CN112056323A - Dioxazine phosphorus microcapsule suspension particle preparation and preparation method thereof - Google Patents
Dioxazine phosphorus microcapsule suspension particle preparation and preparation method thereof Download PDFInfo
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- CN112056323A CN112056323A CN202010614565.4A CN202010614565A CN112056323A CN 112056323 A CN112056323 A CN 112056323A CN 202010614565 A CN202010614565 A CN 202010614565A CN 112056323 A CN112056323 A CN 112056323A
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- water
- diazinon
- soluble capsule
- wall material
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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
- A01N57/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing heterocyclic 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
- A01N25/02—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
Abstract
The invention discloses a diazinon microcapsule suspension particle preparation and a preparation method thereof, wherein diazinon is used as an active ingredient, an oil-soluble capsule wall material and a water-soluble capsule wall material wrap the active ingredient through interfacial polymerization or a layered coating method, and then a thickening agent, an antifreezing agent, a preservative, an antifoaming agent and the like are added to suspend a microcapsule containing the active ingredient in water to finally form a microcapsule suspension agent. The oil-soluble capsule wall material and the water-soluble capsule wall material form a net structure to wrap the effective components. The two capsule materials are combined for use, so that the lasting period of the pesticide is prolonged, the pesticide application times and the pesticide application amount for preventing and controlling pests are reduced, and the yield of fruit trees and crops is improved.
Description
Technical Field
The invention relates to a pesticide and a production technology of a preparation thereof.
Background
The Diazinon (Diazinon) has a chemical name of O, O-diethyl-O- (2-isopropyl-4-methyl-6-pyrimidyl) thiophosphate and also names Diazinon and diosmetin, is a broad-spectrum and high-efficiency organophosphorus insecticide and acaricide, has low Diazinon toxicity, and has contact poisoning, stomach toxicity, fumigation and certain systemic action. The diazinon pesticide has a good control effect on various pests such as Lepidoptera, Homoptera and the like, is mainly used for crops such as rice, cotton, fruit trees, vegetables, sugarcane, corn, tobacco, potato and the like, and is used for controlling piercing-sucking mouthpart pests and leaf eating pests.
Diazinon has the structural formula:
but diazinon has high toxicity to birds, aquatic organisms, bees and the like, is one of common pesticide residue pollutants in water, and biological toxicity experiments show that the diazinon has toxic action to the nervous system of an organism and brings long-term ecological risks to the surrounding ecological environment, and a proper dosage form is needed to control the release rate of the diazinon, improve the utilization rate of effective components and reduce the harm to the ecological environment.
With the adjustment of national pesticide policy, the continuous production limitation and production stoppage of high-toxicity and high-residue pesticides, the continuous development of environmental protection and resource saving policies, the revolution of high-efficiency agriculture and farming systems, the pesticide preparation develops towards the direction of low solvation, water-based granulation, slow release and convenience.
The microcapsule suspending agent is a sustained-release formulation, and has the advantages of long lasting effect, low toxicity, alleviation of phytotoxicity, stable effective components, reduction of the times and dosage of administration, labor saving, resource saving and the like.
The oil-soluble capsule core material is generally selected from water-soluble capsule wall materials, and the water-soluble capsule core material is selected from oil-soluble capsule wall materials; i.e., the wall material should not react with, and be immiscible with, the core.
Patent application No.: 2018109491331 discloses a water-encapsulated microcapsule with water-insoluble high polymer as capsule wall material and its preparation method, wherein the water-encapsulated microcapsule is prepared by coating the outer surface of core material with mixed organic solution containing water-insoluble high polymer compound, water-insoluble polymeric monomer, initiator and cross-linking agent, and then carrying out polymerization reaction and removing solvent. The invention only refers to an application technology of oil-soluble capsule materials.
A thesis of Shuichi of Xinjiang agriculture university in 2008 on application of water-soluble soybean polysaccharide as a coating material of phytase microcapsules is that the phytase microcapsules are prepared by a complex coacervation method of the water-soluble soybean polysaccharide and gelatin, and compared with the high-temperature resistant effect of the phytase microcapsules prepared by a curdlan adsorption method and a sodium alginate solidification method, and the coating effect of self-extracting modified high-molecular water-soluble soybean polysaccharide and commercial water-soluble soybean polysaccharide is compared. The invention only refers to an application technology of water-soluble capsule materials.
