Mollusk control water dispersible granule and preparation method thereof
Technical Field
The invention relates to the technical field of pesticide preparation, and particularly relates to a mollusk control water dispersible granule and a preparation method thereof.
Background
Conventionally, the prevention and treatment of mollusks (such as oncomelania, ampullaria gigas, slug, snail and the like) adopts high-efficacy and environment-friendly metaldehyde or niclosamide ethanolamine salt as main drugs, and because the two raw drugs are insoluble in water, the application effect is achieved by preparing the two raw drugs into wettable powder, suspending agent or granules, but the three dosage forms have the defects.
The granules have the advantages that: 1. the transportation is convenient; 2. the storage stability is higher; 3. the production process basically has no dust, and the environmental management cost is low; 4. when in use, no dust drifts, and the influence on operators and the surrounding environment is less. The disadvantages are that: 1. the composition can not be dissolved in water or sprayed, and only can be spread, in order to prevent a large amount of medicine from remaining in the environment, the content of effective components is lower, generally lower than 10%, and the control effect on mollusks on the leaf surfaces of crops is poor because the medicament is distributed on the roots of the crops; 2. the large amount of inactive carriers results in waste and higher transportation costs.
The wettable powder has the advantages that: 1. the transportation is convenient; 2. the content of effective components is high; 3. the storage stability is higher. The disadvantages are that: 1. the production process is dry grinding, the dust is large, and the requirement on environmental management is high; 2. when in use, dust drifts, harms the health of operators, pollutes the environment and easily causes phytotoxicity; 3. the spraying is carried out after being diluted by water, and the spray head is easy to block.
The suspending agent has the advantages that: 1. the production process basically has no dust, and the environmental management cost is low; 2. when in use, no dust drift exists, the influence on operators and the surrounding environment is less, and the pesticide damage and the environmental pollution are not easy to occur; 3. the water-based spraying agent is diluted and then sprayed, so that the residue of the medicine in the environment is reduced, and the spray head is not easy to block. The disadvantages are that: 1. the content of the effective components is lower than that of wettable powder; 2. a large amount of water in the product causes inconvenience and waste in transportation, and increases the transportation cost; 3. the storage stability is poor and the caking is easy.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the mollusk control water dispersible granule which takes metaldehyde and/or niclosamide ethanolamine salt as main medicines and has high content of effective components, short wetting time, high dispersibility and high suspension rate.
The invention also provides a preparation method of the mollusk control water dispersible granule.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a mollusk control water dispersible granule comprises the following components in percentage by mass: 0-85% of metaldehyde, 0-85% of niclosamide ethanolamine, 1-3% of wetting agent, 5-20% of emulsifying dispersant, 0-5% of disintegrating agent, 0-10% of binder, 0.5% of defoaming agent and 100% of carrier;
wherein the dosages of metaldehyde and niclosamide ethanolamine salt cannot be 0 at the same time.
The application method of the water dispersible granule is to dissolve the water dispersible granule in water for spraying, and the water dispersible granule is required to have better dispersibility in water (the wetting time is less than 60 seconds, and the suspension rate and the dispersibility are more than or equal to 90 percent). The preparation process of the methaldehyde and/or niclosamide ethanolamine salt water dispersible granules with high content is not available in the prior art, and the reason is that when the two medicines are used for preparing the water dispersible granules with high content, if the preparation process is not appropriate (including the types and the matching of an emulsifying dispersant and a wetting agent are not matched), the wetting time is long (300 seconds) due to 120 plus materials, the dispersibility is poor (lower than 60%), the suspension rate is low (lower than 60%), the product is particularly characterized in that when the preparation is dispersed in water for spraying and applying, the medicines are difficult to disperse in the water, a formed system is uneven, and even precipitates appear, the medicine effect is influenced and a spray gun is blocked.
The invention takes metaldehyde and/or niclosamide ethanolamine salt as main medicine, and is matched with wetting agent, emulsifying dispersant, disintegrating agent, binder and defoaming agent with proper types and dosage to form an emulsifying dispersion system with strong pertinence of metaldehyde and niclosamide ethanolamine salt, and a wet grinding method is adopted to carry out primary or secondary granulation process to prepare the water dispersible granule.
Preferably, the mollusk control water dispersible granule consists of the following components in percentage by mass: 1-80% of metaldehyde, 10-80% of niclosamide ethanolamine salt, 1-3% of wetting agent, 5-20% of emulsifying dispersant, 0-5% of disintegrating agent, 0-10% of binder, 0.5% of defoaming agent and the balance of carrier to 100%.
