CN112205419B - Water dispersible granule containing propamocarb and fosetyl-aluminum and application thereof - Google Patents
Water dispersible granule containing propamocarb and fosetyl-aluminum and application thereof Download PDFInfo
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- CN112205419B CN112205419B CN202011264823.7A CN202011264823A CN112205419B CN 112205419 B CN112205419 B CN 112205419B CN 202011264823 A CN202011264823 A CN 202011264823A CN 112205419 B CN112205419 B CN 112205419B
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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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/12—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing acyclic or cycloaliphatic radicals
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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
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/12—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, neither directly attached to a ring nor the nitrogen atom being a member of a heterocyclic ring
Abstract
The invention discloses a water dispersible granule containing propamocarb and fosetyl-aluminum and application thereof, wherein the weight ratio of propamocarb to fosetyl-aluminum is 1:10-40, and the content is 10-50 wt%. The water dispersible granule has higher control effect than a single agent, and has special effect on fungal diseases on vegetables, particularly downy mildew and epidemic diseases; through the selection of the auxiliary agent, particularly the optimization of the dispersing agent and the wetting agent, the problem of poor heat storage stability of the water dispersible granule prepared from propamocarb and fosetyl-aluminum is solved, so that the water dispersible granule has the advantages of higher suspension percentage, good stability, low degradation rate and good dispersibility, high content of active ingredients of the medicine can be realized, the requirement on a packaging material of the preparation is reduced, the preparation cost is reduced, and the consumption market of the preparation is expanded.
Description
Technical Field
The invention relates to a water dispersible granule containing propamocarb and fosetyl-aluminum and application thereof, belonging to the technical field of pesticides.
Background
Propamocarb (chemical name: 3-dimethylaminopropyl propyl carbamate) belongs to an aliphatic bactericide, is low in toxicity and safe, has a good local systemic effect, can be quickly absorbed by root systems and upwards conveyed to the whole plant after soil treatment, and can be quickly absorbed by leaves to play a role in protection after stem and leaf spraying treatment. The propamocarb has the action mechanism of inhibiting the synthesis of phosphoric acid and fatty acid of germ cell membrane components, and inhibiting the growth and spread of hyphae, the formation of sporangia and the germination of spores. Propamocarb is a broad-spectrum bactericide, is particularly effective on algae class fungi, has good killing effect on fungus such as tow mold, plenophora, peronospora, phytophthora, pythium and the like, and can also be used as a dipping treatment and seed protective agent.
Fosetyl-aluminum (fosetyl-aluminum), chemical name: aluminum tris- (ethylphosphonate), belonging to an organic phosphine bactericide, has therapeutic and protective effects. The fosetyl-aluminum can be conducted in an up-down direction in a plant body, has strong systemic permeability, long lasting period and safe use, and can be widely used for preventing and treating various fungal diseases such as downy mildew, epidemic disease, rot disease, damping-off, black shank, powdery mildew, blight, (pepper) blast, canker, stripe ulcer, scab, anthracnose, ring spot, scab, black spot, brown spot, wheel spot, spot disease, leaf spot, stem leaf spot, rice leaf curl disease, sheath rot and the like of cucumber, melon, watermelon, pumpkin, balsam pear, wax gourd, tomato, hot pepper, eggplant, celery, asparagus, kidney bean, cowpea, pea, mung bean, potato, cruciferous vegetable, tobacco, cotton, apple, grape, pear, strawberry, orange, litchi, vegetable, pepper, banana and flower plants.
The single bactericide is used in large quantity for a long time, so that the diseases are easy to generate drug resistance, the dosage is increased, the control effect is reduced, the lasting period is shortened, and the environment sustainable development is not facilitated. The compounding of the pesticide not only can delay the generation of pesticide resistance, but also can expand the bactericidal spectrum and improve the control effect. At present, a propamocarb and fosetyl-aluminum compound preparation, in particular a water dispersible granule preparation of the propamocarb and the fosetyl-aluminum compound preparation is not seen.
Disclosure of Invention
The invention aims to provide water dispersible granules containing propamocarb and fosetyl-aluminum, which take propamocarb and fosetyl-aluminum as active ingredients of a medicament, have good synergistic effect after being compounded, can improve the sterilization efficiency, expand the sterilization spectrum, reduce the dosage, delay the drug resistance of diseases, prolong the lasting period of the medicament, and are beneficial to relieving sustainable development.
