CN115462388B - Indoxacarb water suspension and preparation method thereof - Google Patents

Indoxacarb water suspension and preparation method thereof Download PDF

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Publication number
CN115462388B
CN115462388B CN202211069915.9A CN202211069915A CN115462388B CN 115462388 B CN115462388 B CN 115462388B CN 202211069915 A CN202211069915 A CN 202211069915A CN 115462388 B CN115462388 B CN 115462388B
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indoxacarb
sodium alginate
ferric chloride
preparation
release
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CN115462388A (en
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刘建华
刘文华
沈建
刘杨
沈连国
王曌倩
袁园
何海燕
周天宇
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Nantong Shi Zhuang Chemical Co ltd
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Nantong Shi Zhuang Chemical Co ltd
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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
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
    • 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
    • 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
    • A01N25/08—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 solids as carriers or diluents
    • A01N25/10—Macromolecular compounds
    • 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
    • A01N25/22—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 ingredients stabilising the active ingredients
    • 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
    • A01N25/26—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 in coated particulate form
    • A01N25/28—Microcapsules or nanocapsules
    • 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
    • A01N61/00—Biocides, pest repellants or attractants, or plant growth regulators containing substances of unknown or undetermined composition, e.g. substances characterised only by the mode of action
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P21/00—Plant growth regulators
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P7/00—Arthropodicides
    • A01P7/04—Insecticides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The application relates to the technical field of pesticides, and in particular discloses an indoxacarb water suspension and a preparation method thereof. The indoxacarb water suspending agent comprises the following raw materials in percentage by mass: 15-25% of slow-release indoxacarb microspheres, 1-5% of dispersing agent, 1-5% of suspending aid, 1-5% of wetting agent, 0.1-5% of other auxiliary agents and the balance of water; the raw materials of the sustained-release indoxacarb microsphere comprise the following components in parts by mass: 10 to 20 parts of indoxacarb technical material, 0.2 to 1 part of humic acid, 0.5 to 1.5 parts of modified ferric chloride and 30 to 50 parts of sodium alginate; and the modified ferric chloride is obtained by pre-coating ferric chloride with sodium alginate. The indoxacarb aqueous suspension prepared by the method has good slow release property and lower pesticide residue rate, so that the problem of pesticide residue can be effectively solved while an excellent pest control effect is achieved.

Description

Indoxacarb water suspension and preparation method thereof
Technical Field
The application relates to the technical field of pesticides, in particular to an indoxacarb water suspension and a preparation method thereof.
Background
Indoxacarb is a broad-spectrum oxadiazine pesticide, and can effectively prevent and treat various pests on crops such as grains, cotton, fruits, vegetables and the like by blocking sodium ion channels in nerve cells of insects to ensure that the nerve cells lose functions and have stomach poisoning effect.
In the actual production process, a mode of improving the adhesive force of the suspending agent and the slow release effect of the indoxacarb original drug is generally adopted, so that a better pest control effect is achieved by prolonging the drug effect of the indoxacarb.
However, in practice, the indoxacarb has the advantages of prolonged efficacy, and easily caused large pesticide residue, and further easily caused a series of problems of certain hidden danger of crop edible safety, environmental pollution and the like.
Disclosure of Invention
In order to achieve an excellent pest control effect and effectively reduce pesticide residues, the application provides the indoxacarb water suspension and a preparation method thereof.
In a first aspect, the present application provides an indoxacarb aqueous suspension, which adopts the following technical scheme:
the indoxacarb water suspending agent comprises the following raw materials in percentage by mass: 15-25% of slow-release indoxacarb microspheres, 1-5% of dispersing agent, 1-5% of suspending aid, 1-5% of wetting agent, 0.1-5% of other auxiliary agents and the balance of water;
the raw materials of the sustained-release indoxacarb microsphere comprise the following components in parts by mass: 10 to 20 parts of indoxacarb technical material, 0.2 to 1 part of humic acid, 0.5 to 1.5 parts of modified ferric chloride and 30 to 50 parts of sodium alginate; and the modified ferric chloride is obtained by pre-coating ferric chloride with sodium alginate.
