CN114557351B - Cyclodextrin derivative-based seed coating material and preparation method and application thereof - Google Patents
Cyclodextrin derivative-based seed coating material and preparation method and application thereof Download PDFInfo
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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
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/06—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings
- A01N43/12—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings condensed with a carbocyclic ring
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01C—PLANTING; SOWING; FERTILISING
- A01C1/00—Apparatus, or methods of use thereof, for testing or treating seed, roots, or the like, prior to sowing or planting
- A01C1/06—Coating or dressing seed
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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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
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- 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
- A01N25/32—Ingredients for reducing the noxious effect of the active substances to organisms other than pests, e.g. toxicity reducing compositions, self-destructing compositions
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N45/00—Biocides, pest repellants or attractants, or plant growth regulators, containing compounds having three or more carbocyclic rings condensed among themselves, at least one ring not being a six-membered ring
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/18—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, directly attached to a heterocyclic or cycloaliphatic ring
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- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
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- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/22—O-Aryl or S-Aryl esters 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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/14—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing aromatic radicals
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N61/00—Biocides, pest repellants or attractants, or plant growth regulators containing substances of unknown or undetermined composition, e.g. substances characterised only by the mode of action
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
The invention belongs to the technical field of seed coating, and relates to a preparation method of a cyclodextrin derivative-based seed coating material, wherein the cyclodextrin derivative-based seed coating material comprises cyclodextrin derivative gel and ethylcellulose solution; preparation of cyclodextrin derivative gel: preparing beta-cyclodextrin derivative dissolution liquid, and then adding humate and urea into the beta-cyclodextrin derivative dissolution liquid to obtain mixed liquid A; dissolving gibberellin, pesticide and bactericide in water to obtain a mixed solution B; adding the mixed solution A into the mixed solution B, and adding benzoic acid, an initiator and a cross-linking agent to obtain gel; washing and drying the gel to obtain cyclodextrin derivative gel; preparation of ethylcellulose solution: dissolving ethyl cellulose and lactic acid into ethanol solution, and stirring until the ethyl cellulose and lactic acid are completely dissolved to obtain ethyl cellulose solution. Solves the problems of active ingredient loss and environmental pollution caused by poor indexes such as seed coating agent viscosity, pesticide stability and the like.
Description
Technical Field
The invention belongs to the technical field of seed coating, and particularly relates to a cyclodextrin derivative-based seed coating material, and a preparation method and application thereof.
Background
The seed coating is a new technology for seed treatment, which utilizes the colloid stabilization principle and the high polymer film forming principle to coat a layer of film which is quite thin, uniform in thickness and permeable and breathable on the surface of the seed. The seed coating can only be absorbed and expanded in soil without being dissolved when meeting water, so that seed coating substances such as medicines and micro-fertilizers can be gradually released, the medicines and fertilizer effects can continuously play a role, the seed quality is improved, the application times of the medicines and the fertilizer are reduced, and the effects of reducing the production cost, killing insects, preventing diseases, promoting growth and the like are achieved.
There is a certain problem in the current seed coating agent used in China. Firstly, the seed coating agent generally contains pesticides, which inevitably causes phytotoxicity to seeds, and is unfavorable for the maximum life substitution of the seeds. Meanwhile, the ecological problems of pesticide residue, environmental pollution and the like are easily caused. Secondly, the coating film of the seed coating agent is easy to dissolve in water, and active ingredients are easy to run off. Meanwhile, the indexes such as viscosity and stability of the seed coating agent are poor, so that the seed coating agent falls off seriously, and the effects of preventing diseases, controlling insects and increasing yield are greatly reduced.
Therefore, it is necessary to develop a mulberry seed coating material having high film-forming strength, water absorption, water resistance and chemical stability.
Disclosure of Invention
The invention aims to provide a cyclodextrin derivative-based seed coating material, a preparation method and application thereof, and solves the problems of active ingredient loss and environmental pollution caused by poor indexes such as seed coating agent viscosity, pesticide stability and the like.
