CN111165486B - Magnetic pesticide loss control agent, preparation method and application - Google Patents

Magnetic pesticide loss control agent, preparation method and application Download PDF

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CN111165486B
CN111165486B CN202010093994.1A CN202010093994A CN111165486B CN 111165486 B CN111165486 B CN 111165486B CN 202010093994 A CN202010093994 A CN 202010093994A CN 111165486 B CN111165486 B CN 111165486B
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pesticide
magnetic
loss control
control agent
meshes
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CN111165486A (en
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蔡冬清
王冬芳
吴正岩
仲乃琴
宗志强
叶静宏
张小江
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Donghua University
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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
    • A01N25/24Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients to enhance the sticking of the active ingredients
    • 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
    • A01N57/00Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
    • A01N57/10Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
    • A01N57/16Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing heterocyclic radicals

Abstract

The invention discloses a magnetic pesticide loss control agent, a preparation method and application. The magnetic pesticide loss control agent is prepared by compounding attapulgite and alkali/ammonium persulfate modified weathered coal. The preparation method comprises the following steps: mixing quicklime and weathered coal, adding into water, and making into suspension; and uniformly mixing ammonium persulfate, ferroferric oxide and attapulgite, adding into the suspension, filtering, and drying filter residues to constant weight to obtain the magnetic pesticide loss control agent. And adding the magnetic pesticide loss control agent into a pesticide to obtain the loss control pesticide. The magnetic pesticide loss control agent is developed through physicochemical modification, so that the adhesion capability of pesticide on crops can be effectively improved, the pesticide mobility is reduced, volatilization is reduced, the water leaching resistance of the pesticide is improved, the pesticide application reduction and synergism are realized, and the purpose of controlling loss is achieved. After the prevention and control are finished, the magnetic pesticide loss control agent on the crops and the pesticide can be recovered together through the magnet, so that the pesticide residue is reduced.