By adopting the technical scheme, the indoxacarb microsphere is used as a medium for loading the indoxacarb technical, and the indoxacarb technical, humic acid and modified ferric chloride are simultaneously loaded on the basis of using sodium alginate as a microsphere base material, so that the pesticide residue can be effectively reduced while the good indoxacarb technical slow release performance and adhesiveness are achieved. The specific scheme is as follows: firstly, the sodium alginate is used as a microsphere base material, has good adhesive force, can improve the adhesion effect of the indoxacarb technical on crops, and has good slow release effect of the carried indoxacarb technical, thereby achieving good pest control effect. In addition, both the modified ferric chloride and the humic acid are loaded on a sodium alginate substrate together with indoxacarb raw material; the humic acid can promote the red shift of the absorption spectrum of the indoxacarb raw medicine, so that the energy absorption efficiency of the indoxacarb raw medicine is slowed down, thereby playing a role in light shielding on the indoxacarb raw medicine, namely effectively inhibiting the photodegradation of the indoxacarb raw medicine. Furthermore, the degradation loss of the indoxacarb original drug is slowed down at the initial stage of storing and validating the indoxacarb aqueous suspension agent, and the pest control effect is improved. The modified ferric chloride obtained by coating the ferric chloride with the sodium alginate in advance can be relatively stably positioned in the sodium alginate base material in the storage stage, so that the contact with the indoxacarb technical product and humic acid is less, and the photodegradation effect of the indoxacarb technical product is promoted to be less.
Meanwhile, after the application, the sodium alginate substrate is gradually decomposed under the influence of the environment, and the indoxacarb technical, humic acid and ferric chloride are gradually separated out. The indoxacarb raw medicine plays a good pest control effect in the early stage of application, and the effect of the hyaluronic acid in inhibiting photodegradation is greater than the effect of ferric chloride in promoting photodegradation in the period that the indoxacarb raw medicine takes effect, namely, the photodegradation rate of the indoxacarb raw medicine is slower, and the negative influence on the control effect is smaller. And over time the humic acid interacts with ferric chloride to form humic acid-Fe 3+ The complex has excellent photodegradation promoting effect, so that the residual indoxacarb raw medicine is effectively promoted to be photodegradation, namely the residual quantity of the indoxacarb raw medicine is effectively reduced in the later period of medicine application.
In addition, humic acid has the effects of fattening soil, promoting crop growth and enhancing crop stress resistance, and has good practical effect.
In conclusion, the method can effectively inhibit photodegradation of the indoxacarb technical product in the storage stage, so that loss of the indoxacarb technical product is reduced. And the photodegradation accelerating effect of the ferric chloride is covered up by the photodegradation inhibiting effect of the humic acid in the early stage of the application, namely the degradation of the indoxacarb raw medicine in the early stage of the application is reduced, and the excellent control effect is maintained. In addition, in the later period of application, the sodium alginate is gradually decomposed, and the humic acid and ferric chloride gradually interact to generate humic acid-Fe 3+ The complex effectively improves the photodegradation rate of the indoxacarb raw material, thereby realizing indeneThe low residue effect of the carbofuran in the later period effectively ensures the edible safety of crops and reduces the environmental pollution.
In a specific embodiment, the preparation method of the sustained-release indoxacarb microsphere comprises the following steps:
preparing sodium alginate solution: dissolving sodium alginate in water to prepare sodium alginate solution, and dividing the sodium alginate solution into A, B parts for later use;
preparing modified ferric chloride: adding ferric chloride into the sodium alginate solution A, fully mixing, then dropwise adding a calcium chloride solution for granulating, and sequentially washing and filtering to obtain modified ferric chloride for later use after low-temperature treatment;
microsphere preparation: adding humic acid and indoxacarb raw material into the sodium alginate solution of the part B, adding modified ferric chloride, fully mixing, then dripping calcium chloride solution for granulating, and washing and filtering to obtain the slow-release indoxacarb microsphere after low-temperature treatment.
By adopting the technical scheme, in the process of preparing the sustained-release indoxacarb microsphere, the sodium alginate solution is divided into A, B parts, and the sodium alginate solution A part is used for coating ferric chloride, namely the modified ferric chloride is obtained in advance for standby. And then the modified ferric chloride is mixed with the indoxacarb technical and the humic acid in the sodium alginate solution of the part B, and the modified ferric chloride is obtained by coating the ferric chloride with the sodium alginate in advance, so that the situation that the ferric chloride contacts with the humic acid and the indoxacarb technical in the sustained-release indoxacarb microspheres can be effectively reduced, and the loss of the indoxacarb technical in the initial stage of storage and drug application can be effectively reduced.