The invention is realized by the following technical scheme:
a method of preparing a cyclodextrin derivative-based seed coating material comprising a cyclodextrin derivative gel as an outer layer film and an ethylcellulose solution as an inner layer film;
the cyclodextrin derivative gel is prepared from the following raw materials in parts by mass:
1) Dissolving 30-50 parts of beta-cyclodextrin derivative in 100-150 parts of distilled water, stirring at 30-35 ℃ to obtain beta-cyclodextrin derivative solution, adding humate solution and urea into the beta-cyclodextrin derivative solution, and stirring to obtain mixed solution A;
2) Dissolving 1-2 parts of gibberellin, 3-5 parts of pesticide and 3-5 parts of bactericide in 10-20 parts of distilled water, and fully stirring at 15-30 ℃ to obtain a mixed solution B;
3) Adding the mixed solution B into the mixed solution A, stirring at 30-35 ℃, introducing nitrogen after the solution is uniformly stabilized, deoxidizing, adding 5 parts of neutralized benzoic acid, an initiator and a cross-linking agent into the mixed solution A, heating to 40-50 ℃ and reacting for 0.5-1h to obtain gel;
4) Washing and drying the gel to constant weight, and crushing to obtain cyclodextrin derivative gel;
the preparation of the ethylcellulose solution comprises the following steps:
and (2) dissolving the ethyl cellulose and the lactic acid into an ethanol solution according to the mass ratio of (2-3), and stirring until the ethyl cellulose and the lactic acid are completely dissolved to obtain an ethyl cellulose solution.
Further, the beta-cyclodextrin derivative in the step 1) is hydroxyethyl-beta-cyclodextrin, hydroxypropyl-beta-cyclodextrin or methylated-beta-cyclodextrin.
In the step 1), the mass ratio of the benzoic acid to the beta-cyclodextrin derivative to the humate solution to the urea is 1 (6-10) (0.6-0.8) (0.2-0.6).
In the step 3), the mass ratio of the benzoic acid to the initiator to the cross-linking agent is 1 (0.2-0.4) to 0.2-0.4.
Further, in the step 1), the stirring time for preparing the beta-cyclodextrin derivative solution is 30-35min, and the stirring time for preparing the mixed solution A is 20-25min;
in the step 2), the stirring time is 15-20min.
Further, in said step 2), the insecticide comprises methyl parathion, carbofuran or carbaryl;
the bactericide comprises carbendazim or trimethoprim.
Further, in the step 3), the initiator adopts potassium persulfate, and the crosslinking agent adopts N, N-methylene bisacrylamide;
in the step 3), the neutralization degree of the benzoic acid is 60-70%.
Further, in the step 4), distilled water is used for washing, and a constant-temperature drying oven is adopted for drying, wherein the temperature is 45-55 ℃.
The invention also discloses a cyclodextrin derivative-based seed coating material prepared by the preparation method, which comprises an inner coating and an outer coating, wherein the inner coating is formed by ethyl cellulose solution, and the outer coating is formed by cyclodextrin derivative gel layers.
The invention also discloses application of the cyclodextrin derivative-based seed coating material, which comprises the following steps:
uniformly spraying an ethyl cellulose solution on the surface of the seeds in a spray mode, drying, and repeating for a plurality of times to form an inner coating on the surface of the mulberry seeds by the ethyl cellulose;
and (3) dissolving the cyclodextrin derivative gel, uniformly adhering the cyclodextrin derivative gel on the inner coating film in the form of atomized water, and drying and repeating the process for a plurality of times to obtain the cyclodextrin derivative-based seed coating film.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a preparation method of cyclodextrin derivative-based seed coating material, which comprises the steps of firstly preparing beta-cyclodextrin derivative solution and mixed solution formed by pesticide molecules, and forming a compound by partially or completely embedding the pesticide molecules into cyclodextrin derivative molecular cavities with cavities on the structure through non-covalent action. By utilizing the inclusion performance of the cyclodextrin derivative, the cyclodextrin derivative is used for clathrating pesticide molecules to form cyclodextrin derivative gel, then the seed is used as an inner core, the ethyl cellulose is used as an inner layer coating, and the cyclodextrin derivative gel is used as an outer layer coating. The ethyl cellulose is used for wrapping seeds, firstly, the ethyl cellulose has film forming property, secondly, the slow release effect of the ethyl cellulose enables the drug effect of the outer layer to be continuously released to the seeds, and the premature occurrence of some water-soluble drugs is avoided; and thirdly, the ethyl cellulose can be used as a stabilizer and a water-retaining agent, so that certain water is stored for seeds, seed germination is facilitated, and the ethyl cellulose is better in film forming property and more stable in viscosity when being singly used compared with the mixture. The inclusion compound formed by the cyclodextrin and the pesticide molecules can play roles in protecting, stabilizing, solubilizing the pesticide molecules, selecting oriented molecules and the like. And the cyclodextrin derivative improves and enhances the inclusion compound forming property of the cyclodextrin. For example, cyclodextrin derivatives can stabilize the active ingredients such as pesticides and bactericides, and can prolong the action time of the active ingredients by controlling the slow release of the active ingredients, reduce the dosage and improve the economic benefit. In addition, the cyclodextrin derivative has good water solubility, is nontoxic and easy to biodegrade, is not absorbed by soil, and cannot be detained in the soil and other mediums to cause secondary pollution. The cyclodextrin derivative gel formed by the cyclodextrin derivative hydrophobic cavity can desorb the hydrophobic pesticide adsorbed by soil organic matters and reduce pesticide residues. Humic acid can increase the absorption of seeds to moisture and nutrient substances in soil, and the humic acid can change the growth condition of the seeds so as to enhance the stress resistance of the seeds. In addition, in the aqueous solution containing humic acid, the cyclodextrin can promote the generation of photo-induced free radicals and has an inclusion effect on the photo-induced free radicals, and the cyclodextrin hydrophobic cavity can promote the photo-degradation reaction of the embedded free radicals to initiate the residual pesticide, so that the environment is protected.
