CN115216103A - Functional liquid mulching film with fluorescence effect and mulching film laying method - Google Patents

Functional liquid mulching film with fluorescence effect and mulching film laying method Download PDF

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Publication number
CN115216103A
CN115216103A CN202210996692.4A CN202210996692A CN115216103A CN 115216103 A CN115216103 A CN 115216103A CN 202210996692 A CN202210996692 A CN 202210996692A CN 115216103 A CN115216103 A CN 115216103A
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Prior art keywords
mulching film
parts
agent
starch
solvent
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Chinese (zh)
Inventor
秦韵涵
刘乾
夏江
孙清松
孙孝敏
聂昌亮
张燕妮
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Runhan Shandong Ecological Technology Co ltd
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Runhan Shandong Ecological Technology Co ltd
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Priority to CN202210996692.4A priority Critical patent/CN115216103A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protecting plants
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protecting plants
    • A01G13/02—Protective coverings for plants; Coverings for the ground; Devices for laying-out or removing coverings
    • A01G13/0256—Ground coverings
    • 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
    • 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
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
    • A01N37/46—N-acyl derivatives
    • 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
    • A01N39/00—Biocides, pest repellants or attractants, or plant growth regulators containing aryloxy- or arylthio-aliphatic or cycloaliphatic compounds, containing the group or, e.g. phenoxyethylamine, phenylthio-acetonitrile, phenoxyacetone
    • A01N39/02—Aryloxy-carboxylic acids; Derivatives thereof
    • A01N39/04—Aryloxy-acetic acids; Derivatives thereof
    • 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
    • A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • 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
    • A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P13/00—Herbicides; Algicides
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P7/00—Arthropodicides
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/80—Soil conditioners
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protecting plants
    • A01G2013/004—Liquid mulch
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/04—Alginic acid; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02—Organic and inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/321—Phosphates
    • C08K2003/324—Alkali metal phosphate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/101—Esters; Ether-esters of monocarboxylic acids
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/15—Heterocyclic compounds having oxygen in the ring
    • C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
    • C08K5/1545—Six-membered rings
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    • C08K5/20—Carboxylic acid amides
    • C—CHEMISTRY; METALLURGY
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    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
    • C08K5/3432—Six-membered rings
    • C08K5/3435—Piperidines

Abstract

The invention discloses a functional liquid mulching film with a fluorescence effect and a mulching film laying method, and mainly relates to the technical field of agricultural mulching films. The functional liquid mulching film is prepared by the steps of enabling starch to partially react with coumarin 343 acyl chloride, then enabling the starch to partially graft with acryloyl chloride (or methacryloyl chloride), enabling a starch modified product to perform addition polymerization with N- (1-naphthyl) -N-phenyl acryloyl chloride and styrene to prepare a final addition polymerization high polymer, and then compounding the final addition polymerization high polymer with a film forming agent, a micro-fertilizer, a bactericide and the like. The invention has the beneficial effects that: it integrates heat preservation, water retention, soil moisture preservation, micro-fertilizer and pesticide into a whole, and has a functional liquid mulching film product with a fluorescence effect.

Description

Functional liquid mulching film with fluorescence effect and mulching film laying method
Technical Field
The invention relates to the technical field of agricultural mulching films, in particular to a functional liquid mulching film with a fluorescence effect and a mulching film laying method.
Background
The agricultural plastic mulching technology has been used in China for nearly forty years, and because the yield increasing and income increasing effects of film mulching cultivation are obvious, the agricultural plastic mulching film is used in large quantity, but as the plastic mulching film cannot be naturally degraded, the residual film influences and destroys the physical and chemical properties of soil, the root system of crops is difficult to grow and develop. The soil with residual film prevents root systems from communicating and influences normal water and nutrient absorption; when fertilizer is applied among crop plants, large residual films exist, the fertilizer separation phenomenon exists, the fertilizer efficiency is influenced, and the yield is reduced.
In addition, the method is not good enough due to the limitation of residual film recycling and incomplete residual film recycling, so that visual pollution is caused. In addition, after the residual membrane on the ground exposed head is eaten by the animals by mistake, the esophagus is blocked to influence digestion, and even the residual membrane dies. Therefore, in order to solve various problems of the plastic mulching film, research on the liquid mulching film is in progress.