Disclosure of Invention
The purpose of the invention is as follows:
the diazinon microcapsule suspension granule preparation and the preparation method thereof are provided, the stability of effective components is improved, the lasting period of the preparation is prolonged, the phytotoxicity to crops is reduced, and the application frequency and the usage amount of underground and fruit tree pests are reduced.
The technical scheme is as follows:
the diazinon microcapsule suspending agent comprises the following components in percentage by mass: 1 to 40 percent of diazinon (preferably 35 to 45 percent), 1 to 5 percent of solvent, 1 to 5 percent of oil-soluble capsule material, 0.01 to 5 percent of water-soluble capsule material, 1 to 10 percent of dispersant, 0.1 to 0.5 percent of defoamer, or 0.05 to 3 percent of thickener, 1 to 5 percent of antifreeze (not easy to freeze when used at the temperature below zero, and also has better control efficiency in winter or frozen soil), 0.1 to 0.5 percent of preservative, and the balance of water is added to 100 percent.
The invention takes diazinon as an active ingredient, the oil-soluble capsule wall material and the water-soluble capsule wall material wrap the active ingredient by a layered coating method or an interfacial polymerization method, or a thickening agent, an antifreezing agent, a preservative, a defoaming agent and the like are added, so that microcapsule particles are finally formed, and a suspension preparation is formed in water after water is supplemented, so that the microcapsule particles containing the active ingredient are suspended in the water.
The particle size of the diazinon microcapsule suspending agent is 1-10 mu m; preferably 1-5 μm.
Preferably, the oil-soluble capsule wall material and the water-soluble capsule wall material form a net structure to wrap the effective components, wherein the oil-soluble capsule wall material forms warps of the net structure, the water-soluble capsule wall material forms wefts of the net structure, and the warps and the wefts are in close contact to form network nodes.
When the diazinon microcapsule suspension is used by adding water, the water-soluble capsule material is firstly dissolved, the effective components are gradually permeated from meshes to exert the drug effect, the oil-soluble capsule material is slowly dissolved, the drug effect can not be released at one time, and the slow-release period is longer.
The weft of the water-soluble capsule material is preferably selected to be at the inner side of the warp of the oil-soluble capsule material, because the diazinon is an organic matter and belongs to an oily substance, the water-soluble capsule material at the inner side is close to the diazinon, so that the water-soluble capsule material is not easy to dissolve and is convenient to store for a long time; the oil-soluble capsule wall material on the outer side is contacted with the air and is not easy to be swelled by trace water vapor in the air. The shelf life of the pesticide is prolonged.
The solvent oil is selected from at least one of 100#, 150#, and 200 #; preferably, the solvent oil is 150 #.
The water-soluble capsule wall material is a polyamine combination and is selected from at least one of ethylenediamine, triethylenetetramine, hexamethylenetetramine and diethylenetriamine; preferably, the polyamine is at least one of ethylenediamine and triethylenetetramine.
The oil-soluble wall material is selected from at least one of toluene-2, 4-diisocyanate, 1, 5-naphthalene diisocyanate, diphenylmethane-4, 4' -diisocyanate and isophorone diisocyanate; preferably, the wall material is at least one selected from toluene-2, 4-diisocyanate and isophorone diisocyanate.
The thickening agent is selected from at least one of xanthan gum, magnesium aluminum silicate, gelatin and sodium carboxymethylcellulose; preferably, the thickening agent is xanthan gum, and can increase the bonding performance of the two capsule materials at the crossed mesh points.
The defoaming agent is at least one selected from long-chain fatty acids, polyethers, silane polyethers and organic silicon; preferably, the defoaming agent is silicone.
The antifreeze is at least one selected from ethylene glycol, glycerol, 1, 2-propylene glycol, isopropanol and urea; preferably, the antifreeze is ethylene glycol.
The preservative is selected from at least one of sodium benzoate, isothiazolinone and potassium sorbate; preferably, the preservative is sodium benzoate.
The dispersing agent is selected from at least one of block polyether, polycarboxylate, naphthalene sulfonate, sodium lignosulfonate, phosphate, alkyl diphenyl sulfonate, polyol ester, calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene and sorbitol monolaurate; preferably, the emulsifier is at least one selected from the group consisting of block polyethers, polycarboxylates and phosphates.
The water is selected from deionized water, ultrapure water, double distilled water, purified water and tap water; preferably, the water is deionized water.
