CN113812416A - Double-release preparation containing thiacloprid and preparation method thereof - Google Patents

Double-release preparation containing thiacloprid and preparation method thereof Download PDF

Info

Publication number
CN113812416A
CN113812416A CN202110886815.4A CN202110886815A CN113812416A CN 113812416 A CN113812416 A CN 113812416A CN 202110886815 A CN202110886815 A CN 202110886815A CN 113812416 A CN113812416 A CN 113812416A
Authority
CN
China
Prior art keywords
thiacloprid
release preparation
suspending agent
zein
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110886815.4A
Other languages
Chinese (zh)
Inventor
邹汶廷
谭葵
王爱臣
廖联安
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Huizhou Yinnong Technology Co ltd
Original Assignee
Huizhou Yinnong Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Huizhou Yinnong Technology Co ltd filed Critical Huizhou Yinnong Technology Co ltd
Priority to CN202110886815.4A priority Critical patent/CN113812416A/en
Publication of CN113812416A publication Critical patent/CN113812416A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, 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
    • A01N47/40Biocides, 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 a double or triple bond to nitrogen, e.g. cyanates, cyanamides
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/26Biocides, 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
    • A01N25/28Microcapsules or nanocapsules

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Medicinal Preparation (AREA)

Abstract

The application provides a double-release preparation containing thiacloprid and a preparation method thereof. The double-release preparation containing thiacloprid comprises a suspending agent containing thiacloprid and a microcapsule suspending agent containing thiacloprid which are mixed and dissolved. The double-release preparation containing thiacloprid not only can quickly release the effective components to achieve the effect of effectively preventing and treating concentration, but also can prolong the effective component duration.

