CN114560972B - Ecological environment-friendly pesticide slow-release material and preparation method and application thereof - Google Patents
Ecological environment-friendly pesticide slow-release material and preparation method and application thereof Download PDFInfo
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- CN114560972B CN114560972B CN202210087961.5A CN202210087961A CN114560972B CN 114560972 B CN114560972 B CN 114560972B CN 202210087961 A CN202210087961 A CN 202210087961A CN 114560972 B CN114560972 B CN 114560972B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/707—1,2,3- or 1,2,4-triazines; Hydrogenated 1,2,3- or 1,2,4-triazines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- General Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Wood Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Agronomy & Crop Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pest Control & Pesticides (AREA)
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Abstract
The invention discloses an ecological environment-friendly pesticide slow-release material, which comprises the following raw materials: 0.2-8 parts of starch, 5.5-39.5 parts of grafting monomer, 2-12 parts of sodium hydroxide, 0.3-5.4 parts of diacetone acrylamide, 0.25-7.5 parts of molecular weight regulator and 50-90 parts of water; mixing the starch, sodium hydroxide and water to gelatinize, mixing with other components, and processing 60 And (5) performing Co gamma ray radiation treatment to obtain the product. The product has high purity and no initiator residue; because starch is introduced as a high molecular framework, the hydrophilic, film-forming and biological degradability are good, and the material is an environment-friendly pesticide slow-release material. The invention also discloses a preparation method and application of the ecological environment-friendly pesticide slow-release material, and the preparation method is simple and has good application effect.
Description
Technical Field
The invention belongs to the technical field of pesticide slow-release materials, and particularly relates to an ecological environment-friendly pesticide slow-release material, a preparation method and application thereof.
Background
The pesticide usage amount in China is the first in the world, but the effective utilization rate of the pesticide is low. The pesticide is loaded by the pesticide slow-release material, which is an effective technical means for improving the utilization rate of the pesticide, can save the use cost of the pesticide and reduce the environmental hazard caused by pesticide loss. At present, pesticide slow-release materials in China can be divided into inorganic substances and organic substances, the inorganic substances have the characteristics of low cost and abundant raw materials, but have the defects of no degradation, large dosage and the like, and the mineral inorganic salt slow-release materials such as alumina, bentonite, zeolite, diatomite or (heavy) metal residues have the risks of poisoning human bodies and polluting the environment. The synthetic inorganic salt slow-release material has complex synthesis process and also has the risks of poisoning human bodies and polluting the environment due to (heavy) metal residues. In the organic slow release materials, natural polymer slow release materials are abundant in sources, but cannot be directly applied generally, the slow release performance is not outstanding, and synthetic polymers or natural polymer modification are synthesized by adopting a conventional chemical synthesis method, so that the synthesis conditions are severe, and the process is complex.
In the application method of pesticide slow-release material in China, the slow-release material and pesticide are generally adopted to be processed into a mixed preparation form for direct use after physical mixing adsorption or chemical bonding reaction in the present stage, the processing process is complex, the processes of grinding, crushing, mixing, drying and the like are needed, dust and air pollution exist in the production process, the toxic effect is caused on human body, and the production cost is increased. Therefore, the pesticide slow release agent is developing towards better economic benefit, social benefit and ecological benefit, and the biodegradable or bioabsorbable pesticide slow release material is an important research direction nowadays.
Disclosure of Invention
The invention aims to solve the technical problems and overcome the defects in the background art, and provides a bio-based active polymer which does not contain chemical initiator residues and is an ecological environment-friendly pesticide slow-release material with degradable products, namely a starch grafting functional group, and a preparation method and a use method with simple production process and high production efficiency.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
an ecological environment-friendly pesticide slow release material comprises the following raw materials: 0.2-8 parts of starch, 5.5-39.5 parts of grafting monomer, 2-12 parts of sodium hydroxide, 0.3-5.4 parts of diacetone acrylamide, 0.25-7.5 parts of molecular weight regulator and 50-90 parts of water; the ecological environment-friendly pesticide slow release material is prepared by mixing the starch, sodium hydroxide and water to gelatinize the starch, mixing the gelatinized starch with other components, and then passing through 60 And (5) performing Co gamma ray radiation treatment to obtain the product.
The above ecological environment-friendly pesticide slow release material is preferably selected from starch contained in various crops, specifically any one or more of potato starch, corn starch, cereal starch, konjak starch and sweet potato starch.