The liquid mulching film is a film forming substance prepared into liquid, and a layer of solid film is formed on the surface layer of soil after spraying, so that soil particles are connected, and the effects of preserving heat, preserving soil moisture, increasing the granular structure of the soil and improving the physical properties of the soil are achieved. In recent years, liquid mulching films have been widely noticed and used by people due to the advantages of good degradability, low cost, capability of being sprayed on site, no limitation of terrain and the like.
Chinese patent application No. 202011549522.9 discloses a biomass-based pesticide-fertilizer liquid mulching film and a preparation method and application thereof, and the method comprises the steps of performing functionalized carboxymethylation modification on waste agriculture and forestry biomass resources to obtain a water-soluble plant fiber component; depositing and loading the biological pesticide on the natural inorganic porous mineral in situ; and (3) blending and crosslinking the water-soluble plant fiber component, the hydrophilic film aid, the medicine-carrying mineral substance, the humic acid and the glycerol, adding a surfactant, homogenizing and emulsifying to obtain the biomass-based pesticide-fertilizer liquid mulching film.
Chinese patent application No. 201510902870.2 discloses an ecological liquid mulching film for farmland weeding and a preparation method and a use method thereof, the method is that konjaku flour, industrial gelatin and quicklime are taken as raw materials, crushed, removed of granules, measured and bagged to prepare raw powder fine materials, and then glycerol and water are added according to the weight ratio to prepare raw liquid which is sprayed on a planting ground.
Chinese patent application No. 200810136827.X discloses a cellulose-based degradable liquid mulching film, which is prepared by taking puffed straw fiber as a main raw material and adding corn starch, acrylic acid starch resin, polyvinyl alcohol, triethanolamine, boric acid, poly (chloro-epichlorohydrin) resin, tween-80 and water. After the synergist and the herbicide are added, the mulching film has certain fertilizer efficiency and weed control functions.
The Chinese patent application number 201710159176.5 discloses a production method of a straw composite liquid mulching film, which comprises the steps of processing crop straws into a cellulose solution, adding an etherifying agent monochloroacetic acid, an initiator potassium persulfate and a cross-linking agent butyl acrylate, and carrying out etherification and cross-linking reaction on the cellulose at 70 ℃ under a stirring condition to obtain cellulose cross-linking liquid; then adding natural polymer chitosan-gelatin blending liquid which has synergistic effect and can improve plasticity and flexibility into the cellulose crosslinking liquid. The chitosan-gelatin blending solution is a bipolar polyelectrolyte formed by coordination crosslinking reaction, and has excellent film-forming property and film-forming strength. Then adding a certain amount of micro-fertilizer, herbicide and pesticide to obtain the straw composite liquid mulching film.
Chinese invention patent application number 201110440063.5 discloses a liquid mulching film and a preparation method thereof, wherein the method comprises the following components by weight percent: 20-30% of methyl silicate, 1-5% of strong base and the balance of water. When in use, the product is added into a common sprayer according to different effective dosage and diluted by adding water, and is uniformly sprayed on the soil surface.
Chinese patent application No. 202010737632.1 discloses a bio-based slow and controlled release pesticide liquid mulching film and a preparation method and application thereof, the method comprises dispersing polysaccharide in a solvent, and oxidizing the polysaccharide with an oxidant to obtain oxidized polysaccharide; reacting oxidized polysaccharide with amino-containing hydrophilic polymer by Schiff base to obtain oxidized polysaccharide graft; simultaneously dissolving the amphiphilic block polymer in a solvent, adding a biological pesticide, and carrying out ultrasonic embedding to obtain drug-loaded microspheres; and finally, blending the prepared oxidized polysaccharide graft and the drug-loaded microspheres, adding a water-absorbing polymer and a plasticizer, and reacting to obtain the bio-based sustained and controlled release pesticide liquid mulching film.
The mulching film technology and the existing mulching film products mainly utilize humic acids, polysaccharides, silicates, straws and waste animal proteins as resources. The mulching film of humic acid has the advantage of improving the soil structure, but the mulching film has poor light transmittance and influences the photosynthesis of plants; and the mulching film is synthesized by heterogeneous crosslinking, the toughness and the tensile property of the film are poor, and the actual application effect is not ideal. The silicate liquid mulching film product is only suitable for sandy land, and the cross-linking interaction between the silicate liquid mulching film product and the soil on the soil layer surface is small; in addition, the use of strong bases still has the potential to cause new environmental pollution.
Therefore, in the aspect of mulching film technology, how to overcome the existing defects and expand the functions of the mulching film is a research hotspot in the field.