In a specific embodiment, in the sodium alginate solution preparation step, the pH of the sodium alginate solution is adjusted to 4 to 5.
By adopting the technical scheme, the pH value of the sodium alginate solution is controlled to be 4-5, so that the condition that ferric chloride precipitates due to overhigh pH value can be effectively reduced, and the stability of the ferric chloride in the sodium alginate solution is maintained.
In a specific embodiment, in the sodium alginate solution preparation step, the mass concentration of the prepared sodium alginate solution is 2% -3%.
By adopting the technical scheme, the mass concentration of the sodium alginate solution is 2% -3%, the obtained sustained-release indoxacarb microsphere has good morphology and mechanical strength, the sustained-release rate and the release amount of the indoxacarb raw medicine after application are suitable, and the time state of gradual decomposition in the application period is matched with the prevention and treatment process of the indoxacarb raw medicine.
In a specific embodiment, in the modified ferric chloride preparation step and the microsphere preparation step, the mass concentration of the calcium chloride solution is 1% -2%.
By adopting the technical scheme, the mass concentration of the calcium chloride solution is controlled to be 1% -2%, the density of microspheres formed by crosslinking calcium chloride and sodium alginate is proper, and the slow release rate and the release amount of the indoxacarb raw drug in the slow release indoxacarb microspheres after the drug application are proper.
In a specific and possible embodiment, in the microsphere preparation step, the crude sustained-release indoxacarb microsphere is obtained after the drying treatment, the crude sustained-release indoxacarb microsphere is added into salicylate, and the drying treatment is carried out after the complete mixing, so that the finished sustained-release indoxacarb microsphere is obtained.
By adopting the technical scheme, sodium alginate can be degraded to a certain extent during the storage of the indoxacarb aqueous suspension, and the indoxacarb technical product, humic acid and ferric chloride can be separated out in a smaller amount. Therefore, in the microsphere preparation step, the crude sustained-release indoxacarb microsphere is added into salicylate, so that a salicylate protective layer is formed on the surface of the finished sustained-release indoxacarb microsphere. Because the salicylate has better ultraviolet absorption effect, the degradation of the sodium alginate and indoxacarb in the storage process can be effectively reduced. And after the pesticide is applied, the salicylate protective layer can be damaged and degraded in a short time under the influence of environmental factors, namely the salicylate protective layer has less negative influence on the decomposition process of sodium alginate after the pesticide is applied. In addition, the salicylate has a good antibacterial effect, has a positive effect on improving the disease resistance of crops, and has excellent practical significance.
In a specific embodiment, the particle size of the finished sustained release indoxacarb microsphere is 2-3 mm.
By adopting the technical scheme, the particle size of the finished sustained-release indoxacarb microsphere is controlled to be 2-3 mm, and the dispersed phase and suspension effect of the sustained-release indoxacarb microsphere in the water suspension agent system are improved.
In a specific embodiment, the suspending aid is diammonium phosphate and ammonium nitrate in a mass ratio of 1: (2.5-4.2).
By adopting the technical scheme, the suspending aid effect is excellent by compounding the diammonium hydrogen phosphate and the ammonium nitrate according to the mass ratio.
In a second aspect, the present application provides a preparation method of indoxacarb aqueous suspension, which adopts the following technical scheme: the preparation method of the indoxacarb water suspension agent comprises the following steps: fully mixing the raw materials of the indoxacarb water suspending agent to obtain a mixed solution; and sequentially carrying out wet sanding and shearing dispersion treatment on the mixed solution to obtain the finished indoxacarb aqueous suspension.
In a specific embodiment, the finished indoxacarb aqueous suspension is stored in the dark.
