CN115067325A - Preparation method of anhydrous dinotefuran suspending agent - Google Patents

Preparation method of anhydrous dinotefuran suspending agent Download PDF

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Publication number
CN115067325A
CN115067325A CN202210673804.2A CN202210673804A CN115067325A CN 115067325 A CN115067325 A CN 115067325A CN 202210673804 A CN202210673804 A CN 202210673804A CN 115067325 A CN115067325 A CN 115067325A
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Prior art keywords
dinotefuran
suspending agent
anhydrous
agent
alcohol
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CN202210673804.2A
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Chinese (zh)
Inventor
陈新星
彭昆
崔大鹏
姜海鹏
武磊
袁剑桥
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Jiangsu Sword Agrochemicals Co ltd
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Jiangsu Sword Agrochemicals Co ltd
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    • 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
    • A01N51/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring

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

Abstract

The invention discloses a preparation method of an anhydrous dinotefuran suspending agent, which comprises a dinotefuran raw pesticide, a dispersing agent, a wetting agent, a thickening agent, a preservative and an alcohol filler, wherein the dinotefuran raw pesticide accounts for 1-50 wt% of the suspending agent, 3-5 wt% of the dispersing agent, 3-5 wt% of the wetting agent, 0.15-0.3 wt% of the thickening agent, 0.3-1 wt% of the preservative and the balance of the alcohol filler, and all the components are added according to mass percentage; the anhydrous dinotefuran suspending agent is obtained by mixing, shearing, sanding, filtering, weighing and detecting the components. The anhydrous suspending agent provided by the invention has the advantages of being capable of being uniformly mixed and dispersed with water in any proportion, good in fluidity, capable of improving the drug effect, free from the influence of water quality and water temperature, convenient to use, not easy to pollute the environment, and capable of spraying after being diluted; the invention greatly improves the adhesion and the permeability of the product by adding the special alcohol mixture as the filler, thereby improving the drug effect.