The invention also discloses an application of the cyclodextrin derivative-based seed coating material, an ethyl cellulose solution is sprayed on the surface of a seed in a spray mode to form a film, the film has certain viscosity, and then cyclodextrin derivative gel is converted into an aerosol form through atomization to be deposited and adhered on an ethyl cellulose layer, and the ethyl cellulose layer also has a tackifying effect, so that the medicine contained in the outer layer can be more firmly and uniformly coated on the outer layer of the seed.
Detailed Description
The invention discloses a preparation method of a cyclodextrin derivative-based seed coating material, which comprises cyclodextrin derivative gel serving as an outer layer film and ethyl cellulose solution serving as an inner layer film;
the cyclodextrin derivative gel is prepared from the following raw materials in parts by mass:
1) Dissolving 30-50 parts of beta-cyclodextrin derivative in 100-150 parts of distilled water, stirring for 30-35min at 30-35 ℃ to obtain beta-cyclodextrin derivative solution, adding potassium humate solution and urea into the beta-cyclodextrin derivative solution, and stirring for 20-25min to obtain mixed solution A;
wherein the beta-cyclodextrin derivative is hydroxyethyl-beta-cyclodextrin, hydroxypropyl-beta-cyclodextrin, or methylated-beta-cyclodextrin.
The mass ratio of benzoic acid to beta-cyclodextrin derivative carboxymethyl starch to potassium humate solution to urea is 1 (6-10) (0.6-0.8) (0.2-0.6).
2) Dissolving 1-2 parts of gibberellin, 3-5 parts of pesticide and 3-5 parts of bactericide in 10-20 parts of distilled water, and fully stirring at 15-30 ℃ for 15-20min to obtain a mixed solution B; wherein the pesticide comprises methyl parathion, carbofuran and carbaryl. The bactericide comprises carbendazim and trimethoprim.
3) Adding the mixed solution B into the mixed solution A, stirring at 30-35 ℃, introducing nitrogen after the solution is uniformly stabilized, deoxidizing, adding 5 parts of neutralized benzoic acid, an initiator and a cross-linking agent into the mixed solution A, heating to 40-50 ℃ and reacting for 0.5-1h to obtain gel;
wherein, the initiator adopts potassium persulfate, and the cross-linking agent adopts N, N-methylene bisacrylamide.
The mass ratio of the benzoic acid to the initiator to the cross-linking agent is 1 (0.2-0.4), and the neutralization degree of the benzoic acid is 60-70%.
4) Washing the gel with distilled water, drying in a constant temperature drying oven at 45-55deg.C to constant weight, and pulverizing with pulverizer to obtain cyclodextrin derivative gel.
The preparation of the ethylcellulose solution comprises the following steps:
the mass ratio of the ethyl cellulose to the lactic acid is (2-3): 1 into 70% ethanol solution to prepare 3.5wt% mixed solution, and magnetically stirring until the ethyl cellulose and the lactic acid are completely dissolved to obtain ethyl cellulose solution.
The invention will now be described in further detail with reference to specific examples and figures, which are intended to illustrate, but not to limit, the invention.