In summary, the present application has the following beneficial effects:
1. the preparation method can effectively inhibit photodegradation of the indoxacarb technical product in the storage stage, and reduce loss of the indoxacarb technical product. The photodegradation accelerating effect of the ferric chloride is covered up by the photodegradation inhibiting effect of the humic acid in the early stage of the application, the degradation of the indoxacarb raw material in the early stage of the application is reduced, and the excellent control effect is maintained. In addition, in the later period of application, along with the gradual decomposition of sodium alginate and the gradual interaction of humic acid and ferric chloride, humic acid-Fe is generated 3+ The complex effectively improves the photodegradation rate of the indoxacarb technical, thereby realizing the low-residue effect of the indoxacarb technical in the later period.
2. According to the preparation method, the preparation process of the sustained-release indoxacarb microspheres is optimized, the condition that ferric chloride generates a precipitate is reduced by optimizing the pH value, and the release rate and the release amount of indoxacarb raw medicine in the sustained-release indoxacarb microspheres are more suitable after the sustained-release indoxacarb microspheres are applied by optimizing the concentration of sodium alginate solution and the concentration of calcium chloride solution, so that the decomposition process of sodium alginate is more suitable with the effective process of indoxacarb raw medicine.
3. The salicylic acid ester protective layer is further formed on the surface of the finished product sustained-release indoxacarb microsphere, so that the degradation condition of sodium alginate in the storage process is further reduced, and the method has positive significance for maintaining the stability of indoxacarb technical, humic acid and ferric chloride in the storage process.
Detailed Description
The present application will be described in further detail with reference to preparation examples, examples and comparative examples, and the raw materials to which the present application relates are all commercially available.
Preparation example 1
The slow-release indoxacarb microsphere comprises the following raw materials in mass: indoxacarb technical 1.6kg, humic acid 0.07kg, modified ferric chloride 0.1kg and sodium alginate 4kg; the modified ferric chloride is prepared by pre-coating ferric chloride with sodium alginate, and the content of the ferric chloride in the modified ferric chloride is 30%.
The preparation method of the sustained-release indoxacarb microsphere comprises the following steps:
preparing A1 sodium alginate solution: dissolving 4.07kg of sodium alginate in water to prepare sodium alginate solution with the mass concentration of 2%, then adjusting the pH value of the sodium alginate solution to be 4 by using 10wt% of hydrochloric acid, and dividing the sodium alginate solution into A, B parts for later use according to the mass ratio of 1:50;
a2, preparing modified ferric chloride: adding 0.03kg of ferric chloride into the sodium alginate solution of the part A, fully mixing, then dropwise adding a calcium chloride solution with the mass concentration of 2% for granulation, fixing for 2 hours at the temperature of 3 ℃, washing for three times by using a sodium chloride solution with the mass concentration of 1%, and filtering to obtain modified ferric chloride for later use;
a3, preparing microspheres: adding humic acid and indoxacarb raw materials into the sodium alginate solution of the part B, fully mixing, then adding modified ferric chloride, continuously mixing, then dropwise adding calcium chloride solution with the mass concentration of 2% for granulating, fixing for 2 hours at the temperature of 3 ℃, washing for three times by using sodium chloride solution with the mass concentration of 1%, and filtering at room temperature to obtain the sustained-release indoxacarb microspheres with the particle size of 1-2 mm.
Preparation example 2
The preparation example differs from preparation example 1 in that humic acid is 0.02kg, modified ferric chloride is 0.05kg, and the sodium alginate and ferric chloride addition amounts and the mass ratio of A, B parts of sodium alginate solution in the preparation method are adjusted accordingly.
Preparation example 3
The preparation example differs from preparation example 1 in that humic acid is 0.1kg, modified ferric chloride is 0.05kg, and the sodium alginate and ferric chloride addition amounts and the mass ratio of A, B parts of sodium alginate solution in the preparation method are adjusted accordingly.
Preparation example 4
The preparation example differs from preparation example 1 in that humic acid is 0.1kg, modified ferric chloride is 0.15kg, and the sodium alginate and ferric chloride addition amounts and the mass ratio of A, B parts of sodium alginate solution in the preparation method are adjusted accordingly.
Preparation example 5
The preparation example differs from preparation example 1 in that humic acid is 0.02kg, modified ferric chloride is 0.15kg, and the sodium alginate and ferric chloride addition amounts and the mass ratio of A, B parts of sodium alginate solution in the preparation method are adjusted accordingly.