Preferably, the molecular weight regulator is any one or more of sodium hypophosphite, isopropanol, sodium formate, mercaptan, sodium methallyl sulfonate and sodium bisulphite, and is an organic or inorganic substance capable of providing chain transfer termination or polymerization inhibition free radicals.
Preferably, the grafting monomer comprises any one or more of acrylic acid, hydroxypropyl acrylate, N-methylolacrylamide, acrylamide, methacrylic acid and methyl acrylate. Wherein, acrylic acid, hydroxypropyl acrylate and N-methylolacrylamide respectively contain functional groups such as carboxyl, ester group, amino, methylol and the like; but may also be one or more copolymerizable monomers containing other functional group monomers of ethylenic origin, such as acrylamide, methacrylic acid, methyl acrylate or other water-soluble or water-insoluble copolymerizable other ethylenic monomers.
More preferably, the grafting monomer comprises 5-30 parts by weight of acrylic acid, 0.35-5 parts by weight of hydroxypropyl acrylate and 0.15-4.5 parts by weight of N-methylolacrylamide, which respectively contain functional groups of carboxyl, ester, amino and methylol.
In addition, the diacetone acrylamide is a monomer containing double bonds and amino active hydrogen, the monomer directly participates in starch graft polymerization to form a long-chain polymer containing carbonyl, and the carbonyl of the monomer can be dehydrated with the amino active hydrogen of adipic dihydrazide at normal temperature to generate a three-dimensional network polymer which is insoluble in water and can be swelled in a hydrophilic way, and the diacetone acrylamide is an indispensable functional monomer in the invention.
Based on a general inventive concept, the invention also provides a preparation method of the ecological environment-friendly pesticide slow-release material, which is prepared by adopting raw materials such as starch, comonomer and the like, controlling radiation dosage under high-energy gamma-ray radiation and adopting a radiation grafting polymerization method, and specifically comprises the following steps:
(1) Dissolving sodium hydroxide with water, adding starch for gelatinization, adding acrylic acid, and finally adding hydroxypropyl acrylate, N-methylolacrylamide, diacetone acrylamide and molecular weight regulator, stirring, dispersing and dissolving to obtain a homogeneous solution;
(2) Placing the homogeneous solution in 60 Performing radiation polymerization in a Co gamma-ray radiation field, and controlling the radiation dose to be 0.2-100kGy after the polymerization is completed, thereby obtaining the ecological environment-friendly pesticide slow-release materialStarch grafted with bio-based polymers of multifunctional groups (amino, ester, carboxyl, hydroxy (methyl), carbonyl).
In the above preparation method, preferably, in the step (1), the gelatinization is performed under conditions of 20 to 30 ℃ (room temperature), and alkalinity (which is achieved by using alkalinity provided by a raw material sodium hydroxide solution); in step (2), the radiation dose is controlled to be in the range of 5-10kGy.
Based on a general inventive concept, the invention also provides an application of the ecological environment-friendly pesticide slow release material in preparing slow release pesticide.
Preferably, the method of application is selected from any one of the following:
the method comprises the following steps: dissolving the ecological environment-friendly pesticide slow-release material in water, adding pesticide, stirring for dispersion or dissolution, adding adipic dihydrazide, stirring for dissolution to form suspension or homogeneous solution, and obtaining slow-release pesticide aqua, so that crops can be sprayed for disinsection and sterilization, and an excellent pesticide slow-release effect can be exerted;
the second method is as follows: mixing the ecological environment-friendly pesticide slow-release material, the pesticide and adipic dihydrazide, and obtaining slow-release pesticide wettable powder through drying reaction and crushing processing.
More preferably, the mass ratio of the ecological environment-friendly pesticide slow-release material to the pesticide is 0.21-2.1:2, and the dosage of the adipic acid dihydrazide is 0.1-2.0 times of the mass of diacetone acrylamide contained in the ecological environment-friendly pesticide slow-release material.
Compared with the prior art, the invention has the beneficial effects that:
1. the ecological environment-friendly pesticide slow-release material has high product purity and no initiator residue; because starch is introduced as a high molecular framework, the hydrophilic, film-forming and biological degradability are good, and the material is an environment-friendly pesticide slow-release material.
2. The preparation method of the invention does not need to add an initiator, has simple radiation preparation process, does not need heating and stirring for reaction, is to initiate polymerization by radiation at normal temperature, has lower cost, saves energy and protects environment.