Description

Magnetic pesticide loss control agent, preparation method and application
Technical Field
The invention relates to a magnetic pesticide loss control agent, a preparation method and application, and belongs to the technical field of agriculture.
Background
The pesticide is an indispensable production data in the agricultural production process, and plays an indispensable role in preventing and treating crop diseases and insect pests, ensuring grain yield and promoting healthy development of agriculture. According to statistics of food and agricultural organization data of the united nations, if no pesticide controls plant diseases and insect pests, the world food loss is as high as 30-40%, and for some special crops, the yield is greatly reduced, even the crop is no longer produced. The annual output of pesticides is more than 500 million tons all over the world. The pesticide can control plant diseases and insect pests, improve yield, and simultaneously cause adverse effects on human living environment, body health and even the whole ecological system. According to the research, only 10-25% of the pesticide is attached to the plants after field spraying, about 30% of the pesticide is attached to the plants during spraying, 40-60% of the pesticide falls on the ground, and 10-30% of the pesticide floats in the air. Under the action of wind blowing and rain, a large amount of unused pesticides enter soil and water through volatilization, air transportation, dry and wet sedimentation, surface runoff, percolation and other ways, so that three-dimensional pollution to air, soil, surface water and underground water is caused. Then, the food enters the human body through a food chain or air, and the health is harmed. Therefore, focusing on the improvement of the existing pesticide variety processing dosage form and formula, the improvement of physical and chemical properties, the improvement of the using method and the like become important problems to be solved urgently in modern agricultural production. Among the many methods, pesticide loss control technology has become one of the major directions in the development of modern pesticides. The loss control technology aims to improve the adhesive force of the pesticide on plant leaves, reduce the loss of the pesticide, improve the utilization rate of the pesticide and the like, can economically, safely, effectively and reasonably control the plant diseases and insect pests, and can reduce the pollution of the pesticide to the environment to the minimum.
At present, the method for controlling the pesticide loss mainly adopts a spreading technology, and generally adopts the addition of a nitrogen ketone-based spreading agent to enhance the spreading speed and the permeation speed of the pesticide on the leaf surface so as to reduce the pesticide loss. Although the technology relieves the loss of pesticide to a certain extent, the technology still cannot work in rainy season due to poor capability of resisting rain washing. A study of Nanjing university shows that the roughness of the surface of the leaves is positively correlated with the dust retention capacity of the leaves. Therefore, pesticide molecules can be attached to the plant leaf surfaces through the nano composite material, the mobility of the pesticide molecules is reduced, volatilization is reduced, and the water leaching resistance of the pesticide molecules is improved, so that the purpose of controlling loss is achieved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to improve the water leaching resistance of the pesticide after application.
In order to solve the technical problem, the invention provides a magnetic pesticide loss control agent which is characterized by being prepared by compounding attapulgite, alkali/ammonium persulfate modified weathered coal.
The invention also provides a preparation method of the magnetic pesticide loss control agent, which is characterized by comprising the following steps:
step 1): mixing quicklime and weathered coal according to the ratio of (1-3): (3-5), adding the mixture into water to prepare a suspension with the initial concentration of 50-100g/L, stirring at normal temperature for 30-50 minutes to enable quick lime to react with water, and enabling generated Ca (OH)2 to enable macromolecular humic acid in weathered coal to be subjected to alkaline hydrolysis to be micromolecular fulvic acid so as to contain a large amount of carboxyl and hydroxyl;
step 2): uniformly mixing ammonium persulfate, ferroferric oxide and attapulgite according to the mass ratio of (1-2) to (6-9);
step 3): adding the mixture obtained in the step 2) into the suspension obtained in the step 1) at a concentration of 50-80g/L, and stirring for 10-30 minutes at 30-80 ℃, wherein ammonium persulfate oxidizes residual macromolecular humic acid in weathered coal into micromolecular fulvic acid through oxidation, the molecules of the fulvic acid are further reduced, and the fulvic acid is modified to the surfaces of ferroferric oxide and attapulgite;
step 4): filtering the suspension obtained in the step 3), drying the filter residue at 30-80 ℃ to constant weight, and crushing to 500-mesh and 1000-mesh to obtain the magnetic pesticide loss control agent.
Preferably, the fineness of the quicklime in the step 1) is 50-100 meshes; the humic acid content of the weathered coal is 20-40% by mass, and the fineness of the weathered coal is 50-100 meshes.
Preferably, the rotation speed of the stirring in the step 1) is 100-200 rpm.
Preferably, the fineness of the ammonium persulfate in the step 2) is 50-100 meshes; the fineness of the ferroferric oxide is 50-100 meshes; the fineness of the attapulgite is 50-100 meshes.
Preferably, the rotation speed of the stirring in the step 3) is 100-200 rpm.
The invention also provides application of the magnetic pesticide loss control agent, which is characterized in that the magnetic pesticide loss control agent is added into pesticide according to the mass percent of 5-15%, and the loss control type pesticide is prepared.
Preferably, the pesticide is in the form of a suspension, a powder, a wettable powder, a tablet or a granule.
The alkali and ammonium persulfate can convert macromolecular humic acid in weathered coal into micromolecular humic acid (fulvic acid), and the humic acid contains a large amount of carboxyl and hydroxyl. After the alkali/ammonium persulfate modified weathered coal is compounded with attapulgite and ferroferric oxide, the groups can be modified on attapulgite rod crystals and ferroferric oxide, so as to prepare the magnetic pesticide loss control agent. The groups can be combined with pesticide molecules through hydrogen bonds and electrostatic attraction, so that the adhesive force of the pesticide on the leaf surfaces of crops is improved, and the pesticide loss is reduced.