Example 1
The invention discloses a preparation method of a cyclodextrin derivative-based seed coating material, which comprises cyclodextrin derivative gel and ethylcellulose solution;
the preparation of the cyclodextrin derivative gel layer comprises the following steps:
1) Dissolving 30 parts of hydroxyethyl-beta-cyclodextrin in 100 parts of distilled water, stirring for 30min at 30 ℃ to obtain hydroxyethyl-beta-cyclodextrin solution, adding 3 parts of potassium humate solution and 1 part of urea into the hydroxyethyl-beta-cyclodextrin solution, and stirring for 20-25min to obtain mixed solution A;
2) 1 part of gibberellin, 3 parts of methyl parathion and 3 parts of carbendazim are taken and dissolved in 10 parts of distilled water, and fully stirred for 15min at 15 ℃ to obtain a mixed solution B;
3) Adding the mixed solution B into the mixed solution A, stirring at 30 ℃, introducing nitrogen after the solution is uniformly stabilized, deoxidizing, adding 5 parts of benzoic acid with the neutralization degree of 60%, 1 part of potassium persulfate and 1 part of N, N-methylene bisacrylamide into the mixed solution A, heating to 40 ℃, and reacting for 0.5h to obtain the gel.
4) Washing the gel with distilled water, drying in a constant temperature drying oven at 45deg.C to constant weight, and pulverizing with pulverizer to obtain cyclodextrin derivative gel.
The preparation of the ethylcellulose solution comprises the following steps:
dissolving ethyl cellulose and lactic acid into 70% ethanol solution according to the mass ratio of 2:1 to prepare 3.5wt% mixed solution, and magnetically stirring until the ethyl cellulose and lactic acid are completely dissolved to obtain ethyl cellulose solution.
Example 2
The invention discloses a preparation method of a cyclodextrin derivative-based seed coating material, which comprises cyclodextrin derivative gel and ethylcellulose solution;
the preparation of the cyclodextrin derivative gel layer comprises the following steps:
1) Dissolving 50 parts of hydroxypropyl-beta-cyclodextrin in 150 parts of distilled water, stirring at 35 ℃ for 35min to obtain hydroxypropyl-beta-cyclodextrin solution, adding 4 parts of potassium humate solution and 3 parts of urea into the hydroxypropyl-beta-cyclodextrin solution, and stirring for 25min to obtain mixed solution A;
2) 2 parts of gibberellin, 5 parts of carbofuran and 5 parts of trimethoprim are taken and dissolved in 20 parts of distilled water, and fully stirred for 20min at 30 ℃ to obtain a mixed solution B;
3) Adding the mixed solution B into the mixed solution A, stirring at 35 ℃, introducing nitrogen after the solution is uniformly stabilized, deoxidizing, adding 5 parts of benzoic acid with the neutralization degree of 70%, 2 parts of potassium persulfate and 2 parts of N, N-methylene bisacrylamide into the mixed solution A, heating to 50 ℃ and reacting for 1h to obtain gel;
4) Washing the gel with distilled water, drying in a constant temperature drying oven at 55deg.C to constant weight, and pulverizing with pulverizer to obtain cyclodextrin derivative gel.
The preparation of the ethylcellulose solution comprises the following steps:
dissolving ethyl cellulose and lactic acid into 70% ethanol solution according to the mass ratio of 3:1 to prepare 3.5wt% mixed solution, and magnetically stirring until the ethyl cellulose and lactic acid are completely dissolved to obtain ethyl cellulose solution.
Example 3
The invention discloses a preparation method of a cyclodextrin derivative-based seed coating material, which comprises cyclodextrin derivative gel and ethylcellulose solution;
the preparation of the cyclodextrin derivative gel layer comprises the following steps:
1) Dissolving 35 parts of methylation-beta-cyclodextrin in 120 parts of distilled water, stirring for 35min at 30 ℃ to obtain a methylation-beta-cyclodextrin solution, adding 3 parts of potassium humate solution and 3 parts of urea into the methylation-beta-cyclodextrin solution, and stirring for 25min to obtain a mixed solution A;
2) 1 part of gibberellin, 4 parts of carbaryl and 4 parts of carbendazim are taken and dissolved in 15 parts of distilled water, and fully stirred for 15min at 20 ℃ to obtain a mixed solution B;
3) Adding the mixed solution B into the mixed solution A, stirring at 30 ℃, introducing nitrogen after the solution is uniformly stabilized, deoxidizing, adding 5 parts of benzoic acid with the neutralization degree of 65%, 1 part of potassium persulfate and 2 parts of N, N-methylene bisacrylamide into the mixed solution A, heating to 45 ℃ and reacting for 0.5h to obtain gel;
4) Washing the gel with distilled water, drying in a constant temperature drying oven at 50deg.C to constant weight, and pulverizing with pulverizer to obtain cyclodextrin derivative gel.