A preparation method;
the invention also provides a preparation method of the diazinon microcapsule suspending agent, which comprises the following steps;
weighing diazinon or a bactericide, a water-soluble capsule material and a solvent, and mixing to obtain a homogeneous phase A;
weighing the defoaming agent, the dispersing agent and water, and mixing to obtain a homogeneous phase B;
weighing the oil-soluble capsule wall material and water, and mixing to obtain a homogeneous phase C;
weighing a dispersing agent (which is convenient for dispersing particles in water), a thickening agent or an antifreezing agent, and mixing to obtain a homogeneous phase D;
and secondly, shearing the mixture B under a high-speed shearing machine, slowly pouring the mixture A into the mixture B at a constant speed while shearing to form an oil-in-water emulsion, wherein the diazinon microcapsules can be uniformly distributed in a water phase system when in use by an external wetting dispersant.
Stirring A + B in a stirrer, and slowly and dropwise adding C into A + B through a peristaltic pump; the stirring speed is 200-800 rpm; preferably 300-;
adding the D into the solution after the dripping is finished to form a homogeneous viscous diazinon microcapsule suspending agent, wherein a dispersing agent, a thickening agent or an antifreezing agent are adhered to the outer surface of the suspended particles;
the water-soluble capsule material is at least one of triethylenetetramine, the oil-soluble wall material is at least one of isophorone diisocyanate, and the water-soluble capsule material and the oil-soluble capsule material are subjected to interfacial polymerization reaction or form hydrogen bonds (between two C =0 and H or between N, H, O), so that the technical product of diazinon and a certain wetting dispersant and emulsifier are better coated to be isolated from water.
Preferably, the rotating direction of the high-speed shearing machine in the step II is opposite to that of the stirring machine in the step III, so that the warp threads and the weft threads of the oil-soluble capsule materials with different rotation directions are formed.
Moreover, the thickness of the shearing blades of the two shearing machines is 0.03-0.3mm, and the thin strip-shaped jet flow is convenient to form when the two shearing machines rotate at high speed, so that the warp and weft with micron-sized dimensions are formed, and the warp and the weft are bonded in a grid shape in a staggered manner.
The stirring speed of the step (c) is 200-; the stirring speed of the step (iv) is 200-.
Controlling the time of the third step and the fourth step to be 0.5-3 h; preferably 1-1.5 h. The stirring dispersion is uniform, and simultaneously, the warp and the weft are better formed, are not easy to tear and break, and are not easy to be disordered and crossed.
Has the advantages that:
1. the diazinon microcapsule suspending agent has mild reaction conditions, can be prepared at room temperature, does not use strong acid or strong base, and has small corrosivity on production equipment;
2. the investment of production equipment is small, the common reaction kettle can be produced by being equipped with a stirring and high-speed shearing machine, and pH monitoring equipment and temperature control equipment are not needed;
3. the preparation process flow is relatively simple, and the production technology is easy to master;
4. the prepared diazinon microcapsule suspending agent has stable quality, uniform particle size, high content of effective components and better storage stability;
5. the pesticide has the advantages of reduced phytotoxicity, increased safety, long efficacy duration and improved pesticide utilization rate.
The diazinon microcapsule suspending agent has high encapsulation efficiency, is applied to the prevention and the treatment of fruit trees and underground pests, can reduce contact spots on the fruit trees and crops, and can prolong the lasting period of the pesticide, reduce the application times and the dosage of the prevention and the treatment of the pests and improve the yield of the fruit trees and the crops by combining two capsule materials.
Drawings
Fig. 1 is an optical microscope picture of a diazinon microcapsule suspension according to the present invention at 400 times magnification;
FIG. 2 is a schematic cross-sectional view of a micro-capsule structure of the present invention in an enlarged scale;
in the figure, 1-capsule core; 2-water soluble capsule wall material (weft); 3-oil soluble capsule wall material (meridian).
Detailed Description
The invention is further illustrated below with reference to examples (table 1).