Description

Double-release preparation containing thiacloprid and preparation method thereof
Technical Field
The invention relates to the technical field of pesticide preparations, in particular to a thiacloprid-containing double-release preparation and a preparation method thereof.
Background
The pesticide is an important material basis for defending against major biological disasters and promoting the sustainable and stable growth of agricultural products, wherein the nano pesticide preparation is beneficial to controlling the release rate of active ingredients, prolonging the lasting period, reducing the dosage in non-target areas and environments and reducing residual pollution, thereby improving new power for sustainable agricultural development, but the nano pesticide preparation can reach effective control concentration only after being used for a period of time, so that control delay is easily caused when the nano pesticide preparation is used for controlling acute plant diseases and insect pests, irrecoverable crop loss is caused, if the pesticide preparation capable of being quickly released is changed, the effect of lasting pesticide effect cannot be reached, and the pesticide preparation needs to be frequently sprayed on crops for many times, thereby wasting manpower and easily causing the problem of serious pesticide preparation residue.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a thiacloprid-containing double-release preparation which not only can quickly release effective components to achieve the effect of effectively preventing and treating concentration, but also can prolong the effective component duration and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
a dual-release preparation containing thiacloprid comprises a suspending agent containing thiacloprid and a microcapsule suspending agent containing thiacloprid which are mixed and dissolved.
In one embodiment, the mass ratio of the thiacloprid-containing suspending agent to the thiacloprid-containing microcapsule suspending agent is 0.8-2.
In one embodiment, the thiacloprid-containing dual release formulation comprises the following components:
thiacloprid, solvent, modified material, zein, wetting dispersant and water.
In one embodiment, the thiacloprid-containing dual-release preparation comprises the following components in parts by mass:
Figure BDA0003194455700000021
in one embodiment, the solvent is at least one of an alcohol solvent, a ketone solvent, an amide solvent, an aromatic solvent, and an environmentally friendly solvent.
In one embodiment, the modifying material is a phosphate compound.
In one embodiment, the modifying material is at least one of potassium tripolyphosphate, sodium tripolyphosphate, and phosphorus oxychloride.
In one embodiment, the wetting dispersant is at least one of a polycarboxylate dispersant, a gemini-like dispersant, a phosphate-based dispersant, a block polyether dispersant, a carboxylate-based dispersant, and a non-ionic hydroxypolyethylene oxide block copolymer dispersant.
A method for preparing a thiacloprid-containing dual-release preparation, which is used for preparing the thiacloprid-containing dual-release preparation described in any one of the above embodiments, and the method for preparing the thiacloprid-containing dual-release preparation comprises the following steps:
preparing a solvent and part of water to obtain a binary solution;
placing zein, a phosphate compound and part of thiacloprid in the binary solution for dissolving treatment;
placing 80-90% of the rest water in the binary solution after dissolving treatment for nanocrystallization treatment to obtain a thiacloprid-containing microcapsule suspending agent;
grinding the rest water, the wetting dispersant and the rest thiacloprid to obtain grinding fluid;
and adding the grinding liquid into the thiacloprid-containing microcapsule suspending agent for mixing operation to obtain the thiacloprid-containing double-release preparation.
In one embodiment, zein, a phosphate compound and 2% -10% thiacloprid are placed in a binary solution for dissolution treatment.
Compared with the prior art, the invention has at least the following advantages:
in the double-release preparation containing thiacloprid, the miscible thiacloprid-containing suspending agent and thiacloprid-containing microcapsule suspending agent have better slow-release capability and the capability of quickly releasing thiacloprid to effective control concentration, thereby effectively prolonging the pesticide effect duration of thiacloprid, improving the problems of easy control delay and irreparable crop loss during the control of acute insect pests, reducing the frequent degree of spraying pesticide preparations on crops and further reducing the control cost of the crops.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a reaction formula of the present invention using a phosphoric acid compound to modify zein;
fig. 2 is a flowchart of a method for preparing a thiacloprid-containing dual release formulation according to one embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The application provides a thiacloprid-containing dual-release preparation which comprises a suspending agent containing thiacloprid and a microcapsule suspending agent containing thiacloprid which are mixed and dissolved.
According to the double-release preparation containing thiacloprid, the miscible thiacloprid-containing suspending agent and the thiacloprid-containing microcapsule suspending agent have good slow release capability and the capability of quickly releasing thiacloprid to effective control concentration, so that the pesticide effect duration of thiacloprid is effectively prolonged, the problems that the control delay is easily caused during the control of acute insect pests and irretrievable crop loss is caused are solved, the frequency of spraying and drying the pesticide preparation on crops is reduced, and the control cost of the crops is further reduced.
It should be noted that the mixing and dissolving means that several substances are mixed together and can be fused with each other, and the substances are compatible with each other, namely, the substances in the thiacloprid-containing dual release preparation are compatible with each other.
It should be noted that, because the content of water in the thiacloprid-containing suspending agent is relatively high, if the thiacloprid-containing suspending agent and the thiacloprid-containing microcapsule suspending agent are directly mixed, the water in the thiacloprid-containing suspending agent can cause the thiacloprid dissolved in the thiacloprid-containing microcapsule suspending agent to be separated out, namely, the thiacloprid crystal is separated out, the stability of the micro-capsule suspending agent containing the thiacloprid is damaged, therefore, the suspending agent containing the thiacloprid and the micro-capsule suspending agent containing the thiacloprid are difficult to be mixed and dissolved, if the suspending agent and the micro-capsule suspending agent are mixed and used forcibly, the suspension rate of the double-release preparation containing the thiacloprid is reduced, and the pesticide effect of the thiacloprid is further reduced, and the application provides a miscible thiacloprid-containing suspending agent and thiacloprid-containing microcapsule suspending agent, so that the pesticide effect durability and the quick release capacity of the thiacloprid-containing double-release preparation are ensured, and the pesticide effect and the stability of the thiacloprid-containing double-release preparation are ensured.
It can also be understood that if the suspending agent containing thiacloprid and the microcapsule suspending agent containing thiacloprid are sprayed on crops separately, the effect of lasting pesticide effect and quick release are achieved, but the spraying time of a user is prolonged, the labor time of the user is increased, and the cost of crop control is further improved.
In one embodiment, the mass ratio of the thiacloprid-containing suspending agent to the thiacloprid-containing microcapsule suspending agent is 0.8-2. It can be understood that if the content of the thiacloprid-containing suspending agent is too high, the concentration of the quickly released thiacloprid is too high, which causes waste of the thiacloprid suspending agent; if the content of the thiacloprid-containing microcapsule suspending agent is too high, a dispersant with a larger content needs to be added to maintain the stability of the thiacloprid-containing suspending agent, so that the concentration of the dispersant is lower than the critical concentration of the micelle, and a stable dispersion system cannot be formed, thereby causing the problem of reduction of the drug effect of the thiacloprid-containing suspending agent.