More preferably, the mollusk control water dispersible granule consists of the following components in percentage by mass: 2% of metaldehyde, 50% of niclosamide ethanolamine salt, 1-3% of wetting agent, 5-20% of emulsifying dispersant, 0-5% of disintegrating agent, 3-5% of binder, 0.5% of defoaming agent and 100% of carrier.
Or: 40-80% of metaldehyde, 1-3% of wetting agent, 5-20% of emulsifying dispersant, 0-5% of disintegrating agent, 3-5% of binder, 0.5% of defoaming agent and 100% of carrier.
Or: 60% of metaldehyde, 1-3% of wetting agent, 5-20% of emulsifying dispersant, 0-5% of disintegrating agent, 3-5% of binder, 0.5% of defoaming agent and 100% of carrier.
Or: 50-70% of niclosamide ethanolamine salt, 1-3% of wetting agent, 5-20% of emulsifying dispersant, 0-5% of disintegrating agent, 3-5% of binder, 0.5% of defoaming agent and 100% of carrier.
Or: 70% of niclosamide ethanolamine salt, 1-3% of wetting agent, 5-20% of emulsifying dispersant, 0-5% of disintegrating agent, 3-5% of binder, 0.5% of defoaming agent and 100% of carrier.
Preferably, the wetting agent is: one or more of alkylphenol polyoxyethylene, alkylbenzene sulfonate, alkyl naphthalene sulfonate, alkyl sulfate, fatty alcohol polyoxyethylene ether, fatty acid sorbitan ester polyoxyethylene ether or saponin. Wherein, the alkylbenzene sulfonate is preferably sodium dodecylbenzene sulfonate; the alkyl naphthalene sulfonate is preferably sodium dodecyl naphthalene sulfonate.
Preferably, the emulsifying dispersant is: alkyl naphthalene sulfonate formaldehyde condensate, fatty acid ethylene oxide condensate, sodium polycarboxylate, polyacrylic acid derivative, alkylphenol polyoxyethylene phosphate, modified lignosulfonate, alkylglucamide, macromolecular chitosan, alkyl glycoside, sophorolipid, rhamnose, sophorolipid or tea saponin. Among them, the alkyl naphthalene sulfonate formaldehyde condensate is preferably a methyl naphthalene sulfonate formaldehyde condensate.
Preferably, the disintegrating agent is one or a combination of more of anhydrous sodium sulfate, urea, polyvinylpyrrolidone, starch and derivatives, cellulose, or sodium lauryl sulfate.
Preferably, the binder is polyvinyl alcohol or modified starch.
Preferably, the defoamer is a polyether modified organosilane.
Preferably, the carrier is a water-soluble starch.
Compared with the prior art, the invention has the following beneficial effects:
the invention aims to overcome the defects of two high-efficiency and environment-friendly mollusk control medicaments, namely metaldehyde and niclosamide ethanolamine salt, in the prior art, the invention prepares a mollusk (such as oncomelania, ampullaria gigas, slug, snail and the like) control water dispersible granule by using metaldehyde and/or niclosamide ethanolamine salt as main medicaments, matching with a wetting agent, an emulsifying dispersant, a disintegrant, a binder and a defoaming agent and adopting a wet grinding method to carry out primary or secondary granulation, and compared with the original three formulations, the invention keeps good killing effect on mollusks and has the following advantages: 1. the transportation is convenient, and the transportation cost is low; 2. the content of the effective components is high, the dispersibility is good, and the suspension rate is high; 3. the storage stability is higher; 4. the production process basically has no dust, and the environmental management cost is low; 5. the pesticide is diluted by water and sprayed, so that the residue of the pesticide in the environment is reduced, and a spray head is not easy to block; 6. when in use, no dust drift occurs, the influence on operators and the surrounding environment is less, and the pesticide damage and the environmental pollution are not easy to occur.
Detailed Description
The present invention is further described in detail below with reference to specific examples, which are provided for illustration only and are not intended to limit the scope of the present invention. The test methods used in the following examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are, unless otherwise specified, commercially available reagents and materials.
Example 1
A mollusk control water dispersible granule comprises the following components in percentage by mass: 2% of metaldehyde, 50% of niclosamide ethanolamine salt, 2% of sodium dodecyl benzene sulfonate, 8% of methyl naphthalene sulfonate formaldehyde condensate, 2.5% of anhydrous sodium sulfate, 3% of modified starch, 0.5% of polyether modified organosilane and the balance of water-soluble starch to 100%.
The preparation method of the water dispersible granule comprises the following steps: putting various materials into a high-shear homogenizing kettle, adding a proper amount of non-ions, dispersing at a high speed, repeatedly sanding on a sand mill until 95% of particles are smaller than 5 mu m, and granulating by spray drying to obtain the water dispersible granules. The technical indexes of the water dispersible granules prepared in the embodiment are shown in table 1.