In the water dispersible granule containing propamocarb and fosetyl-aluminum, the active pharmaceutical ingredients are propamocarb and fosetyl-aluminum; the content of the pharmaceutically active ingredient is 10-50wt%, preferably, the content of the pharmaceutically active ingredient is 30-50 wt%. The water dispersible granule can simultaneously play a role in synergism by compounding the active ingredients of the medicines, is more convenient to use, and avoids the problem of high pollution caused by large using amount of a single active ingredient preparation.
Furthermore, in the water dispersible granule, the weight ratio of propamocarb to fosetyl-aluminum is 1: 10-40. The two are compounded within the range, so that the better drug synergism can be exerted, the drug usage amount is reduced, and the drug effect is improved.
Further, the weight ratio of propamocarb to fosetyl-aluminum is preferably 1:10-20, more preferably 1: 15-20. Within the range, the combination of propamocarb and fosetyl-aluminum can exert better effect.
According to the invention, propamocarb and fosetyl-aluminum are prepared into water dispersible granules, so that a good synergistic effect is achieved, but in practical application, the propamocarb has a melting point of 45-55 ℃, is high in water solubility and is easy to absorb moisture and agglomerate; the melting point of the fosetyl-aluminum is 300 ℃, and the fosetyl-aluminum is easy to dissolve in water, absorb moisture and agglomerate; the two raw medicines are easy to absorb moisture and agglomerate, so that the agglomeration of a water dispersible granule product is difficult to disperse, the use is influenced, especially, the propamocarb has the problems of easy granulation stickiness and unsmooth granulation in the processing process due to the lower melting point, easy occurrence of dead granules which cannot be dispersed when heated, poor heat storage stability and possible content degradation, and the problems are more prominent when the content of active ingredients is higher. The problems influence the exertion of the drug effect of the water dispersible granule to a certain extent, and simultaneously, higher requirements on packaging materials and storage conditions of the preparation are provided, and the cost is increased. Therefore, the inventor conducts a great deal of research and experiments, screens the auxiliary agent system (the types of the auxiliary agents, the auxiliary agent components and the auxiliary agent content) and finally obtains the auxiliary agent system with good matching degree, stable performance and good sterilization effect. Through the selection of the auxiliary agents, particularly the screening and combination of 2 auxiliary agents, namely the dispersing agent and the wetting agent, the dispersibility of the effective components in the water dispersible granule in water and the dispersibility of the effective components after heat storage are improved, the caking problem of the preparation is relieved or avoided, the stability of the preparation is improved, and the processing difficulty of the preparation formulation is greatly reduced; the propamocarb and the fosetyl-aluminum can realize lower content and 50% high content when being prepared into water dispersible granules, so that the water dispersible granules have the advantages of high suspension rate, good dispersibility, high disintegration speed, good heat storage stability and the like.
The invention further provides a water dispersible granule containing propamocarb and fosetyl-aluminum, which consists of the following components in percentage by weight: 10-50% of active ingredients of the medicine, 2-10% of dispersing agent, 2-6% of wetting agent, 10-20% of disintegrating agent and the balance of filler.
The water dispersible granule provided by the invention is added with the dispersing agent, the wetting agent, the disintegrating agent and the filler as the auxiliary agents, each auxiliary agent synergistically plays a role, the defect of slow wetting of the granule in water is overcome through the combination of the wetting agent and the filler, the defect of easy agglomeration of suspended particles is overcome through the combination of the dispersing agent and the disintegrating agent, and the granule has the advantages of fast dispersion in water, good atomization, high suspension rate, no decomposition in heat storage and the like, so that the water dispersible granule with fast disintegration speed, good suspension dispersibility and stable heat storage is obtained, and the selection of the type of the auxiliary agent also has certain influence on the drug effect of the water dispersible granule.
Further, the dispersant is one or more than two of calcium lignosulfonate, maleic acid-acrylic acid copolymer salt, polyoxyethylene-polyoxypropylene block copolymer, sodium alkyl phenol sulfonate, sodium alkyl naphthalene sulfonic acid formaldehyde condensate, sodium naphthalene sulfonic acid formaldehyde condensate, ethylene oxide-propylene oxide block copolymer and sodium polycarboxylate.