The magnetic pesticide loss control agent is developed through physicochemical modification, so that the adhesion capability of pesticide on crops can be effectively improved, the pesticide mobility is reduced, volatilization is reduced, the water leaching resistance of the pesticide is improved, the pesticide application reduction and synergism are realized, and the purpose of controlling loss is achieved. After the prevention and control are finished, the magnetic pesticide loss control agent on the crops and the pesticide can be recovered together through the magnet, so that the pesticide residue is reduced. The invention has the advantages of low cost, environmental protection and the like, and has wide application prospect.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
Example 1
A preparation method of a magnetic pesticide loss control agent comprises the following steps:
(1) mixing quicklime (50 meshes) and weathered coal (20% of humic acid by mass and 50 meshes) according to the weight ratio of 1: 3, and the mixture was added to tap water to prepare a suspension having an initial concentration (immediately after quicklime was added to water) of 50g/L, and the suspension was stirred at room temperature (100rpm) for 30 minutes to react quicklime with water (CaO + H20 ═ ca (oh))2) Formation of Ca (OH)2Can lead macromolecular humic acid in weathered coal to be alkaline hydrolyzed into micromolecular fulvic acid, thereby containing a large amount of carboxyl and hydroxyl;
(2) uniformly mixing ammonium persulfate (50 meshes), ferroferric oxide (50 meshes) and attapulgite (50 meshes) according to the mass ratio of 1:1: 6;
(3) adding the mixture obtained in the step (2) into the mixture obtained in the step (1) according to the concentration of 50g/L, and stirring at 30 ℃ (100rpm) for 10 minutes, wherein ammonium persulfate oxidizes residual macromolecular humic acid in weathered coal into micromolecular fulvic acid through oxidation, molecules of the fulvic acid are further reduced, and the fulvic acid is modified to the surfaces of ferroferric oxide and attapulgite;
(4) filtering the suspension obtained in the step (3), drying filter residues at 30 ℃ to constant weight, and crushing to 500 meshes to obtain the magnetic pesticide loss control agent;
(5) the magnetic pesticide loss control agent is added into pesticide according to the mass fraction of 5%, and the pesticide dosage form comprises suspending agent, powder, wettable powder, tablets and granules, so that the loss control pesticide is prepared.
Example 2
A preparation method of a magnetic pesticide loss control agent comprises the following steps:
(1) mixing quicklime (70 meshes) and weathered coal (30% of humic acid by mass and 70 meshes) according to the weight ratio of 1: 2, and the mixture was added to tap water to prepare a suspension having an initial concentration of 70g/L (immediately after quicklime was added to water), and the suspension was stirred at room temperature (150rpm) for 40 minutes to react quicklime with water (CaO + H20 ═ ca (oh))2) Formation of Ca (OH)2Can lead macromolecular humic acid in weathered coal to be alkaline hydrolyzed into micromolecular fulvic acid, thereby containing a large amount of carboxyl and hydroxyl;
(2) uniformly mixing ammonium persulfate (70 meshes), ferroferric oxide (70 meshes) and attapulgite (70 meshes) according to the mass ratio of 1:1: 7;
(3) adding the mixture obtained in the step (2) into the mixture obtained in the step (1) according to the concentration of 70g/L, and stirring at 50 ℃ (150rpm) for 20 minutes, wherein ammonium persulfate oxidizes residual macromolecular humic acid in weathered coal into micromolecular fulvic acid through oxidation, molecules of the fulvic acid are further reduced, and the fulvic acid is modified to the surfaces of ferroferric oxide and attapulgite;
(4) filtering the suspension obtained in the step (3), drying filter residues at 50 ℃ to constant weight, and crushing to 700 meshes to obtain the magnetic pesticide loss control agent;
(5) the magnetic pesticide loss control agent is added into pesticide according to the mass fraction of 10%, and the pesticide dosage form comprises suspending agent, powder, wettable powder, tablets and granules, so that the loss control pesticide is prepared.
Example 3
A preparation method of a magnetic pesticide loss control agent comprises the following steps:
(1) mixing quicklime (100 meshes) and weathered coal (40% of humic acid by mass and 100 meshes) according to the weight ratio of 3: 5, and the mixture was added to tap water to prepare a suspension having an initial concentration (immediately after quicklime was added to water) of 100g/L, and the suspension was stirred at room temperature (200rpm) for 50 minutes to react quicklime with water (CaO + H20 ═ ca (oh))2) Formation of Ca (OH)2Can lead macromolecular humic acid in weathered coal to be alkaline hydrolyzed into micromolecular fulvic acid, thereby containing a large amount of carboxyl and hydroxyl;
(2) uniformly mixing ammonium persulfate (100 meshes), ferroferric oxide (100 meshes) and attapulgite (100 meshes) according to the mass ratio of 2:2: 9;
(3) adding the mixture obtained in the step (2) into the mixture obtained in the step (1) according to the concentration of 80g/L, and stirring at 80 ℃ (200rpm) for 30 minutes, wherein ammonium persulfate oxidizes residual macromolecular humic acid in weathered coal into micromolecular fulvic acid through oxidation, molecules of the fulvic acid are further reduced, and the fulvic acid is modified to the surfaces of ferroferric oxide and attapulgite;
(4) filtering the suspension obtained in the step (3), drying filter residues at 80 ℃ to constant weight, and crushing to 1000 meshes to obtain the magnetic pesticide loss control agent;
(5) the magnetic pesticide loss control agent is added into pesticide according to the mass fraction of 15%, and the pesticide dosage form comprises suspending agent, powder, wettable powder, tablets and granules, so that the loss control pesticide is prepared.
The obtained magnetic pesticide loss control agent and different pesticide auxiliaries are used for carrying out related tests on the chlorpyrifos attachment efficiency on different carriers, and the experimental method of the attachment increase rate is as follows:
1) adding the magnetic pesticide loss control agent into a 1g/L (1g/L) water suspension of chlorpyrifos according to the mass fraction of 10%, and uniformly stirring;
2) vertically soaking a cover glass (2cm multiplied by 2cm) and peanut leaves (2cm multiplied by 2cm) in a chlorpyrifos water suspension for 1 minute, vertically taking out, inclining at 50 degrees, and standing for 2 minutes;
3) then placing the cover glass or the peanut leaves obtained in the step (2) in 100mL petroleum ether for 10 minutes, and then detecting the content of chlorpyrifos in the petroleum ether, namely the attachment amount by using an ultraviolet spectrophotometer;
4) the rate of increase (%) of chlorpyrifos attachment (the amount of chlorpyrifos alone attached with the loss-controlling agent)/the amount of chlorpyrifos with the loss-controlling agent × 100%. Influence of (2)
The data obtained are shown in Table 1.
TABLE 1
Figure BDA0002384633030000051

