
3. A trifluralin emulsifiable concentrate according to claim 1, characterized in that: the content of the N, N-dimethylacetamide is 100-230 g/L.
4. A trifluralin emulsifiable concentrate according to claim 3, characterized in that: the content of the N, N-dimethylacetamide is 150-230 g/L.
5. A trifluralin emulsifiable concentrate according to claim 1, characterized in that: the heavy aromatic solvent oil is one or a combination of more of No. 100 solvent oil, No. 150 solvent oil and No. 200 solvent oil.
6. A trifluralin emulsifiable concentrate according to claim 1, characterized in that: the content of the trifluralin is 200-700 g/L.
7. A trifluralin emulsifiable concentrate according to claim 6, characterized in that: the content of the trifluralin is 280-700 g/L.
8. Trifluralin emulsifiable concentrate according to claim 7, characterized in that: the content of the trifluralin is 450-650 g/L.
9. A trifluralin emulsifiable concentrate according to claim 8, characterized in that: the content of the trifluralin is 500-600 g/L.
10. Trifluralin emulsifiable concentrates according to one of claims 1 to 9, characterized in that: the trifluralin emulsifiable solution consists of trifluralin, an emulsifier and a solvent, wherein the content of the trifluralin is 600g/L, the content of the N, N-dimethylacetamide is 150-230 g/L, and the content of the heavy aromatic solvent oil is 180-265 g/L.
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| CN201911050732.0A CN112741083A (en) | 2019-10-31 | 2019-10-31 | Trifluralin missible oil |
| PCT/CN2020/095321 WO2021082457A1 (en) | 2019-10-31 | 2020-06-10 | Trifluralin emulsifiable composition |
| AU2020244369A AU2020244369B2 (en) | 2019-10-31 | 2020-06-10 | Trifluralin emulsifiable composition |
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Citations (5)
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|---|---|---|---|---|
| US4213776A (en) * | 1978-12-13 | 1980-07-22 | Uniroyal Ltd. | Herbicidal concentrate containing ketone and amide solvents |
| CN102125029A (en) * | 2010-12-21 | 2011-07-20 | 威海韩孚生化药业有限公司 | Trifluralin emulsion in water and preparation method thereof |
| CN104114022A (en) * | 2012-02-27 | 2014-10-22 | 胡茨曼澳大利亚股份有限公司 | Agrochemical emulsifiable concentrate formulation |
| CN104839155A (en) * | 2015-05-30 | 2015-08-19 | 张掖市农业科学研究院 | Herbicide composition for preventing and killing off volunteer rapes in spring rape fields |
| CN106234376A (en) * | 2016-07-29 | 2016-12-21 | 浙江新农化工股份有限公司 | Containing etoxazole and the Pesticidal combination of Amitraz and preparation thereof and application |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1187532B1 (en) * | 1999-06-22 | 2003-08-06 | Basf Aktiengesellschaft | Herbicidal emulsifiable concentrate compositions of dinitroaniline and oxyacetamide herbicides |
| AU2014274610A1 (en) * | 2013-12-11 | 2015-06-25 | 4Farmers Australia Pty Ltd | Process for Preparing Herbicide Compositions |
| CN110946138A (en) * | 2018-09-26 | 2020-04-03 | 江苏七洲绿色化工股份有限公司 | Trifluralin missible oil and preparation method thereof |
| CN109452267A (en) * | 2018-11-22 | 2019-03-12 | 深圳诺普信农化股份有限公司 | The preparation method and aqueous pesticide formulations of aqueous pesticide formulations |
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2019
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- 2020-06-10 AU AU2020244369A patent/AU2020244369B2/en active Active
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4213776A (en) * | 1978-12-13 | 1980-07-22 | Uniroyal Ltd. | Herbicidal concentrate containing ketone and amide solvents |
| CN102125029A (en) * | 2010-12-21 | 2011-07-20 | 威海韩孚生化药业有限公司 | Trifluralin emulsion in water and preparation method thereof |
| CN104114022A (en) * | 2012-02-27 | 2014-10-22 | 胡茨曼澳大利亚股份有限公司 | Agrochemical emulsifiable concentrate formulation |
| CN104839155A (en) * | 2015-05-30 | 2015-08-19 | 张掖市农业科学研究院 | Herbicide composition for preventing and killing off volunteer rapes in spring rape fields |
| CN106234376A (en) * | 2016-07-29 | 2016-12-21 | 浙江新农化工股份有限公司 | Containing etoxazole and the Pesticidal combination of Amitraz and preparation thereof and application |
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| WO2021082457A1 (en) | 2021-05-06 |
| AU2020244369B2 (en) | 2021-12-02 |
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