Further, the wetting agent is one or more than two of sodium dodecyl sulfate, a-sulfo fatty acid methyl ester, tetradecyl sodium sulfate, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, a-olefin sodium sulfonate, sodium alkylphenol polyoxyethylene ether sulfate, sodium lignin sulfonate, nekal BX, fatty acid sulfate and fatty acid ester sulfate.
Further, the disintegrating agent is one or more than two of potassium sulfate, sodium carboxymethylcellulose, potassium chloride, diammonium hydrogen phosphate, urea, sodium sulfate, ammonium sulfate, calcium chloride and sodium chloride.
Further, the filler is one or more than two of kaolin, bentonite, talcum powder, attapulgite, diatomite, white carbon black, starch and light calcium carbonate.
Further, the auxiliary is preferably the following components: the dispersing agent consists of an ethylene oxide-propylene oxide block copolymer and sodium polycarboxylate according to the mass ratio of 1-2: 1; the wetting agent consists of sodium dodecyl benzene sulfonate and fatty acid sulfate in a mass ratio of 1-2.5: 1; the disintegrating agent consists of diammonium hydrogen phosphate and urea according to the mass ratio of 1-1.5: 1; the filler is white carbon black. Under the condition that other components and the proportion are not changed, compared with other auxiliary agents (the auxiliary agents refer to dispersing agents, wetting agents, disintegrating agents and fillers), the water dispersible granule prepared by selecting the optimal auxiliary agent has better thermal stability and processing performance.
Further, the water dispersible granule comprises the following components in percentage by weight: 30-50% of active ingredients of the medicine, 2.5-6% of dispersing agent, 2-3% of wetting agent, 10-15% of disintegrating agent and the balance of filler.
Further, the invention also provides a preparation method of the water dispersible granule, which comprises the following steps:
(1) mixing propamocarb, fosetyl-aluminum, a dispersing agent, a wetting agent, a disintegrating agent and a filler until the mixture is uniformly mixed; the mixing time is preferably 10-20 min.
(2) After mixing, carrying out airflow superfine grinding to obtain powder; the pressure of the airflow superfine grinding is preferably 0.6-0.8 Mpa, the particle size D90 of the obtained powder is preferably 10-20 mu m, and the powder is preferably 99.9% detected by a 325-mesh sieve.
(3) After crushing, adding water into the materials for kneading and granulating; the materials are preferably mixed for 20-30 min, then water is added, preferably in a mixed state, the mass of the added water is 10-20% of the mass of the materials, after the water is added, preferably, the materials are continuously mixed for 2-4 min, and then kneading and granulation are carried out.
(4) Drying after granulation to obtain the water dispersible granule; the drying is preferably boiling drying, which is preferably drying in a boiling fluidized bed; the drying temperature is preferably 40 ℃ to 60 ℃.
The water dispersible granule has the advantages of high suspension rate, good dispersibility, high disintegration speed, good heat storage stability and the like; the water dispersible granule is environment-friendly, free of organic solvent, safe to use and convenient to transport, and can overcome the defects of water dispersible granules prepared from active pharmaceutical ingredients through selection of auxiliaries and the like. The water dispersible granule can be used for preventing and treating vegetable fungal diseases, can delay the generation of medicament resistance, expands the bactericidal spectrum, has good killing effect on a plurality of fungal diseases such as fasciola, aureobasidium, peronospora, phytophthora, pythium, late blight, damping-off, black shank, powdery mildew, fusarium wilt, blast, canker, stripe ulcer, scab, anthracnose, ring spot, scab, black spot, brown spot, wheel spot, leaf spot, stem blight, false smut, sheath rot and the like, and particularly has excellent preventing and treating effect on downy mildew and epidemic diseases.