TABLE 1
Technical index
|
Results
|
Mass fraction of metaldehyde
|
2.02%
|
Niclosamide ethanolamine salt mass fraction
|
50.8%
|
Wetting time, s
|
56 seconds
|
Wet sieve test (passing 44 μm test sieve)
|
98%
|
Suspension rate
|
95%
|
Dispersibility
|
90%
|
Particle size range (0.2mm-0.5mm)
|
95% |
Example 2
A mollusk control water dispersible granule comprises the following components in percentage by mass: 60% of metaldehyde, 2% of fatty alcohol-polyoxyethylene ether, 5.5% of macromolecular chitosan, 3% of modified lignosulfonate, 3% of cellulose, 5% of modified starch, 0.5% of polyether modified organosilane and the balance of water-soluble starch to 100%.
The preparation method of the water dispersible granule comprises the following steps: putting various materials into a high-shear homogenizing kettle, adding a proper amount of non-ions, dispersing at high speed, repeatedly sanding on a sand mill until 95% of particles are smaller than 5 mu m, performing spray drying granulation to obtain water dispersible granules with small particle size, and continuously spraying water drops containing a binder on the obtained water dispersible granules with small particle size (performing secondary granulation by adopting an agglomeration method) to obtain the water dispersible granules with larger particle size so as to meet the use requirement. The technical indexes of the water dispersible granules prepared in the embodiment are shown in table 2.
TABLE 2
Example 3
A mollusk control water dispersible granule comprises the following components in percentage by mass: 70% of metaldehyde, 3% of fatty alcohol-polyoxyethylene ether, 5% of sodium polycarboxylate, 6% of tea saponin, 3% of cellulose, 3% of modified starch, 0.5% of polyether modified organosilane and the balance of water-soluble starch to 100%.
The preparation method of the water dispersible granule comprises the following steps: putting various materials into a high-shear homogenizing kettle, adding a proper amount of non-ions, dispersing at a high speed, repeatedly sanding on a sand mill until 95% of particles are smaller than 5 mu m, and granulating by spray drying to obtain the water dispersible granules. The technical indexes of the water dispersible granules prepared in the embodiment are shown in table 3.
TABLE 3
Technical index
|
Results
|
Mass fraction of metaldehyde
|
70.5%
|
Wetting time, s
|
53 seconds
|
Wet sieve test (passing 44 μm test sieve)
|
98%
|
Suspension rate
|
93%
|
Dispersibility
|
90%
|
Particle size range (0.2mm-0.5mm)
|
95% |
Example 4
A mollusk control water dispersible granule comprises the following components in percentage by mass: 50% of niclosamide ethanolamine salt, 3% of saponin, 8% of alkylphenol polyoxyethylene ether phosphate, 3.5% of urea, 5% of modified starch, 0.5% of polyether modified organosilane and the balance of water-soluble starch to 100%.
The preparation method of the water dispersible granule comprises the following steps: putting various materials into a high-shear homogenizing kettle, adding a proper amount of non-ions, dispersing at high speed, repeatedly sanding on a sand mill until 95% of particles are smaller than 5 mu m, performing spray drying granulation to obtain water dispersible granules with small particle size, and continuously spraying water drops containing a binder on the obtained water dispersible granules with small particle size (performing secondary granulation by adopting an agglomeration method) to obtain the water dispersible granules with larger particle size so as to meet the use requirement. The technical indexes of the water dispersible granules prepared in the embodiment are shown in table 4.
TABLE 4
Example 5
A mollusk control water dispersible granule comprises the following components in percentage by mass: 70% of niclosamide ethanolamine salt, 3% of sodium dodecyl naphthalene sulfonate, 10% of methyl naphthalene sulfonate formaldehyde condensate, 5% of alkyl glycoside, 3.5% of urea, 5% of modified starch, 0.5% of polyether modified organosilane and the balance of water-soluble starch to 100%.
The preparation method of the water dispersible granule comprises the following steps: putting various materials into a high-shear homogenizing kettle, adding a proper amount of non-ions, dispersing at high speed, repeatedly sanding on a sand mill until 95% of particles are smaller than 5 mu m, performing spray drying granulation to obtain water dispersible granules with small particle size, and continuously spraying water drops containing a binder on the obtained water dispersible granules with small particle size (performing secondary granulation by adopting an agglomeration method) to obtain the water dispersible granules with larger particle size so as to meet the use requirement. The technical indexes of the water dispersible granules prepared in the embodiment are shown in table 5.
TABLE 5
Application example 1
The invention aims at two mollusk control drugs of metaldehyde and niclosamide ethanolamine salt, and prepares a novel dosage form of water dispersible granules by matching with a wetting agent, an emulsifying dispersant, a disintegrating agent and a binder.