3. The application of the invention takes the ecological environment-friendly pesticide slow-release material and adipic dihydrazide as a pesticide slow-release bi-component system, the slow-release bi-component system can be condensed, dehydrated and crosslinked at normal temperature after water volatilizes, a three-dimensional network polymer can be formed, the network three-dimensional space of the slow-release material can store pesticides, the polymer chains of the network space contain amino groups, ester groups, carboxyl groups, hydroxyl (methyl) groups, carbonyl groups and other electron donors or functional groups of acceptors and the like, and the functional groups and the groups in pesticide molecules form a ligand, so that the slow-release effect of the pesticides can be excellent, and the insecticidal and bactericidal effects of the sprayed crops are good.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the variation of pymetrozine concentration in various water bodies in example 1;
FIG. 2 is a graph showing the percent pymetrozine released at various times in example 1;
FIG. 3 is a graph showing the variation of pymetrozine concentration in various water bodies in example 2;
FIG. 4 is a graph showing the percent pymetrozine released at various times in example 2;
FIG. 5 is a graph showing the variation of pymetrozine concentration in various water bodies in example 3;
FIG. 6 is a graph showing the percentage change in pymetrozine release at various times in example 4.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1:
a preparation method of an ecological environment-friendly pesticide slow-release material-starch grafted multifunctional group bio-based active polymer comprises the following steps:
(1) The raw materials are prepared according to the following mass:
table 1: raw material composition of example 1
(2) According to the raw material formulation, sodium hydroxide is first dissolved in water in a vessel, kept at room temperature (25 ℃), and then starch is added to gelatinize it. Adding acrylic acid, and finally adding hydroxypropyl acrylate, N-methylolacrylamide, diacetone acrylamide and sodium hypophosphite, stirring, dispersing and dissolving to obtain a homogeneous solution;
(3) Placing the above homogeneous solution 60 Performing radiation polymerization in a Co gamma-ray radiation field, and controlling the radiation dose to 5kGy after the polymerization is completed, so as to obtain the water-soluble pesticide slow-release material, namely the starch bio-based grafted multifunctional group bio-based active polymer.
The application of the ecological environment-friendly pesticide slow release material prepared by the embodiment in preparing slow release pesticide is as follows:
dissolving the above radiation synthesized pesticide slow release material, namely the water-soluble starch grafted multifunctional group bio-based active polymer, in water, adding into the powder solid pesticide, stirring to disperse or dissolve, then adding adipic acid dihydrazide, stirring to dissolve (or adding starch and attapulgite), forming suspension or homogeneous solution.
The test method is as follows:
2.000g of the above suspension or homogeneous solution was weighed and 1 test sample was uniformly coated on a 400cm2 glass sheet, and each sample was repeated 3 times. The sample was dried in an oven at 40 c for 1.5h and then all immersed in a container containing 1300ml distilled water, the system was thermostated at 20 c and the pesticide was gradually released from the glass flakes into the water and the solution with the dissolved pesticide was removed at different times to be tested. According to GB/T35670-2017 pymetrozine water dispersible granule, high performance liquid chromatography is adopted to detect and analyze the pymetrozine content.
To illustrate the benefits of this patent, we make a comparison with the control in the examples:
the control samples were 3 in total:
control 1, blank, no slow release material; a control sample 2, which uses starch as a slow-release material; in the control sample 3, attapulgite is used as a slow release material.
Treatment samples 2:
the sample 1 is treated, the starch bio-based polymer grafted with the multifunctional group and synthesized by the radiation is taken as a pesticide slow release material, and 0.8g of 2.5% adipic acid dihydrazide aqueous solution is added.
Sample 2 is treated, the starch bio-based polymer grafted with the multifunctional group and synthesized by the radiation is taken as a pesticide slow release material, and 1.6g of 2.5% adipic acid dihydrazide aqueous solution is added.
The composition of each sample is shown in Table 2 below:
table 2: example 1 composition of each sample tested
The test analysis results are shown in fig. 1 and 2 below. As is evident from fig. 1 and 2, the pesticide slow-release material of the present invention has obvious slow-release effect, and is superior to that of a control sample. We only describe 2 time points, 5 minutes later, the percent pymetrozine release for treatment 1 and 2 was 10-20% and the control was greater than 50%, with the blank being greater than 90%. At 20 minutes, the release percentages of treatment 1 and treatment 2 were 51-62%, while the control was greater than 85%, and the blank had been substantially completely released, reaching more than 99%.
Example 2:
the procedure, application, test method and other conditions of the preparation method were as in example 1, except that the amounts of the raw material components were changed to 8kGy based on example 1.