In one embodiment, the thiacloprid-containing dual release formulation comprises the following components: thiacloprid, solvent, modified material, zein, wetting dispersant and water. It can be understood that the phosphoric acid compound is adopted to carry out hydrophilic modification on the zein, the usage amount of an organic solvent is reduced, the influence of a double-release preparation containing thiacloprid on the environment is further reduced, the hydrophilicity and the electronegativity of the zein are improved, and further when the thiacloprid is coated by the modified zein, the stability and the biocompatibility of the thiacloprid are improved, so that the thiacloprid has stable bioactivity, crops have better systemic property on the thiacloprid and better conductivity of the thiacloprid in the crops, and further the drug effect and the utilization rate of the thiacloprid are improved. It can be understood that the thiacloprid is dispersed by adopting the wetting dispersant, so that the dispersion stability of the thiacloprid is effectively ensured, and the stability of the thiacloprid-containing dual-release preparation is further improved. In one embodiment, the thiacloprid-containing dual release formulation further comprises the following components: synergist, antifreezing agent, thickener and preservative. It can be understood that the synergist mainly inhibits or weakens targets, such as the detoxification and phytotoxicity prevention effects of pests, weeds, germs and the like on the activity of the thiacloprid, and delays the metabolic rate of the thiacloprid in crops, thereby increasing the biological control effect of the thiacloprid. The synergist has no activity, but when the synergist is mixed with thiacloprid, the wetting, spreading, dispersing, detention and permeability of the thiacloprid can be obviously improved, the double-release preparation containing the thiacloprid can be spread and adhered on the leaf surface, the decomposition of the thiacloprid by ultraviolet rays is reduced, and the aims of prolonging the effective period of the thiacloprid, improving the bioactivity of the thiacloprid, reducing the dosage of the thiacloprid, reducing the control cost of crops and protecting the ecological environment are fulfilled; the antifreezing agent effectively ensures the antifreezing capability of the double-release preparation containing thiacloprid; the thickening agent further improves the system stability of the thiacloprid-containing double-release preparation; the preservative slows down the failure of the thiacloprid-containing double-release preparation, and further improves the drug effect durability of the thiacloprid-containing double-release preparation.
In one embodiment, the thiacloprid-containing dual-release preparation comprises the following components in parts by mass: 20.5 to 30 portions of thiacloprid; 10-15 parts of a solvent; 1-5 parts of modified material; 1-5 parts of zein; 2-4 parts of wetting dispersant; 38 to 58 portions of water. It can be understood that 1 to 5 parts of the modified material is matched with 1 to 5 parts of the zein, so that the stability and the biocompatibility of the micro-capsule suspending agent containing thiacloprid are effectively ensured, the thiacloprid has stable bioactivity, crops have better systemic property on the thiacloprid and better conductivity of the thiacloprid in the crops, and the drug effect and the utilization rate of the double-release preparation containing the thiacloprid are further improved; 2-4 parts of wetting dispersant effectively ensures the stability of the suspending agent containing thiacloprid, and further improves the drug effect and the utilization rate of the double-release preparation containing thiacloprid.
In one embodiment, the thiacloprid-containing dual-release preparation comprises the following components in parts by mass: 20.5 to 25 portions of thiacloprid; 10-15 parts of a solvent; 1-5 parts of modified material; 1-5 parts of zein; 2-4 parts of wetting dispersant; 38 to 58 portions of water. It can be understood that 1 to 5 parts of the modified material is matched with 1 to 5 parts of the zein, so that the stability and the biocompatibility of the micro-capsule suspending agent containing thiacloprid are effectively ensured, the thiacloprid has stable bioactivity, crops have better systemic property on the thiacloprid and better conductivity of the thiacloprid in the crops, and the drug effect and the utilization rate of the double-release preparation containing the thiacloprid are further improved; 2-4 parts of wetting dispersant effectively ensures the stability of the suspending agent containing thiacloprid, and further improves the drug effect and the utilization rate of the double-release preparation containing thiacloprid.
In one embodiment, the thiacloprid-containing dual-release preparation further comprises the following components in parts by mass: 2-4 parts of a synergist; 3-6 parts of an antifreezing agent; 0.2-1.5 parts of a thickening agent; 0.5-1 part of preservative. It can be understood that 2-4 parts of synergist, 3-6 parts of antifreezing agent, 0.2-1.5 parts of thickener, 0.5-1 part of preservative and other components of the thiacloprid-containing double-release preparation are matched, so that the drug effect and stability of the thiacloprid-containing double-release preparation are effectively ensured.
In one embodiment, the solvent is at least one of an alcohol solvent, a ketone solvent, an amide solvent, an aromatic solvent, and an environmentally friendly solvent. It can be understood that the solubility of the zein in the aqueous solution of the alcohol solvent, the ketone solvent, the amide solvent, the aromatic solvent and the environment-friendly solvent is good, the encapsulation rate of the zein on the thiacloprid is effectively improved, the content of the thiacloprid-containing double-release preparation is further improved, the usage amount of the organic solvent is reduced, and the influence of the thiacloprid-containing double-release preparation on the environment is further reduced.
In one embodiment, the alcoholic solvent is at least one of ethanol, isopropanol, ethylene glycol, and n-butanol. It can be understood that the solubility of the zein in the aqueous solution of alcohol solvents of ethanol, isopropanol, ethylene glycol and n-butanol is high, and the solubility of the thiacloprid in the mixture of the aqueous solution of alcohol solvents of ethanol, isopropanol, ethylene glycol and n-butanol is high, so that the solubility of the zein and the solubility of the thiacloprid are effectively ensured.
In one embodiment, the ketone solvent is acetone and/or cyclohexanone. It can be understood that the solubility of the zein in the aqueous solution of the ketone solvents acetone and cyclohexanone is high, and the solubility of the thiacloprid in the mixture of the ketone solvents acetone and cyclohexanone is high, so that the solubility of the zein and the solubility of the thiacloprid are effectively ensured.
In one embodiment, the amide solvent is dimethylformamide. It can be understood that the solubility of the zein in the aqueous solution of the amide solvent dimethylformamide is high, and the solubility of the thiacloprid in the mixture of the amide solvent dimethylformamide and the aqueous solution of the amide solvent dimethylformamide is high, so that the solubility of the zein and the solubility of the thiacloprid are effectively ensured.
In one embodiment, the aromatic hydrocarbon solvent is at least one of benzene, toluene, and xylene. It can be understood that the solubility of the zein in the water solution of aromatic solvents of benzene, toluene and xylene is higher, and the solubility of the thiacloprid in the mixture of the aromatic solvents of benzene, toluene and xylene is higher, so that the solubility of the zein and the solubility of the thiacloprid are effectively ensured.
In one embodiment, the environmentally friendly solvent is at least one of SV-92, GREEN 21, and FMPC. In addition, the SV-92 molecule composition comprises ether bonds and hydroxyl groups, has good solubility for both zein and thiacloprid, and effectively ensures the solubility of the zein and the solubility of the thiacloprid. The GREEN 21 is a mixture of an amide dispersant and an amide ester dispersant, the molecular composition of the GREEN 21 comprises amide and ester, the amide and ester are non-toxic and harmless to plants and soil, the influence of a thiacloprid-containing double-release preparation on the environment is reduced, in addition, the zein and the thiacloprid both have good solubility, and the solubility of the zein and the solubility of the thiacloprid are effectively ensured. FMPC is a mixture of morpholine derivatives and carbonic acid ester, is non-toxic and harmless to plants and soil, reduces the influence of a double-release preparation containing thiacloprid on the environment, has good miscibility with water, has good solubility for both zein and thiacloprid, and effectively ensures the solubility of the zein and the solubility of the thiacloprid.
In one embodiment, the solvent is a mixed solvent of SV-92 and GREEN 21, so that the solubility of the zein is better improved, the solubility of the thiacloprid is better improved, the use amount of an organic solvent is reduced, and the encapsulation rate of the zein on the thiacloprid and the content of the thiacloprid are ensured.
In one embodiment, the mass ratio of SV-92 to GREEN 21 is 3-7. It is understood that SV-92: the GREEN 21 is 3-7, so that the use amount of an organic solvent is further reduced, and the encapsulation rate of the zein to the thiacloprid and the content of the thiacloprid are ensured. In one embodiment, the modifying material is a phosphate compound. It can be understood that the zein contains about 225 amino acid residues, wherein more than 50% of the zein contains hydrophobic amino acid residues, and specifically contains leucine, proline and alanine with higher content, so that the zein has stronger hydrophobicity, and therefore, if the zein is directly used for preparing the thiacloprid-containing dual-release preparation, the zein is easy to agglomerate and is difficult to uniformly coat the periphery of the thiacloprid, and further the effect of improving the utilization rate and the drug effect of the thiacloprid is better achieved, therefore, in order to improve the hydrophilicity and the electronegativity of the zein, the zein is subjected to hydrophilic modification by using the phosphate compound, and as the phosphate compound is an inorganic compound, the use of an organic solvent in the thiacloprid-containing dual-release preparation is reduced, and the influence of the thiacloprid-containing dual-release preparation on the environment is reduced, in addition, the phosphoric acid compound is easier to dissolve in water, phosphate radicals in water form electronegativity, and has positive and negative charge attraction with electropositive groups formed by zein dissolved in a solvent and water, so that the combination of zein and the phosphoric acid compound is effectively improved, the hydrophilic modification of the zein is facilitated, and after the zein is modified by adopting the phosphoric acid compound, the zein contains the phosphate radicals, so that the property of the zein is closer to the property of a cell membrane, the biocompatibility of the zein is further improved, and the double-release preparation containing the thiacloprid, which is prepared by coating the thiacloprid by adopting the zein modified by the phosphoric acid compound, has better biocompatibility and higher stability, the thiacloprid has stable biological activity, the crops have better systemic property to the thiacloprid and better conductive capability to the thiacloprid in the crops, and the pesticide effect and the utilization rate of the thiacloprid are effectively improved.