The preparation of the ethylcellulose solution comprises the following steps:
dissolving ethyl cellulose and lactic acid into 70% ethanol solution according to the mass ratio of 3:1 to prepare 3.5wt% mixed solution, and magnetically stirring until the ethyl cellulose and lactic acid are completely dissolved to obtain ethyl cellulose solution.
Example 4
The invention discloses a preparation method of a cyclodextrin derivative-based seed coating material, which comprises cyclodextrin derivative gel and ethylcellulose solution;
the preparation of the cyclodextrin derivative gel layer comprises the following steps:
1) Dissolving 40 parts of hydroxyethyl-beta-cyclodextrin in 120 parts of distilled water, stirring for 35min at 35 ℃ to obtain hydroxyethyl-beta-cyclodextrin solution, adding 4 parts of potassium humate solution and 3 parts of urea into the hydroxyethyl-beta-cyclodextrin solution, and stirring for 20min to obtain mixed solution A;
2) 1 part of gibberellin, 5 parts of methyl parathion and 4 parts of carbendazim are taken and dissolved in 12 parts of distilled water, and fully stirred for 15min at 15 ℃ to obtain a mixed solution B;
3) Adding the mixed solution B into the mixed solution A, stirring at 30 ℃, introducing nitrogen after the solution is uniformly stabilized, deoxidizing, adding 5 parts of benzoic acid with the neutralization degree of 65%, 1 part of potassium persulfate and 2 parts of N, N-methylene bisacrylamide into the mixed solution A, heating to 45 ℃ and reacting for 0.5h to obtain gel;
4) Washing the gel with distilled water, drying in a constant temperature drying oven at 50deg.C to constant weight, and pulverizing with pulverizer to obtain cyclodextrin derivative gel.
The preparation of the ethylcellulose solution comprises the following steps:
dissolving ethyl cellulose and lactic acid into 70% ethanol solution according to the mass ratio of 2:1 to prepare 3.5wt% mixed solution, and magnetically stirring until the ethyl cellulose and lactic acid are completely dissolved to obtain ethyl cellulose solution.
Example 5
The invention discloses a preparation method of a cyclodextrin derivative-based seed coating material, which comprises cyclodextrin derivative gel and ethylcellulose solution;
the preparation of the cyclodextrin derivative gel layer comprises the following steps:
1) Dissolving 45 parts of hydroxypropyl-beta-cyclodextrin in 130 parts of distilled water, stirring for 30min at 35 ℃ to obtain hydroxypropyl-beta-cyclodextrin, adding 4 parts of potassium humate solution and 2 parts of urea into the hydroxypropyl-beta-cyclodextrin solution, and stirring for 20min to obtain a mixed solution A;
2) 1 part of gibberellin, 4 parts of carbofuran and 5 parts of carbendazim are taken and dissolved in 15 parts of distilled water, and fully stirred for 20min at 20 ℃ to obtain a mixed solution B;
3) Adding the mixed solution B into the mixed solution A, stirring at 30 ℃, introducing nitrogen after the solution is uniformly stabilized, deoxidizing, adding 5 parts of benzoic acid with the neutralization degree of 65%, 1 part of potassium persulfate and 2 parts of N, N-methylene bisacrylamide into the mixed solution A, heating to 45 ℃ and reacting for 0.5h to obtain gel;
4) Washing the gel with distilled water, drying in a constant temperature drying oven at 50deg.C to constant weight, and pulverizing with pulverizer to obtain cyclodextrin derivative gel.
The preparation of the ethylcellulose solution comprises the following steps:
dissolving ethyl cellulose and lactic acid into 70% ethanol solution according to the mass ratio of 3:1 to prepare 3.5wt% mixed solution, and magnetically stirring until the ethyl cellulose and lactic acid are completely dissolved to obtain ethyl cellulose solution.