(1) The raw materials are prepared as follows:
table 3: raw material composition of example 2
(2) The composition of each sample is shown in Table 4 below:
table 4: example 2 composition of each sample tested
The test analysis results are shown in fig. 3 and 4. As can be seen from fig. 3, fig. 4 and fig. 1 and fig. 2, the pesticide slow-release material of the present invention has obvious slow-release effect. At 5 minutes of this treatment, the percent pymetrozine release was 17.6%, while the control was greater than 50%, with the blank being greater than 90%. The percent of pymetrozine released by this treatment sample at 20 minutes was 69.1%, while the control sample was greater than 85%, with the blank having been substantially completely released, reaching over 99%.
Example 3:
the procedure, application, test method and other conditions of the preparation method were as in example 1, except that the amounts of the raw material components were changed to 10kGy based on example 1.
(1) The raw materials are prepared as follows:
table 5: raw material composition of example 3
(2) The composition of each sample is shown in Table 6 below:
table 6: example 3 composition of each sample tested
The test analysis results are shown in fig. 5 and 6. As can be seen by comparing fig. 5 and fig. 6 with fig. 1 and fig. 2, the pesticide slow-release material of the present invention has obvious slow-release effect. At 5 minutes of this treatment, the pymetrozine release percentage treatment was 29% and the control was greater than 50%, with the blank being greater than 90%; at 20 minutes, the percent release was 57.4% and the control was greater than 85% with the blank having been substantially completely released, reaching over 99%.
Claims (4)
1. The application of the ecological environment-friendly pesticide slow release material in preparing the slow release pesticide is characterized in that the application method is selected from any one of the following:
the method comprises the following steps: dissolving the ecological environment-friendly pesticide slow-release material in water, adding the pesticide, stirring for dispersion or dissolution, and then adding adipic dihydrazide, stirring for dissolution to form suspension or homogeneous solution, thus obtaining slow-release pesticide aqua;
the second method is as follows: mixing the ecological environment-friendly pesticide slow-release material, pesticide and adipic dihydrazide, and obtaining slow-release pesticide wettable powder through drying reaction and crushing processing;
the raw materials of the ecological environment-friendly pesticide slow-release material comprise the following components: 0.2-8 parts of starch, 5.5-39.5 parts of grafting monomer, 2-12 parts of sodium hydroxide, 0.3-5.4 parts of diacetone acrylamide, 0.25-7.5 parts of molecular weight regulator and 50-90 parts of water; the grafting monomer comprises 5-30 parts by weight of acrylic acid, 0.35-5 parts by weight of hydroxypropyl acrylate and 0.15-4.5 parts by weight of N-methylolacrylamide;
the ecological environment-friendly pesticide slow release material is prepared by mixing the starch, sodium hydroxide and water to gelatinize the starch, mixing the gelatinized starch with other components, and then passing through 60 After Co gamma-ray radiation treatmentObtained.
2. The application of the ecological environment-friendly pesticide slow release material in preparing the slow release pesticide according to claim 1, wherein the starch is any one or more of cereal starch, konjak starch and sweet potato starch.
3. The application of the ecological environment-friendly pesticide slow release material in preparing slow release pesticides according to claim 1, wherein the molecular weight regulator is any one or more of sodium hypophosphite, isopropanol, sodium formate, mercaptan, sodium methallyl sulfonate and sodium bisulphite.
4. The application of the ecological environment-friendly pesticide slow release material in preparing the slow release pesticide according to claim 1, wherein the mass ratio of the ecological environment-friendly pesticide slow release material to the pesticide is 0.21-2.1:2, and the dosage of adipic acid dihydrazide is 0.1-2.0 times of the mass of diacetone acrylamide contained in the ecological environment-friendly pesticide slow release material.
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CN101280044A (en) * | 2008-05-29 | 2008-10-08 | 四川师范大学 | Biodegradable agricultural high-absorbent resin and preparation thereof |
CN101314627A (en) * | 2008-06-04 | 2008-12-03 | 中国农业大学 | Film-forming agent for seed clothing sheet and preparation method thereof |
CN103665702A (en) * | 2012-09-13 | 2014-03-26 | 何诚慧 | Seed coating with water absorbing function and preparation method thereof |
CN109776730A (en) * | 2019-03-15 | 2019-05-21 | 贵州大学 | A kind of environmentally friendly water-loss reducer of soil and preparation method with slow-release function |
Non-Patent Citations (1)
Title |
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利用60Coγ辐射聚合技术研制淀粉型农用高吸水材料;王庆军等;《核技术》;第26卷(第4期);第311-314页 * |
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