The invention has the following beneficial effects:
1. the invention prepares the active pharmaceutical ingredients propamocarb and fosetyl-aluminum into water dispersible granules, the two bactericides belong to two different action mechanisms, the mutual mixing of the two bactericides can not generate conflict, but the two bactericides have good synergistic effect and higher control effect than a single dose, and have special effects on fungal diseases on vegetables, particularly downy mildew and epidemic diseases;
2. the water dispersible granule has high sterilization efficiency and small dosage, avoids the drug resistance of diseases, prolongs the drug duration and is beneficial to the sustainable development of the environment;
3. the water dispersible granule of the invention relieves or avoids the problems of poor heat storage stability, easy moisture absorption and easy caking of the water dispersible granule prepared from propamocarb and fosetyl-aluminum through the selection of the auxiliary agent, especially the optimization of the dispersing agent and the wetting agent, has higher suspension percentage, better stability, difficult caking and moisture absorption and good dispersibility, can realize high content of active ingredients of medicaments, reduces the requirement of packaging materials of the preparation, reduces the preparation cost and enlarges the consumption market of the preparation.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited thereto. Unless otherwise specified, the percentages in the following examples are percentages by weight.
Determination of indoor toxicity of propamocarb and fosetyl-aluminum complex on vegetable downy mildew
Indoor toxicity measurement shows that the Synergistic Ratio (SR) of two compounded medicaments in a certain proportion is defined, the SR < 0.5 is antagonism, the SR < 0.5 and less than or equal to 1.5 are additive action, and the SR > 1.5 is synergistic action.
The test agents are all commercially available.
After the effective inhibition concentration range of each medicament is determined through pre-test, each medicament is respectively treated by a series of concentration gradients according to the content of effective components, and clear water is used as a reference. The method is carried out according to 'indoor pesticide bioassay test criteria bactericide', and the toxicity of the medicament on the downy mildew of vegetables is determined by adopting a hypha growth rate method. And measuring the colony diameter by a cross method after 72h, and calculating the net growth amount and the hypha growth inhibition rate of each treatment.
The net growth (mm) is a measure of colony diameter-5
Linear regression was performed using the hyphal growth inhibition ratio y and the drug solution concentration (μ g/mL) x to obtain a virulence regression equation (y ═ a + bx), and EC of each drug was calculated from this equation50The value is obtained. Meanwhile, the combined Synergistic Ratio (SR) of the two medicaments in different proportions is calculated according to the Wadley method, the antagonism is achieved when the SR is less than 0.5, the addition effect is achieved when the SR is more than or equal to 0.5 and less than or equal to 1.5, and the synergism is achieved when the SR is more than 1.5. The calculation formula is as follows:
wherein:
a1 and b1 are respectively the proportion of propamocarb and fosetyl-aluminum in the combination;
a is propamocarb;
b is fosetyl-aluminum.
The test results are shown in table 1:
TABLE 1 toxicity test results analysis table for propamocarb, fosetyl-aluminum and their combinations against vegetable downy mildew
As can be seen from Table 1, the EC of propamocarb and fosetyl-aluminum for downy mildew50Respectively 0.935mg/L and 23.416 mg/L. The toxicity of propamocarb is obviously higher than that of fosetyl-aluminum. The propamocarb and the fosetyl-aluminum both show synergistic effect when mixed in a ratio of 1:10-40, preferably in a ratio of 1:10-20, more preferably in a ratio of 1: 15-20.
In the following, several examples of the water dispersible granule of the present invention are specifically listed to further demonstrate the advantages of the present invention.
Example 121% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: 1% of propamocarb, 20% of fosetyl-aluminum, 1.5% of ethylene oxide-propylene oxide block copolymer, 1.5% of sodium polycarboxylate, 1% of sodium dodecyl benzene sulfonate, 1% of fatty acid sulfate, 7.5% of diammonium hydrogen phosphate, 5% of urea and 100% of white carbon black.
The preparation method comprises the following steps: the components of the formula are put into a pre-mixer to be fully mixed uniformly (for 10-20 minutes), then airflow superfine grinding is carried out to obtain fine powder with the particle size (D90) ranging from 10 to 20 micrometers, the powdery material is subjected to secondary mixing (for 20-30 minutes), a small amount of water is added into a mixer for 10 percent and is kneaded, the mixture is granulated by an extrusion type granulator, and the mixture is dried in a boiling fluidized bed for 3-5 minutes at 60 ℃ to prepare a water dispersible granule product. The product granulation is normal, the phenomenon of sticking is avoided, the granules can be dried at a higher temperature, and the efficiency is improved.