Preparation example 6
The difference between this preparation example and preparation example 1 is that in the preparation step of the sodium alginate solution A1, the pH of the sodium alginate solution is adjusted to 5.
Preparation example 7
The difference between this preparation example and preparation example 1 is that in the preparation step of the sodium alginate solution A1, the pH of the sodium alginate solution is adjusted to 7.
Preparation example 8
The difference between this preparation example and preparation example 1 is that in the preparation step of the sodium alginate solution A1, the pH of the sodium alginate solution is adjusted to 3.
Preparation example 9
The preparation example differs from the preparation example 1 in that in the preparation step of the sodium alginate solution A1, the mass concentration of the prepared sodium alginate solution is 3%, and the addition amount of ferric chloride and the mass ratio of the A, B part of sodium alginate solution are correspondingly adjusted.
Preparation example 10
The preparation example differs from the preparation example 1 in that in the preparation step of the sodium alginate solution A1, the mass concentration of the prepared sodium alginate solution is 5%, and the addition amount of ferric chloride and the mass ratio of the A, B part of sodium alginate solution are correspondingly adjusted.
PREPARATION EXAMPLE 11
The preparation example differs from the preparation example 1 in that in the preparation step of the sodium alginate solution A1, the mass concentration of the prepared sodium alginate solution is 1%, and the addition amount of ferric chloride and the mass ratio of the A, B part of sodium alginate solution are correspondingly adjusted.
Preparation example 12
The difference between this preparation example and preparation example 1 is that the mass concentration of the calcium chloride solution in the preparation method is 1%.
Preparation example 13
The difference between this preparation example and preparation example 1 is that the mass concentration of the calcium chloride solution in the preparation method is 3%.
PREPARATION EXAMPLE 14
The difference between this preparation example and preparation example 1 is that the mass concentration of the calcium chloride solution in the preparation method is 0.5%.
Preparation example 15
The preparation example is different from the preparation example 1 in that in the preparation step of the A3 microsphere, humic acid and indoxacarb raw material are added into a sodium alginate solution of a part B, after being fully mixed, modified ferric chloride is added for continuous mixing, then calcium chloride solution with the mass concentration of 2% is added dropwise for granulation, the mixture is fixed for 2 hours at the temperature of 3 ℃, then sodium chloride solution with the mass concentration of 1% is used for washing for three times, and the mixture is filtered at room temperature to obtain crude slow-release indoxacarb microsphere with the particle size of 1-2 mm;
adding the crude sustained-release indoxacarb microsphere into salicylate, fully mixing, and filtering to obtain the finished sustained-release indoxacarb microsphere with the particle size of 2-3 mm.
Comparative preparation example 1
This comparative preparation differs from preparation 1 in that no humic acid was added.
Comparative preparation example 2
The comparative preparation differs from preparation 1 in that no modified ferric chloride was added, corresponding preparation method was as follows:
preparing A1 sodium alginate solution: sodium alginate is dissolved in water to prepare sodium alginate solution with the mass concentration of 2%, and then 10wt% hydrochloric acid is used for adjusting the pH value of the sodium alginate solution to be 4;
a3, preparing microspheres: adding humic acid and indoxacarb raw medicine into sodium alginate solution, fully mixing, then dropwise adding calcium chloride solution with the mass concentration of 2% for granulation, fixing for 2 hours at the temperature of 3 ℃, washing for three times by using sodium chloride solution with the mass concentration of 1%, and filtering to dryness at room temperature to obtain the sustained-release indoxacarb microsphere with the particle size of 1-2 mm.
Comparative preparation example 3
The comparative preparation differs from preparation 1 in that the modified ferric chloride is replaced by an equivalent amount of ferric chloride, corresponding to the preparation method as follows:
preparing A1 sodium alginate solution: sodium alginate is dissolved in water to prepare sodium alginate solution with the mass concentration of 2%, and then 10wt% hydrochloric acid is used for adjusting the pH value of the sodium alginate solution to be 4;
a3, preparing microspheres: adding humic acid, indoxacarb technical and ferric chloride into a sodium alginate solution, fully mixing, then dropwise adding a calcium chloride solution with the mass concentration of 2% for granulation, fixing for 2 hours at the temperature of 3 ℃, washing for three times by using a sodium chloride solution with the mass concentration of 1%, and filtering at room temperature to obtain the sustained-release indoxacarb microspheres with the particle size of 1-2 mm.