Claims (7)

1. A magnetic pesticide loss control agent is characterized by being prepared by compounding attapulgite, alkali/ammonium persulfate modified weathered coal; the preparation method of the magnetic pesticide loss control agent comprises the following steps:
step 1): mixing quicklime and weathered coal according to the ratio of (1-3): (3-5), adding the mixture into water to prepare a suspension with the initial concentration of 50-100g/L, and stirring at normal temperature for 30-50 minutes to react quicklime with the water; the mass content of humic acid in the weathered coal is 20-40%;
step 2): uniformly mixing ammonium persulfate, ferroferric oxide and attapulgite according to the mass ratio of (1-2) to (6-9);
step 3): adding the mixture obtained in the step 2) into the suspension obtained in the step 1) at the concentration of 50-80g/L, and stirring for 10-30 minutes at the temperature of 30-80 ℃;
step 4): filtering the suspension obtained in the step 3), drying the filter residue at 30-80 ℃ to constant weight, and crushing to 500-mesh and 1000-mesh to obtain the magnetic pesticide loss control agent.
2. The magnetic pesticide loss control agent of claim 1, wherein the fineness of the quicklime in the step 1) is 50-100 meshes; the fineness of the weathered coal is 50-100 meshes.
3. The magnetic pesticide loss control agent as defined in claim 1, wherein the rotation speed of the stirring in the step 1) is 100-200 rpm.
4. The loss control agent for magnetic pesticides as claimed in claim 1, wherein the fineness of ammonium persulfate in step 2) is 50-100 mesh; the fineness of the ferroferric oxide is 50-100 meshes; the fineness of the attapulgite is 50-100 meshes.
5. The magnetic pesticide loss control agent as defined in claim 1, wherein the rotation speed of the stirring in the step 3) is 100-200 rpm.
6. The application of the magnetic pesticide loss control agent as claimed in claim 1, wherein the magnetic pesticide loss control agent is added into pesticide in a proportion of 5-15% by mass to obtain loss control type pesticide.
7. The use as claimed in claim 6, wherein the pesticides are in the form of suspensions, dusts, wettable powders, tablets or granules.
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CN111134115B (en) * 2019-12-24 2021-08-10 东华大学 Pesticide retention agent and preparation method thereof
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CN103355291A (en) * 2013-05-10 2013-10-23 中国科学院合肥物质科学研究院 Novel efficient method for improving adhesive capability of pesticide
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CN105837340A (en) * 2016-05-18 2016-08-10 凤台县农之梦家庭农场有限公司 Rainwater-resistant fertilizer for plants in hill area and preparation method of rainwater-resistant fertilizer
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CN108704617B (en) * 2018-05-16 2019-10-25 西安科技大学 Humic acid/attapulgite magnetic composite material preparation method and applications
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