Table 6 shows the comparison of water dispersible granules with granules
Remarking: the comparative test is used for preventing and treating vegetable snail.
As can be seen from the comparative application test in table 6, the following differences were observed when similar final control effects were achieved: (1) the granular formulation has the advantages that the application method is broadcast application, most of the medicament is distributed at the roots of crops, the control effect on the mollusks climbing up to the leaf surfaces and the like is poor, and the application method of the water dispersible granule is spray application, the instant control effect on the mollusks climbing up to the leaf surfaces and the like is achieved, and the quick action is high. (2) The consumption of the active ingredients of the granules is high, and the granules are large because the granule medicament is spread to the roots of plants, cannot be completely swallowed by mollusks, and part of the granules remain in the environment to cause waste and pollution. (3) In order to reduce the residue of effective components in the environment, a large amount of carriers are added into the granules to reduce the content of the effective components, so that the dosage of the medicament is larger, and the waste of carriers and transportation is brought.
Application example 2
Table 7 shows the comparison between water dispersible granules and wettable powder
Remarking: the comparative test is the control of mud flat spraying oncomelania
As can be seen from table 7 using the comparison results: (1) the water dispersible granule and the wettable powder have the same control effect under the condition of the same content. (2) The wettable powder takes diatomite, argil, kaolin and other substances which can not be dissolved in water as carriers, and is ground by a dry method, so that the requirement on dust treatment in the production process is high, the grinding efficiency is low, the ground particles are thicker compared with spraying and applying, the suspension rate is low, the particles are easy to accumulate to cause spray gun blockage, and the particles are too light compared with the dissolving operation process, so that the dust drift is easy to cause, the health of operators is harmed, and the phytotoxicity is easy to cause. (3) The water dispersible granule prepared by the invention takes soluble starch as a carrier, and is ground and crushed by a wet method, no dust is generated in the production process, and the grinding effect is good; the granulation method adopted by the invention ensures that the preparation has larger granules, and no dust drift exists in the dissolving operation process during the application; after the preparation is dispersed in water, the suspension rate is higher, smaller particles can be obtained, and the spray gun is not easy to block.
Application example 3
Table 8 shows a comparison of water dispersible granules and suspending agents
Remarking: the comparative test is the control of mud flat spraying oncomelania
From the results of the comparative experiments applied in table 8 it can be seen that: under the condition of similar control effect, the suspending agent dosage form and the water dispersant dosage form are different as follows: (1) under the condition of same raw medicine, when the content of the active ingredients of the water dispersible granule is higher, the system can still be kept stable, and when the suspending agent is processed, the higher the active ingredients are, the more easily the caking is caused. (2) Water dispersible granules can be processed into high-content preparations, so that the dosage of the preparation is greatly reduced, and the suspending agent takes a large amount of water as a carrier, thereby causing inconvenience in transportation and increase in cost.
Comparative example 1
A mollusk control water dispersible granule comprises the following components in percentage by mass: 60% of metaldehyde, 2% of glyceryl stearate, 5.5% of sucrose, 3% of alkyl quaternary ammonium salt, 3% of cellulose, 5% of modified starch, 0.5% of polyether modified organosilane and the balance of water-soluble starch to 100%.
The preparation method of the water dispersible granule is the same as that of example 2. The wetting time of the water dispersible granule prepared in the example is 180 seconds, the suspension percentage is 49%, and the dispersibility is 46%.
Comparative example 2
A mollusk control water dispersible granule comprises the following components in percentage by mass: niclosamide ethanolamine 50%, betaine 3%, lecithin 8%, urea 3.5%, modified starch 5%, polyether modified organosilane 0.5%, and water-soluble starch to make up 100%.
The preparation method of the water dispersible granule is the same as that of example 4. The wetting time of the water dispersible granule prepared in the example is 150 seconds, the suspension percentage is 56%, and the dispersibility is 51%.
Comparative example 3
A mollusk control water dispersible granule comprises the following components in percentage by mass: 2% of metaldehyde, 50% of niclosamide ethanolamine salt, 2% of sodium lauroyl glutamate, 8% of polyethylene glycol, 2.5% of anhydrous sodium sulfate, 3% of modified starch, 0.5% of polyether modified organosilane and the balance of water-soluble starch to 100%.
The preparation method of the water dispersible granule is the same as that of example 1. The wetting time of the water dispersible granule prepared in the example is 210 seconds, the suspension percentage is 42%, and the dispersity is 39%.
The water dispersible granules with high content, easy wetting, high dispersibility and high suspension rate can be prepared only by forming a proper emulsification dispersion system aiming at metaldehyde and niclosamide ethanolamine salt through proper emulsification dispersant types and compatibility.