Table 140% diazinon microcapsule suspension formulation table
Weighing 40% of diazinon, 2% of oil-soluble capsule GT-100, 2.5% of solvent No. 150, 0.33% of water-soluble capsule GT-200,5% of dispersant D-300, 3.4% of xanthan gum, 5% of ethylene glycol, 0.1% of sodium benzoate, 0.1% of defoamer SAG1572, 5% of dispersant D-500,1% of dispersant D-200 and deionized water to complement to 100% by mass. Uniformly mixing a dispersing agent D-300, xanthan gum, ethylene glycol and sodium benzoate to obtain D; dissolving diazinon and an oil-soluble capsule material GT-100 in an organic solvent 150#, and uniformly stirring to obtain an oil phase; dissolving a dispersing agent D-500, a dispersing agent D-200 and a defoaming agent SAG1572 into water to form a water phase; and (2) shearing the water phase for 1min by a high-speed shearing machine, slowly pouring the oil phase into the water phase at a constant speed, shearing at 12000rpm to obtain the particle size with the average particle size of 1-3.5 mu m, dropwise adding the water-soluble capsule material GT-200 by a peristaltic pump under the stirring condition of 350rpm for reacting for 1h, adding D, and continuously stirring for 1h to obtain the 40% diazinon microcapsule suspending agent.
The detection shows that the content of diazinon in the preparation is 40.74%, the encapsulation rate is more than or equal to 90%, the suspension rate is more than or equal to 75%, the wet sieve test is more than or equal to 98%, the detected particle size is 1-6 mu m, the dispersibility is more than or equal to 75%, the pH value is 6-9, the lasting foamability (after 1 min) is less than or equal to 60ml, the heat storage stability is qualified, and the low-temperature stability is qualified.
Test example 1:
results of the storage stability test of the 40% diazinon microcapsule suspension (table 2).
TABLE 240% Dizinophos microcapsule suspension storage stability test results
As can be seen from Table 2, the diazinon microcapsule suspension prepared by the invention has good heat storage stability and low temperature stability.
Test example 2:
the test is used for testing the control effect, recommended application dosage, key application technology and the like of the 40% diazinon microcapsule suspending agent prepared in the embodiment on peanut underground pests in seed dressing, and provides scientific basis for large-area popularization and application.
Test time: 2019.7-2019.9; test site: the test land has flat topography and moderate fertility in Wangchun village of Shandong Linyi city, lan and mountain area. Treatment dose of 40% diazinon microcapsule suspension 5 treatments were set: (1) 250 g/mu of 40% diazinon microcapsule suspending agent; (2) 300 g/mu of 40% diazinon microcapsule suspending agent; (3) 350 g/mu of 40% diazinon microcapsule suspending agent; (4) a control medicament chlorpyrifos microcapsule (Jiatiansheng) 400 g/mu; (5) blank control.
Experimental field example 3:
each processing cell has an area of 200 square meters; peanut variety: sea flower number 1; the average row spacing is 82 cm, the plant spacing is 20 cm, the density is 8130 holes, and each hole is 2 seeds. After seedling alignment, emergence of 200 seedlings was investigated.
(r) influence of seed dressing with 40% diazinon microcapsule suspension on peanut emergence (Table 3)
TABLE 340% Dioxazinophos microcapsule suspension for seed dressing emergence
The test result shows that under the test condition, the emergence rate of the seeds without dressing reaches 99%, the emergence rate of the seeds with the contrast agent reaches 98%, and the emergence rates of the seeds with the 40% diazinon microcapsule suspending agent of 250 ml, 300 ml and 350 ml respectively reach 100%, 98.5% and 98.5%. This indicates that the seed dressing with the 40% diazinon microcapsule suspension has no significant difference in peanut emergence compared with the control group.
② 40 percent diazinon microcapsule suspending agent has effects of seed dressing and peanut underground pest (grub) control (table 4, table 5)
Seed dressing of diazinon microcapsule suspending agent with content of 440% in table for controlling underground pests of peanuts
TABLE 540% diazinon microcapsule suspension for seed dressing to control underground pest of peanut
As can be seen from tables 4 and 5: under the test condition, the harm rate of peanut underground pest plants of blank control is 16.7%, the harm rate of peanut plants is 18.5%, the harm rates of peanut plants and peanut plants dressed with 40% diazinon microcapsule suspending agent and control medicament are both 0, and the plant control effect is 100%.