It should be noted that, referring to fig. 1, in the reaction formula of modifying zein with a phosphate compound, since the phosphate compound has a smaller molecular weight, when the phosphate compound is used to modify zein in a hydrophilic manner, the binding resistance between the phosphate compound and the zein is smaller, which is beneficial to the binding between the zein and the phosphate compound, and improves the binding rate between the phosphate compound and the zein, thereby effectively improving the hydrophilicity of the zein, so that when thiacloprid is coated with zein by high zein content, the encapsulation rate of thiacloprid by the zein is higher, and the prepared thiacloprid-containing double release preparation has a smaller particle size, and the thiacloprid-containing double release preparation is more stable.
In one embodiment, the modifying material is at least one of potassium tripolyphosphate, sodium tripolyphosphate, and phosphorus oxychloride. It can be understood that potassium tripolyphosphate, sodium tripolyphosphate and phosphorus oxychloride are all easily soluble in water, and can form electronegative phosphate radicals after being dissolved in water, and have positive and negative charge attraction with electropositive groups formed by zein dissolved in a solvent and water, so that the combination of zein and a phosphoric acid compound is effectively improved, the hydrophilic modification of zein is facilitated, and after the zein is modified by adopting a phosphoric acid compound, the zein contains phosphate radicals, so that the property of the zein is closer to that of a cell membrane, the biocompatibility of the zein is further improved, and the biocompatibility of a thiacloprid-containing double-release preparation is further improved.
In one embodiment, the phosphoric acid based compound is potassium tripolyphosphate. It can be understood that potassium tripolyphosphate forms potassium ions and phosphate ions after being dissolved in water, wherein phosphate is used for modifying zein, potassium ions are absorbed and utilized by plants to facilitate the growth of the potassium tripolyphosphate, the deposition of chemical substances in soil is reduced, and the thiacloprid-containing double-release preparation has a growth promoting effect on the plants.
In one embodiment, the wetting dispersant is at least one of a polycarboxylate dispersant, a gemini-like dispersant, a phosphate-based dispersant, a block polyether dispersant, a carboxylate-based dispersant, and a non-ionic hydroxy polyethylene oxide block copolymer dispersant. It can be understood that the polycarboxylate dispersant, the gemini dispersant, the phosphate dispersant, the block polyether dispersant, the carboxylate dispersant and the non-ionic hydroxy polyethylene oxide block copolymer dispersant all have a good compatibilization effect on thiacloprid, can form a stable thiacloprid micelle with thiacloprid, effectively improves the dispersion stability of thiacloprid, further reduces the polymerization of thiacloprid, is beneficial to maintaining the particle size of thiacloprid, and further is beneficial to the absorption and utilization of thiacloprid.
In one embodiment, the gemini-like dispersant comprises sp-sc3, and the main component of sp-sc3 is a polyether modifier.
In one embodiment, the phosphate-based dispersant comprises PEAS 03. The main component of PEAS03 is pentaerythritol diacrylate monostearate.
In one embodiment, the polycarboxylate type dispersant comprises 14105 and/or SP-3645. 14105 a polycarboxylate as the main component; the main component of SP-3645 is polycarboxylate.
In one embodiment, the block polyether dispersant comprises 601 and/or 1601. 601 mainly contains phenol derivative polyoxyethylene/polyoxypropylene ether; 1601 has a main component of phenol derivative polyoxyethylene/polyoxypropylene ether.
In one embodiment, the water is tap or deionized water.
In one embodiment, the water is distilled water.
In one embodiment, the antifreeze agent is at least one of ethylene glycol, propylene glycol, glycerin, and urea. It will be appreciated that ethylene glycol, propylene glycol, glycerol and urea all provide better protection against freezing for the thiacloprid-containing dual release formulation.
In one embodiment, the thickener is at least one of xanthan gum, magnesium aluminum silicate, and attapulgite. It can be understood that the xanthan gum, the magnesium aluminum silicate and the attapulgite all have a good thickening effect on the thiacloprid, and are beneficial to improving the system stability of the double-release preparation containing the thiacloprid.
In one embodiment, the thickening agent comprises xanthan gum and magnesium aluminum silicate. It will be appreciated that the use of a combination of xanthan gum and magnesium aluminum silicate better ensures the system stability of the thiacloprid-containing dual release formulation.
In one embodiment, the thickening agent comprises xanthan gum, magnesium aluminum silicate, and attapulgite. It is understood that the combination of xanthan gum, magnesium aluminum silicate and attapulgite better ensures the system stability of the thiacloprid-containing dual release formulation.
In one embodiment, the mass ratio of the xanthan gum to the magnesium aluminum silicate is 0.8-1.2. It can be understood that when the mass ratio of the xanthan gum to the magnesium aluminum silicate is 0.8-1.2, the system stability of the thiacloprid-containing double-release preparation is better ensured.
In one embodiment, the preservative is cason and/or sodium benzoate. It can be understood that the cason and the sodium benzoate effectively slow down the failure of the thiacloprid-containing dual release preparation, thereby improving the drug effect durability of the thiacloprid-containing dual release preparation.
In one embodiment, the synergist is at least one of BQ-809F, T1118, SK-44 and FS-608A. It is understood that the main components of BQ-809F, T1118, SK-44 and FS-608A are all organic silicon polyoxyethylene ether compounds. BQ-809F, T1118, SK-44 and FS-608A can better delay the metabolism speed of thiacloprid in crops, thereby increasing the biological control effect of thiacloprid. The synergist has no activity, but when the synergist is mixed with thiacloprid, the wetting, spreading, dispersing, detention and permeability of the thiacloprid can be obviously improved, the double-release preparation containing the thiacloprid can be spread and adhered on the leaf surface, the decomposition of the thiacloprid by ultraviolet rays is reduced, and the aims of prolonging the effective period of the thiacloprid, improving the biological activity of the thiacloprid, reducing the using amount of the thiacloprid, reducing the control cost of crops and protecting the ecological environment are fulfilled.
The application also provides a preparation method of the thiacloprid-containing dual-release preparation, which is used for preparing the thiacloprid-containing dual-release preparation of any one of the embodiments. The preparation method of the thiacloprid-containing dual-release preparation comprises the following steps: preparing a solvent and part of water to obtain a binary solution; placing zein, a phosphate compound and part of thiacloprid in a binary solution for dissolving; putting 80-90% of the rest water into the binary solution after dissolution treatment for nanocrystallization treatment to obtain a thiacloprid-containing microcapsule suspending agent; grinding the rest water, the wetting dispersant and the rest thiacloprid to obtain grinding fluid; and adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing operation to obtain the double-release preparation containing thiacloprid.
According to the preparation method of the thiacloprid-containing dual-release preparation, the zein, the phosphoric acid compound and the thiacloprid are all placed in the binary solution for dissolving and modifying, so that the using amount of the nonzero organic solvent is reduced, the preparation efficiency of the thiacloprid-containing dual-release preparation is improved, and the preparation cost of the thiacloprid-containing dual-release preparation is reduced; when water with the content of 80-90 percent of the rest water is put into the binary solution after the dissolution treatment for the nanocrystallization treatment, almost most of the water is put into the micro-capsule suspending agent containing thiacloprid, the suspending agent comprises most of water used for the suspending agent containing thiacloprid, effectively ensures that the solubility of the thiacloprid in the mixed solution of the water and the solvent of the microcapsule suspending agent containing thiacloprid is low, when the grinding liquid is added into the micro-capsule suspending agent containing thiacloprid for mixing operation, the solubility change of the thiacloprid is small, the precipitation of the thiacloprid in the double-release preparation containing the thiacloprid is reduced, and the mixing and dissolving of the thiacloprid-containing suspending agent and the thiacloprid-containing microcapsule suspending agent are realized, the drug effect durability and the quick release capacity of the thiacloprid-containing double-release preparation are ensured, and the drug effect and the stability of the thiacloprid-containing double-release preparation are ensured.
In order to better understand the preparation method of the thiacloprid-containing dual release preparation of the present application, the following further explains the preparation method of the thiacloprid-containing dual release preparation of the present application, and referring to fig. 1, the preparation method of the thiacloprid-containing dual release preparation of one embodiment comprises the following steps:
s100, preparing the solvent and part of water to obtain a binary solution. It can be understood that zein contains about 225 amino acid residues, wherein more than 50% of zein is hydrophobic amino acid residues, specifically including leucine, proline and alanine with higher content, so zein has stronger hydrophobicity and weaker hydrophilicity, and in order to dissolve zein, a solvent and water need to be mixed, so that the solubility of zein is ensured.
S200, placing the zein, the phosphoric acid compound and part of thiacloprid in a binary solution for dissolving treatment. It can be understood that after the zein is dissolved, the phosphoric acid compound is added into the binary solution, which is beneficial to the modification of the zein, in addition, the zein, the phosphoric acid compound and the thiacloprid are all placed into the binary solution for dissolution and modification, thereby avoiding the complicated preparation method of the thiacloprid-containing double-release preparation caused by the dissolution of the zein and the phosphoric acid compound by organic solvent and the dissolution of the thiacloprid by organic solvent, thereby increasing the preparation difficulty of the thiacloprid-containing dual-release preparation, reducing the preparation efficiency of the thiacloprid-containing dual-release preparation, increasing the usage amount of the organic solvent, further increasing the influence of the thiacloprid-containing double-release preparation on the environment, improving the preparation efficiency of the thiacloprid-containing double-release preparation and reducing the preparation cost of the thiacloprid-containing double-release preparation.
S300, putting 80-90% of water with the content of the rest water into the binary solution after the dissolution treatment for nanocrystallization treatment to obtain the thiacloprid-containing microcapsule suspending agent. The modified zein and the thiacloprid can be uniformly dissolved in the binary solution, so that the modified zein is difficult to coat the periphery of the thiacloprid, water is added into the binary solution to reduce the solubility of the thiacloprid in the binary solution, the modified zein is coated on the periphery of the thiacloprid, and the preparation of the microcapsule suspending agent containing the thiacloprid is effectively realized. It can be understood that when the water with the content of 80 to 90 percent of the rest water is put into the binary solution after the dissolution treatment for the nanocrystallization treatment, most of the water is almost put into the micro-capsule suspending agent containing thiacloprid, the suspending agent comprises most of water used for the suspending agent containing thiacloprid, effectively ensures that the solubility of the thiacloprid in the mixed solution of the water and the solvent of the microcapsule suspending agent containing thiacloprid is low, further, after the remaining small part of the water used for the suspending agent containing thiacloprid is further added, the solubility change of the thiacloprid is small, the precipitation of the thiacloprid in the double-release preparation containing thiacloprid is reduced, and the mixing and dissolving of the thiacloprid-containing suspending agent and the thiacloprid-containing microcapsule suspending agent are realized, the drug effect durability and the quick release capacity of the thiacloprid-containing double-release preparation are ensured, and the drug effect and the stability of the thiacloprid-containing double-release preparation are ensured.
S400, grinding the residual water, the wetting dispersant and the residual thiacloprid to obtain the grinding fluid. The grinding also plays a role in mixing the added substances, and is beneficial to increasing the mixing uniformity and the dispersion stability of the added substances, so that the wetting dispersant and the residual thiacloprid are ground together, the mixing uniformity is greatly higher than that of the stirring and mixing in the later period, and the uniformity and the stability of the thiacloprid-containing double-release preparation are effectively improved; in addition, the wetting dispersant further improves the wettability of thiacloprid in water, better ensures the dispersion uniformity of the thermosensitive original drug in water, is favorable for fully grinding the thiacloprid, has larger specific heat capacity, is favorable for reducing the grinding temperature of the thiacloprid, and reduces the qualitative change or agglomeration of the thiacloprid caused by the large-degree increase of the temperature due to long-time grinding.
And S500, adding the grinding liquid into a thiacloprid-containing microcapsule suspending agent for mixing operation to obtain a thiacloprid-containing double-release preparation. It can be understood that when the water with the content of 80 to 90 percent of the rest water is put into the binary solution after the dissolution treatment for the nanocrystallization treatment, most of the water is almost put into the micro-capsule suspending agent containing thiacloprid, the suspending agent comprises most of water used for the suspending agent containing thiacloprid, effectively ensures that the solubility of the thiacloprid in the mixed solution of the water and the solvent of the microcapsule suspending agent containing thiacloprid is low, when the grinding liquid is added into the micro-capsule suspending agent containing thiacloprid for mixing operation, the solubility change of the thiacloprid is small, the precipitation of the thiacloprid in the double-release preparation containing the thiacloprid is reduced, and the mixing and dissolving of the thiacloprid-containing suspending agent and the thiacloprid-containing microcapsule suspending agent are realized, the drug effect durability and the quick release capacity of the thiacloprid-containing double-release preparation are ensured, and the drug effect and the stability of the thiacloprid-containing double-release preparation are ensured.
According to the preparation method of the thiacloprid-containing dual-release preparation, the zein, the phosphoric acid compound and the thiacloprid are all placed in the binary solution for dissolving and modifying, so that the using amount of the nonzero organic solvent is reduced, the preparation efficiency of the thiacloprid-containing dual-release preparation is improved, and the preparation cost of the thiacloprid-containing dual-release preparation is reduced; when water with the content of 80-90 percent of the rest water is put into the binary solution after the dissolution treatment for the nanocrystallization treatment, almost most of the water is put into the micro-capsule suspending agent containing thiacloprid, the suspending agent comprises most of water used for the suspending agent containing thiacloprid, effectively ensures that the solubility of the thiacloprid in the mixed solution of the water and the solvent of the microcapsule suspending agent containing thiacloprid is low, when the grinding liquid is added into the micro-capsule suspending agent containing thiacloprid for mixing operation, the solubility change of the thiacloprid is small, the precipitation of the thiacloprid in the double-release preparation containing the thiacloprid is reduced, and the mixing and dissolving of the thiacloprid-containing suspending agent and the thiacloprid-containing microcapsule suspending agent are realized, the drug effect durability and the quick release capacity of the thiacloprid-containing double-release preparation are ensured, and the drug effect and the stability of the thiacloprid-containing double-release preparation are ensured.
In one embodiment, the zein, the phosphate compound and part of thiacloprid are placed in a binary solution for dissolution treatment, and the method comprises the following steps:
putting zein and a phosphate compound into a binary solution for first dissolution treatment. The method has the advantages that the zein and the phosphoric acid compounds are placed in the binary solution for first dissolving treatment, so that the full hydrophilic modification of the zein is effectively realized, the coating effect of the zein on thiacloprid is further ensured, and the stability of the thiacloprid-containing microcapsule suspending agent is improved.
Further, the thiacloprid is placed in the binary solution after the first dissolving treatment to be subjected to a second dissolving treatment. It can be understood that the phosphoric acid compound can change the acid-base property of the binary solution, and further influence the decomposition speed of the thiacloprid, so that in order to reduce the decomposition of the thiacloprid, after the zein is fully modified by the phosphoric acid compound and the content is greatly reduced, the thiacloprid is added for dissolution, and the biological activity of the thiacloprid is ensured.
In one embodiment, under the condition that the rotating speed is 200 r/min-250 r/min, the zein, the phosphoric acid compound and part of thiacloprid are placed in a binary solution for dissolving treatment, so that the sufficiency of hydrophilic modification of the zein is ensured, and the mixing uniformity of the zein and the thiacloprid is ensured.
In one embodiment, the zein and the phosphate compound are placed in the binary solution for the first dissolving treatment, and the dissolving time is more than 3 hours, so that the sufficiency of hydrophilic modification of the zein is ensured.
In one embodiment, the dissolving time of the thiacloprid in the binary solution after the first dissolving treatment for the second dissolving treatment is more than 30min, so that the mixing uniformity of the zein and the thiacloprid is ensured.