Example 1
The indoxacarb water suspending agent comprises the following raw materials in mass: 20kg of slow-release indoxacarb microspheres, 3kg of dispersing agent, 4kg of suspending aid, 2kg of wetting agent, 3.5kg of other auxiliary agents and 67.5kg of water;
wherein the sustained-release indoxacarb microsphere is prepared in preparation example 1;
the dispersing agent is sodium dodecyl sulfate;
the suspending aid is diammonium hydrogen phosphate and ammonium nitrate according to the mass ratio of 1:3.2 a mixture of;
the wetting agent is phenethyl phenylpropyl phenol polyoxyethylene ether;
the other auxiliary agents are defoamer, antifreezing agent, preservative and thickener according to the mass ratio of 1:1:1:1, wherein the defoaming agent is butanol, the antifreezing agent is glycerol, the preservative is sodium salicylate, and the thickening agent is polyvinyl alcohol.
The preparation method of the indoxacarb water suspending agent comprises the following steps:
fully mixing the raw materials of the indoxacarb water suspending agent to obtain a mixed solution; and (3) carrying out wet sanding on the mixed solution for 2 hours, then carrying out shearing and dispersing treatment on the mixed solution after wet sanding, wherein the rotating speed of the shearing and dispersing process is 7000rpm, and shearing and dispersing for 20 minutes to obtain the finished indoxacarb aqueous suspension, and storing in a dark place.
Examples 2 to 5 differ from example 1 in the proportions of the raw materials, as shown in the following table:
table 1 raw materials proportioning table of indoxacarb aqueous suspension
Raw materials/kg Example 1 Example 2 Example 3 Example 4 Example 5
Sustained release indoxacarb microsphere 20 15 18 22 25
Dispersing agent 3 2 1 5 4
Suspending aid 4 1 3 2 5
Wetting agent 2 1 5 4 3
Other auxiliary agents 3.5 1 0.1 2.5 5
Water and its preparation method 67.5 80 72.9 64.5 58
Examples 6 to 19 are different from example 1 in that the sustained-release indoxacarb microspheres are prepared from different preparation examples, and specific corresponding relations are shown in the following table.
Table 2 table of correspondence between sustained-release indoxacarb microspheres and preparation examples in examples
Example 6 Preparation example 2
Example 7 Preparation example 3
Example 8 Preparation example 4
Example 9 Preparation example 5
Example 10 Preparation example 6
Example 11 Preparation example 7
Example 12 Preparation example 8
Example 13 Preparation example 9
Example 14 Preparation example 10
Example 15 PREPARATION EXAMPLE 11
Example 16 Preparation example 12
Example 17 Preparation example 13
Example 18 PREPARATION EXAMPLE 14
Example 19 Preparation example 15
Example 20
The difference between this example and example 1 is that the suspending aid is diammonium phosphate and ammonium nitrate according to a mass ratio of 1: 2.5.
Example 21
The difference between this example and example 1 is that the suspending aid is diammonium phosphate and ammonium nitrate according to a mass ratio of 1: 4.2.
Example 22
The difference between this example and example 1 is that the suspending aid is diammonium phosphate and ammonium nitrate according to a mass ratio of 1: 1.
Example 23
The difference between this example and example 1 is that the suspending aid is diammonium phosphate and ammonium nitrate according to a mass ratio of 1: 6.
Comparative example 1
This comparative example differs from example 1 in that the extended release indoxacarb microsphere was prepared from comparative preparation 1.
Comparative example 2
This comparative example differs from example 1 in that the extended release indoxacarb microsphere was prepared from comparative preparation 2.
Comparative example 3
This comparative example differs from example 1 in that the extended release indoxacarb microsphere was prepared from comparative preparation 3.
Comparative example 4
This comparative example differs from example 1 in that the sustained release indoxacarb microspheres are replaced with an equivalent amount of indoxacarb drug substance.