Disclosure of Invention
The invention aims to provide a functional liquid mulching film with a fluorescence effect and a mulching film laying method, which integrate heat preservation, water preservation, soil moisture preservation, trace fertilizer and pesticide into a whole and are a functional liquid mulching film product with the fluorescence effect.
In order to realize the purpose, the invention adopts the following technical scheme
A functional liquid mulching film with a fluorescence effect comprises, by weight, 30-60 parts of a polymer, 5-20 parts of a second solvent, 10-20 parts of a film forming agent, 2-5 parts of a surfactant, 1-5 parts of a micro-fertilizer, 1-5 parts of an insecticide, 1-5 parts of a herbicide and 2-15 parts of water;
the polymer is obtained by the addition polymerization of partial graft modified starch, N- (1-naphthyl) -N-phenyl acryloyl chloride and styrene.
Further, the second solvent comprises any one or a combination of several of ethanol, glycerol, propylene glycol, butanol, pentanol, hexanol, ethylene glycol and benzyl alcohol;
and/or
The film forming agent is any one or combination of more of modified starch, redispersible latex powder, polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, gum arabic, guar gum, gelatin, konjac glucomannan, sodium alginate, carboxymethyl cellulose, hydroxyethyl cellulose and sodium lignosulfonate;
and/or
The surfactant is any one or a combination of more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium stearate, fatty acid methyl ester sodium sulfate, long-chain fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene, fatty acid polyoxyethylene ester, polyoxyethylene alkylamine and polyoxyethylene alkyl alcohol acyl chloride;
and/or
The micro-fertilizer is any one or combination of more of potassium fulvate, zinc fulvate, potassium dihydrogen phosphate, seaweed meal and chitin;
and/or
The pesticide is any one or combination of more of nicotine, metalaxyl, abamectin, matrine and natural chrysanthemum-removing insect;
and/or
The herbicide is any one of 2-4D butyl ester, acetochlor and butachlor;
and/or
The water is tap water or deionized water.
Further, the preparation method comprises the following steps:
adding the polymer and the second solvent into a reaction kettle, adding water, the surfactant and the film forming agent after the surfaces of the polymer and the second solvent are wetted, stirring at a high speed of 1000-3000 r/min, then adding the micro-fertilizer, the pesticide and the herbicide while stirring, and stirring uniformly to obtain a finished product of the liquid mulching film.
Further, the preparation method of the polymer comprises the following steps:
step one, preparation of an agent A: adding starch into a first solvent under the stirring state, continuously stirring, dropwise adding coumarin 343 acyl chloride, taking triethylamine as an acid-binding agent, and reacting for 24 hours in an ice-water bath to room temperature under the protection of nitrogen to obtain an agent A;
step two, preparing a B agent: adding triethylamine into the agent A, continuously stirring and dropwise adding acryloyl chloride or methacryloyl chloride, and reacting for 24 hours in an ice water bath to room temperature under the protection of nitrogen to obtain an agent B;
step three, preparation of a preparation C: and (2) in a system of the agent B, under the protection of temperature and nitrogen, sequentially adding an initiator and monomers N- (1-naphthyl) -N-phenyl acryloyl chloride and styrene within 30min, stirring and dropwise adding the monomers, heating in a water bath to 65-85 ℃ after dropwise adding is finished, starting addition polymerization reaction, after the reaction, slowly dropwise adding the reactant solution into a mixed solution of ethanol and water for precipitation, and precipitating a polymer.
Further, the first solvent is any one or a combination of several of tetrahydrofuran, chloroform and dimethyl sulfoxide; before use, the first solvent is subjected to circulating reflux at the boiling point temperature based on benzophenone as a color developing agent, and the first solvent obtained by reflux separation is used for the reaction in the first step.
Further, the starch is any one of corn starch, cassava starch and potato starch;
the initiator is any one or combination of several of azodiisobutyronitrile, azodiisoheptonitrile, benzoyl peroxide tert-butyl ester and methyl ethyl ketone peroxide.
Further, the used raw materials are respectively as follows according to parts by weight: 30-50 parts of starch, 10-30 parts of first solvent, 1-3 parts of coumarin 343 acyl chloride, 2-6 parts of triethylamine, 2-5 parts of acryloyl chloride or methacryloyl chloride, 0.2-0.5 part of initiator, 3-8 parts of N- (1-naphthyl) -N-phenyl acryloyl chloride and 3-6 parts of styrene.
The mulching film laying method uses the liquid mulching film, the using amount of the liquid mulching film per mu is 2.5-3 kg, and the liquid mulching film is directly sprayed on target soil after being diluted by 50-100 times with water.