Description

Preparation method of anhydrous dinotefuran suspending agent
Technical Field
The invention belongs to the technical field of plant pesticides, and particularly relates to a preparation method of an anhydrous dinotefuran suspending agent which has a good pesticidal effect and is stable in quality.
Background
Dinotefuran is mainly oriented to the market by soluble liquid, water dispersible granules and water suspending agent in China. The soluble agent uses a large amount of organic solvent in production, which wastes resources and pollutes the environment after being used. The water dispersible granules are easy to generate dust pollution during processing and use, and the existing flying prevention application is common, so that the spray head is easy to block due to poor dispersion of the water dispersible granules, and the operation efficiency is influenced. The water suspending agent can generate crystallization and large grain diameter due to the high solubility of the dinotefuran in water, which affects the quality of products, and liquid medicine can not be poured out and cleaned by farmers when in use.
The dinotefuran pure product is white crystal, has the melting point of 107.5 ℃, the solubility of 40 g/L water and is difficult to dissolve in organic solvents such as xylene, cyclohexane and the like. The action mechanism is as follows: dinotefuran mainly acts on insect nerve transmission systems, so that pests are paralyzed to play a role in killing insects. Also known as nicotinic acetylcholine receptor (nAChR) agonists, which causes the insect to die by abnormal excitation, general spasm, paralysis. It has not only contact poisoning and stomach poisoning action, but also excellent systemic and osmotic action, and can be quickly absorbed by root, stem and leaf of plant and upwards conducted. Belongs to the third generation of nicotine pesticide. Has the functions of contact killing and stomach toxicity, strong systemic property and long lasting period, has wider insecticidal spectrum and more convenient use compared with first and second generation insecticides, and can overcome the resistance risk brought by the first and second generation insecticides.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide an anhydrous dinotefuran suspending agent aiming at the defects of the prior art, wherein an alcohol product is used as a filler instead of water, so that the product quality is improved, and the product adhesiveness, permeability and moisture retention are improved to achieve a synergistic effect.
The technical scheme is as follows: the invention relates to a preparation method of an anhydrous dinotefuran suspending agent, which comprises a dinotefuran raw pesticide, a dispersing agent, a wetting agent, a thickening agent, a preservative and an alcohol filler, wherein the dinotefuran raw pesticide accounts for 1-50 wt% of the suspending agent, 3-5 wt% of the dispersing agent, 3-5 wt% of the wetting agent, 0.15-0.3 wt% of the thickening agent, 0.3-1 wt% of the preservative and the balance of the alcohol filler, and all the components are added according to mass percentage; the anhydrous dinotefuran suspending agent is obtained by mixing, shearing, sanding, filtering, weighing and detecting the components.
Further, as a preferred embodiment, the alcohol filler is one or a combination of ethanol, ethylene glycol, propylene glycol, glycerol, isooctanol, benzyl alcohol, sorbitol or xylitol.
Further, as a preferred embodiment, the dispersant is one or a mixture of more of triphenylethylene phenol polyoxyethylene ether phosphate triethanolamine, acrylic copolymer sodium polycarboxylate, alkylphenol polyoxyethylene ether and naphthalene sulfonate complex or alkylphenol polyoxyethylene ether and naphthalene sulfonate complex.
Further, as a preferred embodiment, the wetting agent is one or a mixture of several of fatty alcohol-polyoxyethylene ether, fatty alcohol-dodecyl sulfate, dodecyl sulfonate or dodecyl sulfate.
Further, as a preferred embodiment, the thickening agent is one or a mixture of more of xanthan gum, magnesium aluminum silicate, starch, attapulgite, organic bentonite, pectin, acacia, gelatin, methyl cellulose, carboxymethyl cellulose, polyvinyl alcohol, silicon dioxide and alginic acid.
Further, as a preferred embodiment, the preservative is one or a mixture of several of benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, isothiazolinone, formaldehyde or paraformaldehyde.
Has the advantages that: (1) the anhydrous suspending agent provided by the invention has the advantages of being capable of being uniformly mixed and dispersed with water in any proportion, good in fluidity, capable of improving the drug effect, free from the influence of water quality and water temperature, convenient to use, not easy to pollute the environment, and capable of spraying after being diluted; (2) in the invention, a special alcohol mixture is added as a filler, so that the adhesion and the permeability of the product are greatly improved, and the drug effect is improved; (3) the anhydrous suspending agent provided by the invention is processed by a wet method, does not generate dust, replaces benzene organic solvent with naturally degraded alcohol mixture, meets the requirement of environmental protection, has finer particle size than water dispersible granules, uniform dispersion of active ingredients, high suspension rate and higher drug effect than the water dispersible granules, and is an ideal new environment-friendly formulation at present; (4) the anhydrous dinotefuran suspending agent is prepared by replacing water with alcohol mixture, the quality problems of crystallization and creaming are avoided, and the product quality is stable.
Detailed Description
The technical solution of the present invention is described in detail by the following examples, but the scope of the present invention is not limited to the examples.
Example 1: a preparation method of an anhydrous dinotefuran suspending agent comprises the following steps of: 2% of dinotefuran original drug, 2% of dispersant tristyrene phenol polyoxyethylene ether phosphate triethanolamine, 1% of compound of alkylphenol polyoxyethylene ether and naphthalenesulfonate, 2% of wetting agent deca fatty alcohol polyoxyethylene, 1% of lauryl sulfate, 0.25% of thickening agent xanthan gum, 0.1% of magnesium aluminum silicate, 0.3% of preservative isothiazoline, 0.2% of paraformaldehyde, 30% of filler sorbitol and 61.1% of ethylene glycol, mixing, shearing, sanding and filtering to prepare a sample 1.
Example 2: a preparation method of an anhydrous dinotefuran suspending agent comprises the following steps of: 20% of dinotefuran original drug, 2% of dispersant tristyrylphenol polyoxyethylene ether phosphate triethanolamine, 1% of acrylic copolymer sodium polycarboxylate, 1% of alkylphenol polyoxyethylene ether and naphthalenesulfonate complex, 2% of wetting agent fatty alcohol polyoxyethylene, 2% of lauryl sulfate, 0.15% of thickening agent xanthan gum, 0.05% of magnesium aluminum silicate, 0.3% of preservative isothiazoline, 0.2% of paraformaldehyde, 20% of filler sorbitol and 50.9% of ethylene glycol, and mixing, shearing, sanding and filtering to prepare a sample 2.
Example 3: a preparation method of an anhydrous dinotefuran suspending agent comprises the following steps of: 40% of dinotefuran original drug, 2% of dispersant tristyrylphenol polyoxyethylene ether phosphate triethanolamine, 2% of acrylic copolymer sodium polycarboxylate, 1% of alkylphenol polyoxyethylene ether and naphthalenesulfonate complex, 3% of wetting agent fatty alcohol polyoxyethylene, 2% of lauryl sulfate, 0.1% of thickening agent xanthan gum, 0.1% of magnesium aluminum silicate, 0.4% of preservative isothiazoline, 0.2% of paraformaldehyde, 10% of filler sorbitol and 38.4% of ethylene glycol, and mixing, shearing, sanding and filtering to prepare a sample 3.
Example 4: test and control data for samples prepared in examples 1-3
And (3) detecting the fineness, namely, respectively passing the products of examples 1 to 3 through three different screens of 200 meshes, 325 meshes and 500 meshes to measure the fineness of the products. The higher the fineness, the smaller the particle size of the product and the more stable the product quality, the results are shown in Table 1. The results show that the sample schemes 1-3 of the anhydrous dinotefuran suspending agent are superior to the commercial comparative sample 20% dinotefuran aqueous suspending agent.
TABLE 1 comparison of fineness measurements of samples from examples 1-3 with commercially available similar products
Figure BDA0003694100080000031
Wherein the dinotefuran technical material recorded in the examples 1-3 is purchased from: jingmen Jinxianda Biotech Co., Ltd;
the commercially available products of the same type in Table 1 are selected from: shandong province LvShi pesticide Co., Ltd, its name is Laifei.
The control effect test shows that the control effect is investigated on 7 days and 14 days after the application of the pesticide by diluting the schemes 1 to 3 with water by 1000 times and spraying the water to rice planthoppers and 1500 times to wheat aphids, and the control effect is shown in the attached table 2.
Test results show that the anhydrous dinotefuran suspending agent has remarkable control effect on rice planthopper and wheat aphid, the control effect on the rice planthopper and the wheat aphid in 4 days and 7 days is more than 85%, the control effect in 14 days is more than 75%, and the control effect is obviously higher than that of a comparative sample which is 20% of dinotefuran suspending agent.
TABLE 2 comparison of control effect test results of samples of examples 1-3 with similar products on the market
Figure BDA0003694100080000041
Wherein the dinotefuran technical material described in examples 1-3 is purchased from: jingmen Jinxianda Biotech Co., Ltd;
the commercially available products of the same type in Table 1 are selected from: shandong province LvShi pesticide Co., Ltd, its name is Laifei.
As noted above, while the present invention has been shown and described with reference to certain preferred embodiments, it is not to be construed as limited thereto. Various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (6)