Comparative example 5
The indoxacarb water suspending agent comprises the following raw materials in mass: 15kg of indoxacarb technical, 2kg of dispersing agent, 1kg of wetting agent, 1.5kg of suspending aid, 1kg of thickening agent, 1kg of defoaming agent, 0.5kg of antifreezing agent, 0.5kg of preservative and water to 100kg; wherein the dispersing agent is sodium lignin sulfonate; the wetting agent is alkyl naphthalene sulfonate; the suspending aid is ammonium nitrate; the thickener is xanthan gum; the defoaming agent is methyl silicone oil; the antifreezing agent is glycerol; the preservative is sodium benzoate.
The preparation method of the indoxacarb water suspending agent comprises the following steps:
fully mixing the raw materials to obtain a mixture, and grinding the mixture for 3 hours to obtain a crude water suspension; and (3) carrying out homogenizing dispersion on the crude product water suspending agent by using a high-speed shearing emulsifying machine with the rotating speed of 8000rpm, and stirring for 30min to obtain the finished product indoxacarb water suspending agent.
Performance test method field efficacy test: the test is carried out by referring to the test method in GB/T17980.13-2000 pesticide field efficacy test criterion. Cabbage is used as a test crop, the test medicament is indoxacarb water suspending agent which is prepared in the same batch in examples 1-23 and comparative examples 1-5 and has consistent storage environment, the medicament used for blank control is clear water, the application amount is 15 ml/mu, and the water consumption is 30 kg/mu.
The method comprises the steps of applying the pesticide once in the peak period of 2-3 instar larvae of plutella xylostella, repeating the pesticide three times, surveying and recording the number of live insects before the pesticide is applied, after the pesticide is applied for 3d, after the pesticide is applied for 7d and after the pesticide is applied for 14d, and calculating the control effect; and a five-point sampling method is adopted in the mode of investigation and recording. The formula of the control effect calculation is as follows:
control (%) = (1- (number of live insects before the drug treatment in the blank area×number of live insects after the drug treatment in the drug treatment area)/(number of live insects after the drug treatment in the blank area×number of live insects before the drug treatment area)) ×100.
Table 3 data sheet of control effect
Detecting the residual amount of the indene micro-original drug: five-point sampling method is adopted to sample cabbage samples before drug application, 3d after drug application, 7d after drug application and 14d after drug application, and the residual quantity of indoxacarb technical in the cabbage samples is determined by high performance liquid chromatography-mass spectrometry.
Table 4 indoxacarb crude drug residual amount detection data sheet
As can be seen from tables 3 and 4 and by combining the test results of examples 1-5 and comparative examples 4-5, the indoxacarb aqueous suspension prepared by the method achieves better control effect and has less residual quantity after 14d application. Meanwhile, from the specific data, the indoxacarb water suspension prepared by the application can basically achieve about 96% of prevention effect after 7d of application, and the residual amount of indoxacarb after 14d of application is about 0.06. The indoxacarb aqueous suspension of comparative examples 4 to 5 can only achieve about 87% of prevention effect after 7d of application, namely the original drug effect of indoxacarb is poor in durability, and the residual amount of indoxacarb after 14d of application is also large.
From the test results of the embodiment 1 and the embodiment 19, the formation of the salicylate protective layer on the surface of the sustained-release indoxacarb microsphere has positive significance for improving the control effect. In addition, from the residual quantity after 3d of application, the salicylate protective layer is favorable for reducing the original drug loss of indoxacarb in the storage stage and the initial stage of application of the aqueous suspension agent, and the residual quantity of indoxacarb cannot be too high in the later stage of application of the aqueous suspension agent, so that the salicylate protective layer starts to be gradually decomposed in the middle stage before application of the aqueous suspension agent, namely, the slow release process of the slow release indoxacarb microsphere and the process of promoting photodegradation in the later stage are relatively compatible.
The test results of the combination of the example 1 and the comparative examples 1 to 3 show that the humic acid can play a good role in inhibiting photodegradation in the storage stage and the early stage of application of the water suspending agent, and the photodegradation promoting effect of ferric chloride is obvious under the condition of no humic acid, so that the loss of the indoxacarb water suspending agent in the storage stage and the early stage of application is large. On the premise of not coating ferric chloride with sodium alginate in advance, the ferric chloride in the slow-release indoxacarb microspheres can be contacted with indoxacarb original drug and humic acid in advance; ferric chloride and humic acid which are contacted and interacted in advance simultaneously, and the generated humic acid-Fe 3+ On the contrary, the effect of promoting the photodegradation of the indoxacarb original drug is more obvious, namely, the loss of the indoxacarb original drug in the storage stage and the drug administration initial stage is larger, and the prevention and treatment effect is obviously affected.