Example 211% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: 1% of propamocarb, 10% of fosetyl-aluminum, 1.5% of ethylene oxide-propylene oxide block copolymer, 1% of sodium polycarboxylate, 1% of sodium dodecyl benzene sulfonate, 1% of fatty acid sulfate, 7.5% of diammonium hydrogen phosphate, 5% of urea and 100% of white carbon black. The preparation method is the same as that of the embodiment 1, the product granulation is normal, the sticking phenomenon is avoided, the particles can be dried at a higher temperature, and the efficiency is improved.
Example 332% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: 2% of propamocarb, 30% of fosetyl-aluminum, 2% of ethylene oxide-propylene oxide block copolymer, 1.5% of sodium polycarboxylate, 1% of sodium dodecyl benzene sulfonate, 1% of fatty acid sulfate, 7.5% of diammonium hydrogen phosphate, 5% of urea and 100% of white carbon black. The preparation method is the same as that of the embodiment 1, the product granulation is normal, the sticking phenomenon is avoided, the particles can be dried at a higher temperature, and the efficiency is improved.
Example 441% Pericarb-fosetyl-Al water dispersible granule
The formula is as follows: 1% of propamocarb, 40% of fosetyl-aluminum, 3% of ethylene oxide-propylene oxide block copolymer, 1.5% of sodium polycarboxylate, 2% of sodium dodecyl benzene sulfonate, 1% of fatty acid sulfate, 7.5% of diammonium hydrogen phosphate, 5% of urea and 100% of white carbon black. The preparation method is the same as that of the embodiment 1, the product granulation is normal, the sticking phenomenon is avoided, the particles can be dried at a higher temperature, and the efficiency is improved.
Example 550% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: 2.5 percent of propamocarb, 47.5 percent of fosetyl-aluminum, 4 percent of ethylene oxide-propylene oxide block copolymer, 2 percent of sodium polycarboxylate, 1 percent of sodium dodecyl benzene sulfonate, 1 percent of fatty acid sulfate, 7.5 percent of diammonium hydrogen phosphate, 7.5 percent of urea and 100 percent of white carbon black
The preparation method is the same as that of the embodiment 1, the product granulation is normal, the sticking phenomenon is avoided, the particles can be dried at a higher temperature, and the efficiency is improved.
Example 621% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: 1% of propamocarb, 20% of fosetyl-aluminum, 4% of sodium polycarboxylate, 1.5% of sodium naphthalene sulfonate formaldehyde condensate, 2% of ethylene oxide-propylene oxide block copolymer, 1% of sodium dodecyl sulfate, 2% of sodium alpha-olefin sulfonate, 20% of sodium chloride and 100% of talcum powder. The preparation method is the same as example 1.
Water dispersible granules were prepared as in example 1, except that: drying the mixture in a boiling fluidized bed for 15-20 minutes at 55 ℃. Through observation and touch, the phenomenon of stickiness appears during granulation, the drying time is longer, and the obtained water dispersible granules are not full in particles and weak in particle strength. The drying temperature is increased, and the problem of high degradation rate occurs in heat storage.
Example 721% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: 1% of propamocarb, 20% of fosetyl-aluminum, 3% of sodium polycarboxylate, 1.5% of calcium lignosulfonate, 1% of sodium dodecyl sulfate, 1% of sodium lignosulfonate, 7.5% of ammonium sulfate, 5% of urea and 100% of kaolin. The preparation method is the same as example 1. The difference is that: drying the mixture in a boiling fluidized bed for 15-20 minutes at 55 ℃. Through observation and touch, the phenomenon of stickiness appears during granulation, the drying time is longer, and the obtained water dispersible granules are not full in particles and weak in particle strength. The drying temperature is increased, and the problem of high degradation rate occurs in heat storage.
Example 811% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: 1% of propamocarb, 10% of fosetyl-aluminum, 1.5% of sodium polycarboxylate, 1.5% of polyoxyethylene-polyoxypropylene block copolymer, 1% of alkylphenol polyoxyethylene ether sodium sulfate, 2% of nekal BX, 25% of sodium chloride and 100% of talcum powder. The preparation method is the same as example 1. The difference is that: drying the mixture in a boiling fluidized bed for 15-20 minutes at 55 ℃. Through observation and touch, the phenomenon of stickiness appears during granulation, the drying time is longer, and the obtained water dispersible granules are not full in particles and weak in particle strength. The drying temperature is increased, and the problem of high degradation rate occurs in heat storage.