1. A preparation method of an anhydrous dinotefuran suspending agent is characterized by comprising the following steps: the dinotefuran suspending agent comprises 1-50 wt% of dinotefuran raw pesticide, 3-5 wt% of dispersing agent, 3-5 wt% of wetting agent, 0.15-0.3 wt% of thickening agent, 0.3-1 wt% of preservative and the balance of alcohol filler, wherein the dinotefuran raw pesticide accounts for 1-50 wt% of suspending agent; the anhydrous dinotefuran suspending agent is obtained by mixing, shearing, sanding, filtering, weighing and detecting the components.
2. The method for preparing the anhydrous dinotefuran suspending agent according to claim 1, wherein the method comprises the following steps: the alcohol filler is one or a combination of ethanol, ethylene glycol, propylene glycol, glycerol, isooctanol, benzyl alcohol, sorbitol or xylitol.
3. The method for preparing the anhydrous dinotefuran suspending agent according to claim 2, wherein the method comprises the following steps: the dispersing agent is one or a mixture of more of triphenylethylene phenol polyoxyethylene ether phosphate triethanolamine, acrylic acid copolymer sodium polycarboxylate, alkylphenol polyoxyethylene ether and naphthalene sulfonate complex or alkylphenol polyoxyethylene ether and naphthalene sulfonate complex.
4. The method for preparing the anhydrous dinotefuran suspending agent according to claim 3, wherein the method comprises the following steps: the wetting agent is one or a mixture of fatty alcohol-polyoxyethylene ether, fatty alcohol-dodecyl-sulfate, dodecyl sulfonate or dodecyl sulfate.
5. The method for preparing the anhydrous dinotefuran suspending agent according to claim 4, wherein the method comprises the following steps: the thickening agent is one or more of xanthan gum, magnesium aluminum silicate, starch, attapulgite, organic bentonite, pectin, Arabic gum, gelatin, methyl cellulose, carboxymethyl cellulose, polyvinyl alcohol, silicon dioxide and alginic acid.
6. The method for preparing the anhydrous dinotefuran suspending agent according to claim 5, wherein the method comprises the following steps: the preservative is one or a mixture of benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, isothiazolinone, formaldehyde or paraformaldehyde.
CN202210673804.2A 2022-06-14 2022-06-14 Preparation method of anhydrous dinotefuran suspending agent Pending CN115067325A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102239829A (en) * 2011-07-13 2011-11-16 南京扬子鸿利源化学品有限责任公司 Dinotefuran aqueous suspension agent and its preparation method
CN102239878A (en) * 2011-07-05 2011-11-16 江苏丘陵地区镇江农业科学研究所 Insecticide composite containing dinotefuran, preparation formulations and preparation method thereof
CN104663701A (en) * 2015-01-23 2015-06-03 河北威远生化农药有限公司 Dinotefuran synergistic suspending agent and preparation method thereof
CN110903810A (en) * 2019-11-18 2020-03-24 宁波日晟新材料有限公司 Hydrophilic non-oily anhydrous ceramic material suspending agent and preparation method and application thereof
CN115624032A (en) * 2022-07-12 2023-01-20 江苏剑牌农化股份有限公司 Preparation method of prochloraz-epoxiconazole water emulsion

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102239878A (en) * 2011-07-05 2011-11-16 江苏丘陵地区镇江农业科学研究所 Insecticide composite containing dinotefuran, preparation formulations and preparation method thereof
CN102239829A (en) * 2011-07-13 2011-11-16 南京扬子鸿利源化学品有限责任公司 Dinotefuran aqueous suspension agent and its preparation method
CN104663701A (en) * 2015-01-23 2015-06-03 河北威远生化农药有限公司 Dinotefuran synergistic suspending agent and preparation method thereof
CN110903810A (en) * 2019-11-18 2020-03-24 宁波日晟新材料有限公司 Hydrophilic non-oily anhydrous ceramic material suspending agent and preparation method and application thereof
CN115624032A (en) * 2022-07-12 2023-01-20 江苏剑牌农化股份有限公司 Preparation method of prochloraz-epoxiconazole water emulsion

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Application publication date: 20220920