Meanwhile, on the premise of adding the modified ferric chloride, the photodegradation inhibition effect of humic acid on the indoxacarb original drug is always present, the negative influence on the control effect is small, but excessive indoxacarb residue in the later stage can influence the edible safety, and the problem of certain environmental pollution exists.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.

Claims (9)

1. The indoxacarb water suspending agent is characterized by comprising the following raw materials in percentage by mass: 15-25% of slow-release indoxacarb microspheres, 1-5% of dispersing agent, 1-5% of suspending aid, 1-5% of wetting agent, 0.1-5% of other auxiliary agents and the balance of water;
the raw materials of the sustained-release indoxacarb microsphere comprise the following components in parts by mass: 10 to 20 parts of indoxacarb technical material, 0.2 to 1 part of humic acid, 0.5 to 1.5 parts of modified ferric chloride and 30 to 50 parts of sodium alginate; the modified ferric chloride is obtained by pre-coating ferric chloride with sodium alginate;
the preparation method of the sustained-release indoxacarb microsphere comprises the following steps:
preparing sodium alginate solution: dissolving sodium alginate in water to prepare sodium alginate solution, and dividing the sodium alginate solution into A, B parts for later use;
preparing modified ferric chloride: adding ferric chloride into the sodium alginate solution A, fully mixing, then dropwise adding a calcium chloride solution for granulating, and sequentially washing and filtering to obtain modified ferric chloride for later use after low-temperature treatment;
microsphere preparation: adding humic acid and indoxacarb raw material into the sodium alginate solution of the part B, adding modified ferric chloride, fully mixing, then dripping calcium chloride solution for granulating, and washing and filtering to obtain the slow-release indoxacarb microsphere after low-temperature treatment.
2. The indoxacarb aqueous suspension according to claim 1, wherein in the sodium alginate solution preparation step, the pH of the sodium alginate solution is adjusted to 4-5.
3. The indoxacarb aqueous suspension according to claim 1, wherein in the sodium alginate solution preparation step, the mass concentration of the prepared sodium alginate solution is 2% -3%.
4. The indoxacarb aqueous suspension according to claim 3, wherein the mass concentration of the calcium chloride solution in the modified ferric chloride preparation step and the microsphere preparation step is 1% -2%.
5. The indoxacarb aqueous suspension according to claim 1, wherein in the microsphere preparation step, crude indoxacarb microspheres are obtained after the drying treatment, the crude indoxacarb microspheres are added into salicylate, and the drying treatment is carried out after the complete mixing, so as to obtain the finished product indoxacarb microspheres.
6. The indoxacarb aqueous suspension of claim 5, wherein the particle size of the finished sustained-release indoxacarb microsphere is 2-3 mm.
7. The indoxacarb water suspension agent according to claim 1, wherein the suspending aid is diammonium phosphate and ammonium nitrate according to a mass ratio of 1: (2.5-4.2).
8. A process for the preparation of an indoxacarb aqueous suspension according to any one of claims 1 to 7, characterized in that it comprises the following steps: fully mixing the raw materials of the indoxacarb water suspending agent to obtain a mixed solution; and sequentially carrying out wet sanding and shearing dispersion treatment on the mixed solution to obtain the finished indoxacarb aqueous suspension.
9. The preparation method of the indoxacarb aqueous suspension agent according to claim 8, wherein the prepared indoxacarb aqueous suspension agent is stored in a dark place.
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CN107333759A (en) * 2017-06-22 2017-11-10 浙江大学 Light-operated sustained-release pesticides preparation and preparation method thereof
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CN107333759A (en) * 2017-06-22 2017-11-10 浙江大学 Light-operated sustained-release pesticides preparation and preparation method thereof
CN110771619A (en) * 2019-11-26 2020-02-11 深圳市威必达有害生物防治有限公司 Medicament for killing solenopsis invicta and preparation method thereof

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