Claims (7)
1. The diazinon microcapsule suspension particle preparation consists of the following components in percentage by mass: 1 to 40 percent of diazinon, 1 to 5 percent of solvent, 1 to 5 percent of oil-soluble capsule wall material, 0.01 to 5 percent of water-soluble capsule wall material, 1 to 10 percent of dispersant, 0.1 to 0.5 percent of defoaming agent, or 0.05 to 3 percent of thickening agent, 1 to 5 percent of antifreezing agent and 0.1 to 0.5 percent of preservative; supplementing water to 100%; the diazinon is used as an active ingredient, the oil-soluble capsule wall material and the water-soluble capsule wall material wrap or adhere other ingredients through a layered coating method or an interfacial polymerization method, the diazinon microcapsule suspension is finally formed, and the diazinon microcapsule suspension particle preparation is formed after water is supplemented.
2. The diazinon microcapsule suspension particle formulation of claim 1, wherein: the oil-soluble capsule wall material and the water-soluble capsule wall material form a net-shaped structure to wrap the effective components, wherein the oil-soluble capsule wall material forms warps of the net-shaped structure, the water-soluble capsule wall material forms wefts of the net-shaped structure, and the warps and the wefts are in close contact to form network nodes.
3. The diazinon microcapsule suspension particle formulation of claim 1, wherein: the water-soluble capsule material weft is arranged at the inner side of the oil-soluble capsule material warp.
4. The diazinon microcapsule suspension particle formulation of claim 1, wherein: the water-soluble capsule material is at least one selected from ethylenediamine, triethylenetetramine, hexamethylenetetramine and diethylenetriamine; the oil-soluble wall material is selected from at least one of toluene-2, 4-diisocyanate, 1, 5-naphthalene diisocyanate, diphenylmethane-4, 4' -diisocyanate and isophorone diisocyanate; the thickening agent is selected from at least one of xanthan gum, magnesium aluminum silicate, gelatin and sodium carboxymethylcellulose.
5. A preparation method of a diazinon microcapsule suspension particle preparation is characterized by comprising the following steps: comprises the following steps;
weighing diazinon or a bactericide, a water-soluble capsule material and a solvent, and mixing to obtain a homogeneous phase A;
weighing the defoaming agent, the dispersing agent and water, and mixing to obtain a homogeneous phase B;
weighing the oil-soluble capsule wall material and water, and mixing to obtain a homogeneous phase C;
weighing the dispersing agent, the thickening agent or the antifreezing agent, and mixing to obtain a homogeneous phase D;
shearing the B under a high-speed shearing machine, slowly pouring the A into the B at a constant speed while shearing to form oil-in-water emulsion;
stirring A + B in a stirrer, and slowly and dropwise adding C into A + B through a peristaltic pump;
and fourthly, after the dripping is finished, adding the D into the solution to form the homogeneous viscous diazinon microcapsule suspending agent.
6. The method for preparing the suspending granule formulation of the oxazine phosphorus microcapsule of claim 5, wherein: the rotating direction of the high-speed shearing machine in the step II is opposite to that of the stirring machine in the step III so as to form oil-soluble capsule material warps and water-soluble capsule material wefts with different rotating directions.
7. The method for preparing the suspending granule formulation of the oxazine phosphorus microcapsule of claim 5, wherein: the thickness of the shearing paddle of the two shearing machines is 0.03-0.3mm, and the thin strip-shaped jet flow is convenient to form when the two shearing machines rotate at high speed, the warp and weft with micron-sized dimensions are formed, and the warp and the weft are bonded into a grid shape.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4851227A (en) * | 1986-07-31 | 1989-07-25 | Ben-Gurion University Of The Negev Research & Development Authority | Insecticidal composition comprising diazinon and process for the preparation thereof |
| CN102413683A (en) * | 2009-03-04 | 2012-04-11 | 陶氏益农公司 | Microencapsulated insecticide formulations |
| CN105557747A (en) * | 2016-02-02 | 2016-05-11 | 南京高正农用化工有限公司 | Stable pesticide microcapsule suspending agent |
-
2020
- 2020-06-30 CN CN202010614565.4A patent/CN112056323A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4851227A (en) * | 1986-07-31 | 1989-07-25 | Ben-Gurion University Of The Negev Research & Development Authority | Insecticidal composition comprising diazinon and process for the preparation thereof |
| CN102413683A (en) * | 2009-03-04 | 2012-04-11 | 陶氏益农公司 | Microencapsulated insecticide formulations |
| CN105557747A (en) * | 2016-02-02 | 2016-05-11 | 南京高正农用化工有限公司 | Stable pesticide microcapsule suspending agent |
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