Example 932% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: 2% of propamocarb, 30% of fosetyl-aluminum, 4% of alkyl naphthalene sulfonic acid formaldehyde condensate sodium salt, 2% of sodium alkyl phenol sulfonate, 1% of fatty acid ester sulfate, 2% of nekal BX, 22% of calcium chloride and 100% of bentonite. The preparation method is the same as example 1. The difference is that: drying the mixture in a boiling fluidized bed for 15-20 minutes at 55 ℃. Through observation and touch, the phenomenon of stickiness appears during granulation, the drying time is longer, and the obtained water dispersible granules are not full in particles and weak in particle strength. The drying temperature is increased, and the problem of high degradation rate occurs in heat storage.
Example 1041% propamocarb-fosetyl-aluminum Water dispersible granules
The formula is as follows: propamocarb 1%, fosetyl-aluminum 40%, maleic acid-acrylic acid copolymer salt 3%, polyoxyethylene-polyoxypropylene block copolymer 2%, ethylene oxide-propylene oxide block copolymer 1%, fatty acid sulfate 1%, sodium alkylnaphthalene sulfonate 2%, sodium sulfate 20%, and starch to 100%. The preparation method is the same as example 1. The difference is that: drying the mixture in a boiling fluidized bed for 15-20 minutes at 55 ℃. Through observation and touch, the phenomenon of stickiness appears during granulation, the drying time is longer, and the obtained water dispersible granules are not full in particles and weak in particle strength. The drying temperature is increased, and the problem of high degradation rate occurs in heat storage.
Example 1145% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: propamocarb 3%, fosetyl-aluminum 42%, sodium alkyl phenol sulfonate 2%, sodium naphthalene sulfonate formaldehyde condensate 2%, ethylene oxide-propylene oxide block copolymer 1%, sodium dodecyl benzene sulfonate 3.5%, sodium alpha-olefin sulfonate 2%, ammonium nitrate 12.5%, and diatomaceous earth to 100%. The preparation method is the same as example 1. The difference is that: drying the mixture in a boiling fluidized bed for 15-20 minutes at 55 ℃. Through observation and touch, the phenomenon of stickiness appears during granulation, the drying time is longer, and the obtained water dispersible granules are not full in particles and weak in particle strength. The drying temperature is increased, and the problem of high degradation rate occurs in heat storage.
Example 1250% Pericarb-fosetyl-Al Water dispersible granules
The formula is as follows: 2.5 percent of propamocarb, 47.5 percent of fosetyl-aluminum, 3 percent of sodium salt of alkyl naphthalene sulfonic acid formaldehyde condensate, 4 percent of sodium salt of naphthalene sulfonic acid formaldehyde condensate, 1 percent of ethylene oxide-propylene oxide block copolymer, 1 percent of sodium tetradecyl sulfate, 2 percent of sodium alpha-olefin sulfonate, 10 percent of potassium chloride, 5 percent of urea and the total weight of attapulgite to 100 percent. The preparation method is the same as example 1. The difference is that: drying the mixture in a boiling fluidized bed for 15-20 minutes at 55 ℃. Through observation and touch, the phenomenon of stickiness appears during granulation, the drying time is longer, and the obtained water dispersible granules are not full in particles and weak in particle strength. The drying temperature is increased, and the problem of high degradation rate occurs in heat storage.
Comparative example 50% propamocarb-fosetyl-aluminum water dispersible granule
The formula is as follows: 2.5 percent of propamocarb, 47.5 percent of fosetyl-aluminum, 3 percent of dispersant modified lignin, 3 percent of polyoxyethylene ether formaldehyde condensate, 2 percent of wetting agent petroleum sodium sulfonate, 15 percent of disintegrant ammonium nitrate and 100 percent of filler anhydrous sodium sulfate. The water dispersible granules prepared by the method in example 1 have the problems that the stickiness phenomenon is serious during granulation, the drying time is prolonged, the obtained water dispersible granules are not full, the granule strength is very weak, and the degradation is serious during hot storage through observation and touch.
Quality tests were carried out on the propamocarb and fosetyl-aluminum water dispersible granules prepared in the above examples and comparative examples, wherein the screening method was CIPAC MT170, the suspension percentage method was CIPAC MT168, the degradation rate after heat storage was calculated (subtracting the content after heat storage from the content before heat storage and then dividing by the content before heat storage), the heat storage stability method was CIPAC MT46.3, and the dispersibility method was CIPAC MT 174.