Example 6
The invention discloses a preparation method of a cyclodextrin derivative-based seed coating material, which comprises cyclodextrin derivative gel and ethylcellulose solution;
the preparation of the cyclodextrin derivative gel layer comprises the following steps:
1) Dissolving 50 parts of methylation-beta-cyclodextrin in 130 parts of distilled water, stirring for 30min at 30 ℃ to obtain a methylation-beta-cyclodextrin solution, adding 4 parts of potassium humate solution and 3 parts of urea into the methylation-beta-cyclodextrin solution, and stirring for 20min to obtain a mixed solution A;
2) 1 part of gibberellin, 3 parts of carbaryl and 3 parts of trimethoprim are taken and dissolved in 15 parts of distilled water, and fully stirred for 15min at 15 ℃ to obtain a mixed solution B;
3) Adding the mixed solution B into the mixed solution A, stirring at 30 ℃, introducing nitrogen after the solution is uniformly stabilized, deoxidizing, adding 5 parts of benzoic acid with the neutralization degree of 60%, 2 parts of potassium persulfate and 1 part of N, N-methylene bisacrylamide into the mixed solution A, heating to 45 ℃ and reacting for 1h to obtain gel;
4) Washing the gel with distilled water, drying in a constant temperature drying oven at 50deg.C to constant weight, and pulverizing with pulverizer to obtain cyclodextrin derivative gel.
The preparation of the ethylcellulose solution comprises the following steps:
dissolving ethyl cellulose and lactic acid into 70% ethanol solution according to the mass ratio of 2:1 to prepare 3.5wt% mixed solution, and magnetically stirring until the ethyl cellulose and lactic acid are completely dissolved to obtain ethyl cellulose solution.
In order to characterize the effect of the cyclodextrin derivative-based seed coating film prepared by the invention, the seeds treated by the cyclodextrin derivative-based seed coating film are taken as an experimental group, the seeds soaked by distilled water are taken as a control group, the control group is placed in a culture dish with water absorbing paper, the water absorbing paper is kept moist, two groups of mulberry seeds are randomly sampled, 100 grains are respectively sampled, standard germination tests are carried out in a constant temperature incubator at 25 ℃, and the culture is carried out for 20 days, so that the germination rate, germination index, root length and root fresh weight of the mulberry seeds treated by the cyclodextrin derivative-based mulberry seed coating film are sampled and tested.
The experimental group was used as follows: uniformly spraying the dissolved ethyl cellulose on the surface of the mulberry seeds in a spray mode, and drying. Repeating for multiple times to form a coating with a certain thickness on the surface of the mulberry seed by the ethyl cellulose; uniformly adhering the crushed cyclodextrin derivative gel on mulberry seeds under the action of atomized water, and drying. Repeating for multiple times to obtain the cyclodextrin derivative-based mulberry seed coating film.
The mulberry seeds of the control group are fertilized and cultivated conventionally. The specific experimental results are shown in table 1 below.
TABLE 1 influence of Cyclodextrin derivative-based Mulberry seed coating film on the vigor level of Mulberry seeds
| Sample of | Germination rate/% | Germination index | Root length | Fresh weight of root |
| Example 1 | 96.2 | 6.65 | 2.54 | 6.23 |
| Example 2 | 95.97 | 6.45 | 2.48 | 5.91 |
| Example 3 | 95.83 | 6.35 | 2.40 | 5.78 |
| Example 4 | 96.02 | 6.49 | 2.50 | 6.04 |
| Example 5 | 96.14 | 6.53 | 2.52 | 6.17 |
| Example 6 | 95.87 | 6.42 | 2.44 | 5.89 |
| Control group | 86.5 | 4.08 | 2.14 | 3.04 |
As can be seen from Table 1, the germination rate, germination index and root length and root fresh weight of the mulberry seeds treated with the cyclodextrin derivative-based seed coating film were improved. Therefore, the cyclodextrin derivative-based seed coating film of the present invention is illustrated to stabilize the active ingredients and the nutritional ingredients of pesticides, thereby having a promoting effect on the germination of mulberry seeds and the growth of seedlings.
The present invention has been described in detail with reference to the above embodiments, and it should be understood by those skilled in the art that: modifications and equivalents may be made to the specific embodiments of the invention without departing from the spirit and scope of the invention, which are intended to be covered by the scope of the claims.