In one embodiment, under the condition that the temperature is 25-35 ℃, the zein, the phosphate compound and part of thiacloprid are placed in a binary solution for dissolving treatment, so that the hydrophilicity modification sufficiency of the zein is ensured, and the mixing uniformity of the zein and the thiacloprid is ensured.
In one embodiment, the zein, the phosphate compound and 5% -16% of thiacloprid are dissolved in a binary solution, so that the content of the effective components of the microcapsule suspending agent containing thiacloprid is ensured, and the drug effect of the double-release preparation containing thiacloprid in the slow release process is further ensured.
In one embodiment, the zein, the phosphate compound and 2% -10% of thiacloprid are placed in a binary solution for dissolving treatment, so that the content of the effective components of the microcapsule suspending agent containing thiacloprid is ensured, and the drug effect of the double-release preparation containing thiacloprid in the slow release process is further ensured.
In one embodiment, the remaining water, wetting dispersant and remaining thiacloprid are subjected to a milling operation comprising the steps of:
and mixing the residual water, the wetting dispersant and the residual thiacloprid to dissolve the thiacloprid in the water. It can be understood that the residual water, the wetting dispersant and the residual thiacloprid are mixed, so that the wetting dispersant and the thiacloprid are uniformly mixed, the wetting dispersant is ensured to be dispersed at the periphery of the thiacloprid, the thiacloprid has better wettability and dispersibility during grinding, the qualitative change or agglomeration of the thiacloprid is reduced, and the drug effect of the thiacloprid-containing double-release preparation is improved.
And grinding the mixed water, the wetting dispersant and the thiacloprid. The wetting dispersant and the residual thiacloprid are ground together, so that the mixing uniformity is greatly higher than that of the stirring and mixing in the later period, and the uniformity and the stability of the thiacloprid-containing double-release preparation are effectively improved; in addition, the wetting dispersant further improves the wettability of thiacloprid in water, better ensures the dispersion uniformity of the thermosensitive original drug in water, is favorable for fully grinding the thiacloprid, has larger specific heat capacity, is favorable for reducing the grinding temperature of the thiacloprid, and reduces the qualitative change or agglomeration of the thiacloprid caused by the large-degree increase of the temperature due to long-time grinding.
In one embodiment, the mixing time for mixing the residual water, the wetting and dispersing agent and the residual thiacloprid is 20-30 min, so that the residual water, the wetting and dispersing agent and the thiacloprid are fully mixed.
In one embodiment, the mixed water, the wetting dispersant and the thiacloprid are ground until the D98 of the particles of the grinding fluid is less than or equal to 4 μm, so that the drug effect of the thiacloprid-containing dual-release preparation is ensured.
In one embodiment, the water, the wetting dispersant and the thiacloprid after the mixing treatment are ground by a sand mill, so that the grinding effect of the thiacloprid is ensured.
In one embodiment, after the step of grinding the remaining water, the wetting dispersant and the remaining thiacloprid, and before the step of adding the grinding fluid to the thiacloprid-containing microcapsule suspension for mixing operation, the method for preparing the thiacloprid-containing dual release formulation further comprises the following steps: and grinding and mixing the synergist, the antifreezing agent, the thickening agent, the preservative and the grinding fluid. It can be understood that the grinding also plays a role in mixing the added substances, which is beneficial to increasing the mixing uniformity and dispersion stability of the added substances, so that the grinding, mixing and processing operations are carried out on the synergist, the antifreeze, the thickener, the preservative and the grinding fluid, the mixing uniformity degree is greatly higher than that of the later stirring and mixing, and the uniformity and stability of the thiacloprid-containing double-release preparation are effectively improved.
In one embodiment, the synergist, the antifreeze, the thickener, the preservative and the grinding fluid are subjected to grinding and mixing operation by using a homogenizer, so that the grinding effect of the thiacloprid is ensured, and the synergist, the antifreeze, the thickener, the preservative and the grinding fluid are fully mixed.
In one embodiment, the grinding and mixing time for the grinding and mixing operation of the synergist, the antifreeze, the thickener, the preservative and the grinding fluid is 10-15 min, so that the grinding effect of the thiacloprid is further ensured, and the synergist, the antifreeze, the thickener, the preservative and the grinding fluid are fully mixed.
In one embodiment, the percentage content of the solvent in the binary solution is 50% to 70%, which effectively ensures the solubility of zein and the solubility of thiacloprid.
Compared with the prior art, the invention has at least the following advantages:
in the double-release preparation containing thiacloprid, the miscible thiacloprid-containing suspending agent and thiacloprid-containing microcapsule suspending agent have better slow-release capability and the capability of quickly releasing thiacloprid to effective control concentration, thereby effectively prolonging the pesticide effect duration of thiacloprid, improving the problems of easy control delay and irreparable crop loss during the control of acute insect pests, reducing the frequent degree of spraying pesticide preparations on crops and further reducing the control cost of the crops.
Some specific examples are listed below, and if mentioned%, all are expressed in weight percent. It should be noted that the following examples are not intended to be exhaustive of all possible cases, and that the materials used in the following examples are commercially available without specific recitation.
Example 1
Mixing 10kg SV-92 and 10kg water to obtain a binary solution;
1kg of zein and 1kg of potassium tripolyphosphate are placed in a binary solution to be stirred and dissolved, the stirring speed is 200 r/min-250 r/min, and the stirring time is more than 3 h;
then 1kg of thiacloprid is put into the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, 41.5kg of water is put into the binary solution to be stirred to obtain a micro-capsule suspending agent containing thiacloprid;
grinding 5kg of water, 4kg of sp-sc3 and 20kg of thiacloprid in a grinding machine to obtain grinding fluid;
then adding 2kg of BQ-809F, 3kg of propylene glycol, 0.45kg of xanthan gum, 0.55kg of magnesium aluminum silicate and 0.5kg of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 2
Mixing 10kg of green 21 and 7kg of water to prepare a binary solution;
2kg of zein and 1kg of sodium tripolyphosphate are placed in a binary solution to be stirred and dissolved, the stirring speed is 200 r/min-250 r/min, and the stirring time is more than 3 h;
then 2kg of thiacloprid is placed in the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, 40kg of water is placed in the binary solution to be stirred to obtain a micro-capsule suspending agent containing thiacloprid;
grinding 7kg of water, 2kg of PEAS03 and 20kg of thiacloprid in a grinder to obtain grinding fluid;
then adding 4kg of BQ-809F, 3kg of propylene glycol, 0.5kg of xanthan gum, 0.5kg of magnesium aluminum silicate and 1g of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 3
Mixing 15kg of FMPC and 6.4kg of water to prepare a binary solution;
placing 3kg of zein and 1kg of phosphorus oxychloride in a binary solution, stirring and dissolving at the stirring speed of 200-250 r/min for more than 3 h;
then 2.5kg of thiacloprid is put into the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, 34kg of water is placed in the binary solution to be stirred to obtain a micro-capsule suspending agent containing thiacloprid;
grinding 7.6kg of water, 4kg of 601 and 18kg of thiacloprid in a grinding machine to obtain grinding fluid;
then adding 3kg of BQ-809F, 4k of ethylene glycol, 0.55kg of xanthan gum, 0.45kg of magnesium aluminum silicate and 0.5kg of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 4
Mixing 15kg of acetone and 10kg of water to prepare a binary solution;
placing 4kg of zein and 2.5kg of potassium tripolyphosphate in a binary solution, stirring and dissolving at a stirring speed of 200-250 r/min for more than 3 h;
then 4kg of thiacloprid is placed in the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, 25kg of water is placed in the binary solution to be stirred to obtain a thiacloprid-containing microcapsule suspending agent;
grinding 4kg of water, 3kg of 1601 and 21kg of thiacloprid in a grinding machine to obtain grinding fluid;
then adding 4kg of T1118, 6kg of propylene glycol, 0.5kg of xanthan gum, 0.5kg of magnesium aluminum silicate and 0.5kg of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 5
Mixing 15kg of FMPC and 10kg of water to prepare a binary solution;
placing 5kg of zein and 2.5kg of potassium tripolyphosphate in a binary solution, stirring and dissolving at a stirring speed of 200-250 r/min for more than 3 h;
then 3.7kg of thiacloprid is put into the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, 32kg of water is put into the binary solution to be stirred to obtain a micro-capsule suspending agent containing thiacloprid;
grinding 4.5kg of water, 4kg of 14105 and 16.8kg of thiacloprid in a grinder to obtain grinding fluid;
then adding 2kg of SK-44, 3kg of ethylene glycol, 0.55kg of xanthan gum, 0.45kg of magnesium aluminum silicate and 0.5g of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 6
Mixing 15kg of n-butanol and 10kg of water to prepare a binary solution;
placing 3kg of zein and 1.5kg of phosphorus oxychloride in a binary solution, stirring and dissolving at the stirring speed of 200-250 r/min for more than 3 hours;