TABLE 2 quality index of water dispersible granule prepared by compounding propamocarb and fosetyl-aluminum
In the experimental process, the water dispersible granules in the examples 1 to 5 have no caking, flocculation or precipitation phenomena before and after thermal storage, the products in the examples 6 to 10 have no caking, flocculation or precipitation phenomena before thermal storage, the stability after thermal storage is reduced, and a small amount of large particles appear. The product of the comparative example has a serious caking problem before hot storage, flocculation and sedimentation occur when the product is dissolved in water, and the flocculation and sedimentation phenomenon is more serious after hot storage.
As can be seen from the data in Table 2, the water dispersible granules of examples 1-5 have good dispersibility in water, fast product wetting, high suspension rate and low degradation rate; the water dispersible granules of examples 6-12 have slightly poorer performance than the water dispersible granules of examples 1-5, but the performance is far better than that of the comparative example. And the water dispersible granule of the comparative example is poor in performance, uneven in appearance color, patterned, high in degradation rate, greatly reduced in stability after heat storage, reduced in suspension rate and unqualified.
Experiment of drug effect
1. Taking the propamocarb and fosetyl-aluminum compound preparations of examples 5 and 12 and comparative examples as examples, the water dispersible granules are verified to prevent and control cucumber downy mildew. The experiment is arranged to be carried out in Shandong Shouguang city, and the contrast medicament is 35% propamocarb aqueous solution (purchased from the market) and 40% fosetyl-aluminum wettable powder (purchased from the market).
The cucumber is tested in a vegetable planting area, the cucumber is in the early growth stage, and the disease is in the early occurrence stage. Dividing the test land block into a plurality of cells, wherein each cell has an area of about 100m2The test cells are randomly arranged. The experiment is provided with 5 treatment areas and 1 control area, wherein 5 treatment areas are sprayed with different medicaments, the control areas are sprayed with the same amount of clear water, and each treatment is repeated for 3 times. The cucumber downy mildew is applied at the beginning of disease attack, the application is carried out again at intervals of 7 days, the disease index is investigated 14 days after the second application, and the control effect is calculated.
The test method comprises the following steps: spraying stem and leaf with industrial and agricultural-16 type knapsack hand sprayer, and mixing the preparation with 700kg of water per hectare. The investigation method refers to GB/T17980.19-2000, and the prevention and treatment effect is calculated.
The control effect calculation method comprises the following steps:
during the test, the compound preparation of the invention has no adverse effect on cucumber in the test application range, and the test results are shown in the following table 3:
TABLE 3 efficacy test of propamocarb, fosetyl-aluminum and their combination formulations for controlling cucumber downy mildew
| Treatment agent | The effective component dosage (g/ha) | Control effect (%) 14 days after application |
| Example 5 | 600 | 90.2 |
| Example 12 | 600 | 84.0 |
| Comparative example | 600 | 74.0 |
| 35% propamocarb aqueous solution | 800 | 70.6 |
| 40% wettable fosetyl-aluminum powder | 1400 | 65.2 |
As can be seen from Table 3, the propamocarb and fosetyl-aluminum can effectively prevent and treat cucumber downy mildew after being compounded, and the prevention and treatment effects are superior to those of a control medicament.
2. Taking the propamocarb and fosetyl-aluminum compound preparations of examples 5 and 12 and comparative examples as examples, the water dispersible granules are verified to prevent and treat the sweet pepper phytophthora blight. The experiment is arranged to be carried out in Shandong Shouguang city, and the contrast medicament is 35% propamocarb aqueous solution (purchased from the market) and 40% fosetyl-aluminum wettable powder (purchased from the market).
When the test is carried out in a vegetable planting area, the sweet pepper is in the initial growth stage and the disease is in the initial generation stage. Dividing the test land block into a plurality of cells, wherein each cell has an area of about 100m2The test cells are randomly arranged. The experiment is provided with 5 treatment areas and 1 control area, wherein 5 treatment areas are sprayed with different medicaments, the control areas are sprayed with the same amount of clear water, and each treatment is repeated for 3 times. The sweet pepper epidemic disease is applied at the beginning of the disease, and is applied again at an interval of 7 days, and the second application is examined 14 days later
Calculating the disease index and the prevention and treatment effect.