Claims (10)
1. A method for preparing a cyclodextrin derivative-based seed coating material, characterized in that the cyclodextrin derivative-based seed coating material comprises a cyclodextrin derivative gel as an outer layer film and an ethylcellulose solution as an inner layer film;
the cyclodextrin derivative gel is prepared from the following raw materials in parts by mass:
1) Dissolving 30-50 parts of beta-cyclodextrin derivative in 100-150 parts of distilled water, stirring at 30-35 ℃ to obtain beta-cyclodextrin derivative solution, adding humate solution and urea into the beta-cyclodextrin derivative solution, and stirring to obtain mixed solution A;
2) Dissolving 1-2 parts of gibberellin, 3-5 parts of pesticide and 3-5 parts of bactericide in 10-20 parts of distilled water, and fully stirring at 15-30 ℃ to obtain a mixed solution B;
3) Adding the mixed solution B into the mixed solution A, stirring at 30-35 ℃, introducing nitrogen after the solution is uniformly stabilized, deoxidizing, adding 5 parts of neutralized benzoic acid, an initiator and a cross-linking agent into the mixed solution A, heating to 40-50 ℃ and reacting for 0.5-1h to obtain gel;
4) Washing and drying the gel to constant weight, and crushing to obtain cyclodextrin derivative gel;
the preparation of the ethylcellulose solution comprises the following steps:
and (2) dissolving the ethyl cellulose and the lactic acid into an ethanol solution according to the mass ratio of (2-3), and stirring until the ethyl cellulose and the lactic acid are completely dissolved to obtain an ethyl cellulose solution.
2. The method for preparing a cyclodextrin derivative-based seed coating material according to claim 1, wherein the β -cyclodextrin derivative in step 1) is hydroxyethyl- β -cyclodextrin, hydroxypropyl- β -cyclodextrin or methylated- β -cyclodextrin.
3. The method for preparing the cyclodextrin derivative-based seed coating material according to claim 1, wherein the mass ratio of benzoic acid to beta-cyclodextrin derivative to humate solution to urea is 1 (6-10): 0.6-0.8): 0.2-0.6.
4. The method for preparing a cyclodextrin derivative-based seed coating material according to claim 1, wherein in the step 3), the mass ratio of benzoic acid, an initiator and a crosslinking agent is 1 (0.2-0.4): 0.2-0.4.
5. The method for preparing a cyclodextrin derivative-based seed coating material according to claim 1, wherein in the step 1), the stirring time for preparing the beta-cyclodextrin derivative-dissolved solution is 30-35min, and the stirring time for preparing the mixed solution a is 20-25min;
in the step 2), the stirring time is 15-20min.
6. The method for preparing a cyclodextrin derivative-based seed coating material according to claim 1, wherein in the step 2), the insecticide comprises methyl parathion, carbofuran or carbaryl;
the bactericide comprises carbendazim or trimethoprim.
7. The method for preparing a cyclodextrin derivative-based seed coating material according to claim 1, wherein in the step 3), the initiator is potassium persulfate, and the crosslinking agent is N, N-methylenebisacrylamide;
in the step 3), the neutralization degree of the benzoic acid is 60-70%.
8. The method for preparing a cyclodextrin derivative-based seed coating material according to claim 1, wherein in step 4), distilled water is used for washing, and a constant temperature drying oven is used for drying at 45-55 ℃.
9. A cyclodextrin derivative-based seed coating material prepared by the method of any one of claims 1 to 8, comprising an inner coating formed from an ethylcellulose solution and an outer coating formed from a cyclodextrin derivative gel layer.
10. Use of a cyclodextrin derivative-based seed coating material according to claim 9, comprising the steps of:
uniformly spraying an ethyl cellulose solution on the surface of the seeds in a spray mode, drying, and repeating for a plurality of times to form an inner coating on the surface of the mulberry seeds by the ethyl cellulose;
and (3) dissolving the cyclodextrin derivative gel, uniformly adhering the cyclodextrin derivative gel on the inner coating film in the form of atomized water, and drying and repeating the process for a plurality of times to obtain the cyclodextrin derivative-based seed coating film.
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| CN108812023A (en) * | 2018-06-21 | 2018-11-16 | 德宏正信实业股份有限公司 | The method for culturing seedlings of mulberry tree |
| CN108901547A (en) * | 2018-07-03 | 2018-11-30 | 覃选牛 | A kind of mulberry tree implantation methods |
| CN109111294A (en) * | 2018-10-24 | 2019-01-01 | 安文彬 | A kind of organic microbial complex ecological fertilizer and preparation method thereof |
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