then 4kg of thiacloprid is placed in the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, 35kg of water is placed in the binary solution to be stirred to obtain a thiacloprid-containing microcapsule suspending agent;
grinding 6.5kg of water, 2kg of sp-sc3 and 16.5kg of thiacloprid in a grinder to obtain grinding fluid;
adding 2kg of FS-608A, 3kg of ethylene glycol, 0.5kg of xanthan gum, 0.5kg of magnesium aluminum silicate and 0.5kg of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 7
Mixing 10kg of dimethylbenzene and 10kg of water to prepare a binary solution;
placing 4kg of zein and 5kg of potassium tripolyphosphate in a binary solution, stirring and dissolving at a stirring speed of 200 r/min-250 r/min for more than 3 h;
then 4kg of thiacloprid is placed in the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, placing 36kg of water in a binary solution, and stirring to obtain a thiacloprid-containing microcapsule suspending agent;
grinding 6kg of water, 2kg of SP-3645 and 16.5kg of thiacloprid in a grinding machine to obtain grinding fluid;
adding 2kg of FS-608A, 3kg of ethylene glycol, 0.5kg of xanthan gum, 0.5kg of magnesium aluminum silicate and 0.5kg of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 8
Mixing 15kg of acetone and 10kg of water to prepare a binary solution;
placing 4kg of zein and 2.5kg of potassium tripolyphosphate in a binary solution, stirring and dissolving at a stirring speed of 200-250 r/min for more than 3 h;
then 2.4kg of thiacloprid is put into the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, 25kg of water is placed in the binary solution to be stirred to obtain a thiacloprid-containing microcapsule suspending agent;
grinding 5kg of water, 3kg of 1601 and 21.6kg of thiacloprid in a grinding machine to obtain grinding fluid;
then adding 4kg of T1118, 6kg of propylene glycol, 0.5kg of xanthan gum, 0.5kg of magnesium aluminum silicate and 0.5kg of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 9
Mixing 15kg of FMPC and 10kg of water to prepare a binary solution;
placing 5kg of zein and 2.5kg of potassium tripolyphosphate in a binary solution, stirring and dissolving at a stirring speed of 200-250 r/min for more than 3 h;
then 2kg of thiacloprid is placed in the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then placing 27kg of water into the binary solution and stirring to obtain a thiacloprid-containing microcapsule suspending agent;
grinding 5kg of water, 4kg of 14105 and 23kg of thiacloprid in a grinder to obtain grinding fluid;
then adding 2kg of SK-44, 3kg of ethylene glycol, 0.55kg of xanthan gum, 0.45kg of magnesium aluminum silicate and 0.5g of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 10
Mixing 15kg of n-butanol and 10kg of water to prepare a binary solution;
placing 3kg of zein and 1.5kg of phosphorus oxychloride in a binary solution, stirring and dissolving at the stirring speed of 200-250 r/min for more than 3 hours;
then, 1.3kg of thiacloprid is placed in the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, 29kg of water is placed in a binary solution to be stirred to obtain a micro-capsule suspending agent containing thiacloprid;
grinding 7kg of water, 2kg of sp-sc3 and 24.7kg of thiacloprid in a grinder to obtain grinding fluid;
adding 2kg of FS-608A, 3kg of ethylene glycol, 0.5kg of xanthan gum, 0.5kg of magnesium aluminum silicate and 0.5kg of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
Example 11
Mixing 10kg of dimethylbenzene and 10kg of water to prepare a binary solution;
placing 4kg of zein and 5kg of potassium tripolyphosphate in a binary solution, stirring and dissolving at a stirring speed of 200 r/min-250 r/min for more than 3 h;
then 0.6kg of thiacloprid is put into the binary solution to be stirred and dissolved, the stirring speed is 200r/min to 250r/min, and the stirring time is more than 30 min;
then, putting 24.5kg of water into the binary solution, and stirring to obtain a thiacloprid-containing microcapsule suspending agent;
grinding 8kg of water, 2kg of SP-3645 and 29.4kg of thiacloprid in a grinding machine to obtain grinding fluid;
adding 2kg of FS-608A, 3kg of ethylene glycol, 0.5kg of xanthan gum, 0.5kg of magnesium aluminum silicate and 0.5kg of kasong into the grinding fluid in the grinding machine for grinding;
and finally, adding the grinding liquid into a micro-capsule suspending agent containing thiacloprid for mixing to obtain the double-release preparation containing thiacloprid.
The thiacloprid-containing dual-release preparations of examples 1 to 11, which were prepared by the method for preparing the thiacloprid-containing dual-release preparation of the present application, were subjected to the following performance tests:
the test results are shown in table 1:
Figure BDA0003194455700000211
table 1: results of Performance test of Thiacloprid-containing Dual Release formulations of examples 1 to 11
The thiacloprid-containing double-release preparations of examples 1 to 11, which were prepared by the method for preparing the thiacloprid-containing double-release preparation of the present application, were diluted with purified water to a thiacloprid concentration of 100ppm, and the thiacloprid contents of the leaves, roots and stems were measured 48 hours later using the diluted thiacloprid-containing double-release preparations of examples 1 to 11, respectively, in hydroponic pepper seedlings.
The results are shown in table 2:
Figure BDA0003194455700000221
table 2: thiacloprid content detection result of leaf part, root part and stem part
As can be seen from tables 1 and 2, the thiacloprid crystals do not precipitate in the thiacloprid-containing dual-release formulations of examples 1 to 11, and the heat storage stability is both acceptable, which indicates that the thiacloprid-containing dual-release formulations of examples 1 to 11 have better stability, moreover, the micro-capsule encapsulation efficiency and the drug loading rate of the thiacloprid-containing dual-release preparation of the examples 1 to 11 are high, and particularly the thiacloprid-containing dual-release preparation of the examples 5 and 9 show that the thiacloprid-containing dual-release preparation of the examples 1 to 11 has good slow release property and good drug effect durability, and the thiacloprid-containing dual-release preparations of examples 1 to 11 can rapidly make the leaves, roots and stems of the pepper seedlings contain higher content of thiacloprid, especially the thiacloprid-containing dual-release preparations of examples 5 and 9, which shows that the thiacloprid-containing dual-release preparations of examples 1 to 11 have the capability of rapidly releasing thiacloprid to an effective control concentration.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A double-release preparation containing thiacloprid is characterized by comprising a suspending agent containing thiacloprid and a microcapsule suspending agent containing thiacloprid which are mixed and dissolved.
2. The thiacloprid-containing dual-release preparation according to claim 1, wherein the mass ratio of the thiacloprid-containing suspending agent to the thiacloprid-containing microcapsule suspending agent is 0.8 to 1.5.
3. The thiacloprid-containing dual release formulation according to claim 1 characterized in that the thiacloprid-containing dual release formulation comprises the following components:
thiacloprid, solvent, modified material, zein, wetting dispersant and water.
4. The thiacloprid-containing dual-release preparation according to claim 1, which is characterized by comprising the following components in parts by mass:
Figure FDA0003194455690000011
5. the thiacloprid-containing dual-release preparation according to claim 3 or 4, characterized in that the solvent is at least one of an alcohol solvent, a ketone solvent, an amide solvent, an aromatic hydrocarbon solvent and an environmentally friendly solvent.
6. The thiacloprid-containing dual release formulation according to claim 3 or 4 wherein the modifying material is a phosphate compound.
7. The thiacloprid-containing dual release formulation according to claim 3 or 4 wherein the modifying material is at least one of potassium tripolyphosphate, sodium tripolyphosphate, and phosphorus oxychloride.
8. The thiacloprid-containing dual release formulation according to claim 3 or 4, characterized in that the wetting dispersant is at least one of polycarboxylate dispersant, gemini dispersant, phosphate dispersant, block polyether dispersant, carboxylate dispersant and non-ionic hydroxy polyethylene oxide block copolymer dispersant.
9. A method for preparing the thiacloprid-containing dual-release preparation, which is used for preparing the thiacloprid-containing dual-release preparation of any one of claims 1 to 8, and is characterized by comprising the following steps:
preparing a solvent and part of water to obtain a binary solution;
placing zein, a phosphate compound and part of thiacloprid in the binary solution for dissolving treatment;
placing 80-90% of the rest water in the binary solution after dissolving treatment for nanocrystallization treatment to obtain a thiacloprid-containing microcapsule suspending agent;
grinding the rest water, the wetting dispersant and the rest thiacloprid to obtain grinding fluid;
and adding the grinding liquid into the thiacloprid-containing microcapsule suspending agent for mixing operation to obtain the thiacloprid-containing double-release preparation.
10. The method for preparing a thiacloprid-containing dual release preparation according to claim 9, which is characterized in that the zein, the phosphate compound and 2 to 10 percent of thiacloprid are placed in a binary solution for dissolution treatment.
CN202110886815.4A 2021-08-03 2021-08-03 Double-release preparation containing thiacloprid and preparation method thereof Pending CN113812416A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110886815.4A CN113812416A (en) 2021-08-03 2021-08-03 Double-release preparation containing thiacloprid and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110886815.4A CN113812416A (en) 2021-08-03 2021-08-03 Double-release preparation containing thiacloprid and preparation method thereof