The test method comprises the following steps: spraying stem and leaf with industrial and agricultural-16 type knapsack hand sprayer, and mixing the preparation with 700kg of water per hectare. The investigation method refers to GB/T17980.19-2000, and the prevention and treatment effect is calculated.
The control effect calculation method comprises the following steps:
during the test, the compound preparation of the invention has no adverse effect on the sweet pepper in the test application range, and the test results are shown in the following table 4:
TABLE 4 pharmacodynamic test of propamocarb, fosetyl-aluminum and its compound preparation for preventing and treating sweet pepper phytophthora blight
As can be seen from Table 4, the propamocarb and fosetyl-aluminum can effectively prevent and treat the blight of sweet peppers after being compounded, and the prevention and treatment effects are superior to those of control medicaments.
Claims (7)
1. A water dispersible granule containing propamocarb and fosetyl-aluminum is characterized in that: the active pharmaceutical ingredients are propamocarb and fosetyl-aluminum; the content of active ingredients of the medicine is 10-50wt%, and the water dispersible granule comprises the following components in percentage by weight: 10-50% of active ingredients of the medicine, 2-10% of dispersing agent, 2-6% of wetting agent, 10-20% of disintegrating agent and the balance of filler;
the dispersing agent consists of an ethylene oxide-propylene oxide block copolymer and a sodium polycarboxylate salt according to the mass ratio of 1-2: 1; the wetting agent consists of sodium dodecyl benzene sulfonate and fatty acid sulfate in a mass ratio of 1-2.5: 1;
the disintegrating agent consists of diammonium hydrogen phosphate and urea according to the mass ratio of 1-1.5: 1;
the filler is white carbon black.
2. Water dispersible granules according to claim 1, characterized in that: the composition comprises the following components in percentage by weight: 30-50% of active ingredients of the medicine, 2.5-6% of dispersing agent, 2-3% of wetting agent, 10-15% of disintegrating agent and the balance of filler.
3. Water dispersible granules according to claim 1 or 2, characterized in that: the weight ratio of the propamocarb to the fosetyl-aluminum is 1: 10-40.
4. Water dispersible granules according to claim 3, characterized in that: the weight ratio of the propamocarb to the fosetyl-aluminum is 1: 10-20.
5. Water dispersible granules according to claim 4, characterized in that: the weight ratio of the propamocarb to the fosetyl-aluminum is 1: 15-20.
6. Use of the propamocarb and fosetyl-aluminum containing water dispersible granules according to any one of claims 1 to 5 for controlling fungal diseases of vegetables.
7. Use according to claim 6, characterized in that: the fungal diseases are downy mildew and epidemic diseases.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998044801A1 (en) * | 1997-04-04 | 1998-10-15 | Rhone Poulenc Agro | Synergetic fungicide composition |
| CN101553124A (en) * | 2006-12-22 | 2009-10-07 | 拜尔农作物科学股份公司 | Pesticide composition comprising fosetyl-aluminium and an insecticide active substance |
| CN106172388A (en) * | 2016-07-26 | 2016-12-07 | 山东润博生物科技有限公司 | The water dispersible granules of a kind of containing trifloxystrobin and phosethyl-Al and application thereof |
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2020
- 2020-11-13 CN CN202011264823.7A patent/CN112205419B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998044801A1 (en) * | 1997-04-04 | 1998-10-15 | Rhone Poulenc Agro | Synergetic fungicide composition |
| US6358938B1 (en) * | 1997-04-04 | 2002-03-19 | Rhone-Poulenc Agro | Synergistic fungicidal composition |
| CN101553124A (en) * | 2006-12-22 | 2009-10-07 | 拜尔农作物科学股份公司 | Pesticide composition comprising fosetyl-aluminium and an insecticide active substance |
| CN106172388A (en) * | 2016-07-26 | 2016-12-07 | 山东润博生物科技有限公司 | The water dispersible granules of a kind of containing trifloxystrobin and phosethyl-Al and application thereof |
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| Title |
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| Synergistic and antagonistic interactions of fungicides against Pythium aphanidermatum on perennial ryegrass;Houston B. Couch等;《Crop Protection》;19911231;第10卷(第5期);第386-390页 * |
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