Publications (1)

Publication Number Publication Date
CN113812416A true CN113812416A (en) 2021-12-21

Family

ID=78924220

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110886815.4A Pending CN113812416A (en) 2021-08-03 2021-08-03 Double-release preparation containing thiacloprid and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113812416A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101743960A (en) * 2010-02-01 2010-06-23 吴学民 Thiacloprid microcapsule powder agent, suspending agent and preparation method and application thereof
CN102187871A (en) * 2010-11-22 2011-09-21 南通联农农药制剂研究开发有限公司 Thiacloprid microcapsule preparation and preparation method thereof
CN109699656A (en) * 2017-10-26 2019-05-03 江苏克胜集团股份有限公司 A kind of paichongding suspending agent and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101743960A (en) * 2010-02-01 2010-06-23 吴学民 Thiacloprid microcapsule powder agent, suspending agent and preparation method and application thereof
CN102187871A (en) * 2010-11-22 2011-09-21 南通联农农药制剂研究开发有限公司 Thiacloprid microcapsule preparation and preparation method thereof
CN109699656A (en) * 2017-10-26 2019-05-03 江苏克胜集团股份有限公司 A kind of paichongding suspending agent and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
喻祥龙等: ""玉米醇溶蛋白作为纳米运载体的研究进展"", 《天然产物研究与开发》 *
林冠权: ""改性玉米醇溶蛋白负载阿维菌素纳米农药的制备及性能"", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑》 *

Similar Documents

Publication Publication Date Title
CN103283746B (en) One planting fruit-trees, forest trunk disease therapeutic agent
CN1559216A (en) Seed coating agent for preventing smut
CN112568241A (en) Granular insecticide and its preparing process
CN114181460A (en) Antibacterial polypropylene composite plastic and preparation method thereof
CN103875680A (en) Seed coating for preventing aflatoxin contamination of peanuts
CN109699653A (en) Epoxiconazole aqueous suspension agent and preparation method thereof
CN113812416A (en) Double-release preparation containing thiacloprid and preparation method thereof
CN113498782A (en) Emamectin benzoate nano preparation based on zein and preparation method thereof
CN111345294A (en) Butylbenzone-ethyl water dispersible granule and preparation method thereof
CN101953335B (en) Metribuzin colloidal suspension and preparation method thereof
JPS6284004A (en) Improved herbicidal granular composition
CN1593146A (en) Chlorpyrifos containing powder coating agent
JPH01283201A (en) Stable agricultural chemical composition suspended in water
CN104757020A (en) Cupric hydroxide dry suspending agent and preparation method thereof
CN114532334A (en) Azole ether and fine nail cream granules and preparation method thereof
CN112167256A (en) Compound granule containing thifluzamide and fluazinam and preparation method and application thereof
CN112806379B (en) Hexaconazole-kresoxim-methyl suspending agent and preparation method thereof
AU2018101558B4 (en) Synthetic method for a butroxydim water dispersible granule
CN102696682B (en) Wanlongmycin dimethomorph suspending agent, preparation method thereof and application
CN111096329A (en) Microcapsule suspension-suspending agent containing efficient cyhalothrin and clothianidin and preparation method thereof
CN111567540A (en) Bactericide agent composition containing flumorph and pyraclostrobin
CN104604875A (en) Bactericide composition comprising sedaxane and picoxystrobin as well as application of bactericide composition
CN114651833B (en) Insecticidal composition containing dimefon and application thereof
CN115104609B (en) Oligosaccharide plant sterilization synergistic composition and preparation method thereof
CN107467030A (en) Seed treatment compositions containing fludioxonil, Metalaxyl-M and fluorine pyrrole furanone

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20211221

RJ01 Rejection of invention patent application after publication