Compared with the prior art, the invention has the advantages that
The liquid mulching film has the functions of fertilizer slow release, disinsection, sterilization, growth regulation and the like while preserving soil moisture and increasing temperature, integrates agricultural films, fertilizers, pesticides and growth regulators, and has wider development potential.
The concrete effects include:
(1) The invention provides a liquid mulching film technology with a fluorescence effect, and the liquid mulching film technology has the effects of increasing temperature, preserving soil moisture, conserving water sources, keeping water and soil, increasing soil aggregate structures, improving physical properties of soil and the like.
(2) The liquid mulching film has the characteristics of excellent film forming property, efficacy and lasting effect.
(3) After the liquid mulching film is formed, when crops emerge, artificial seedling placement is not needed, seedlings can emerge naturally, and a large amount of manpower and material resources are saved. The mulching film can be used as a soil conditioner after being ploughed and buried, and can be degraded into nutrient substances capable of improving soil fertility.
(4) The liquid mulching film has the advantages that the conjugated structure introduced into the starch macromolecule main chain has an excellent fluorescent effect, the photosynthesis of crops can be properly improved, the physiological metabolism of the crops is stimulated, the stress resistance of the crops is enhanced, and the fruiting quality of the crops is improved. Most raw materials are of polyhydroxy structures, so that the water and fertilizer retention performance is good, and simultaneously, -OH is used as a polar functional group to play a role in hydrogen bond crosslinking in each component of the product, so that the mechanical strength of a formed film can be improved, and the fluorescence effect of conjugated macromolecules can be improved.
(5) The micro-fertilizer adopted by the liquid mulching film can provide certain trace elements such as boron, zinc, potassium and the like for plant growth, improve the root system vigor of plants and play a role in improving the soil fertility.
(6) The synthetic method of the liquid mulching film is simple to operate, the chemical reaction of the grafting modification of the starch is simple, and a complex post-treatment process is not needed. In the production process, the prepared liquid mulching film has good performances in all aspects and can achieve an excellent film forming effect by accurately controlling the dosage and the proportion of each component;
(7) The liquid mulching film disclosed by the invention is simple in use method, can be directly diluted by adding water, can be constructed by adopting a universal agricultural spraying machine, and is particularly suitable for spraying large-area land; and the liquid mulching film product does not contain solid particles, and compared with the liquid mulching film prepared by a humic acid and porous mineral substance system, the liquid mulching film diluted by the liquid mulching film has extremely low probability of blocking spraying equipment.
(8) The invention creatively invents a novel liquid mulching film which has the characteristics of ecological environmental protection, rich fertilizer efficiency and pesticide effect and the like. The soil conditioner integrates pesticide, fertilizer and agricultural film, can inhibit the growth of weeds in a planting area, can become a soil conditioner by turning into soil after use, and has the characteristics of capability of spraying and film making on site, capability of naturally emerging, strong adaptability to landform and the like. The main raw materials adopted in the preparation method are all from the nature, can be naturally degraded in the ecological environment, do not pollute the environment, and have the characteristic of ecological environmental protection.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the present application.
Unless otherwise specified, the instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like known in the art and are commercially available. Unless otherwise specified, the experimental methods, detection methods, and the like in the following examples are all conventional experimental methods, detection methods, and the like in the prior art.
Example 1: functional liquid mulching film with fluorescence effect
Step one, preparing an agent A;
the prepared raw materials comprise corn starch, coumarin 343 acyl chloride and a first solvent;
the mass ratio of the corn starch to the first solvent is 2-7;
the molar ratio of the coumarin 343 acyl chloride to the starch is 0.2: 1;
the molar ratio of triethylamine to coumarin 343 acyl chloride is 1.3: 1.
The first solvent uses tetrahydrofuran, and effluent treatment is carried out by the following method: adding benzophenone as a color developing agent into tetrahydrofuran, adding triethylamine as an acid binding agent, adding a metal sodium wire at a boiling point temperature for circulating reflux, stopping reflux until the benzophenone shows blue, and separating to obtain a first solvent;
adding a first solvent into a three-neck flask with magnetic stirring, adding quantitative starch under the stirring state, dropwise adding coumarin 343 acyl chloride under the stirring state, and reacting for 24 hours under the ice-water bath condition under the protection of nitrogen to obtain an agent A.
Step two, preparing a B agent;
after the agent A reacts, adding a proper amount of triethylamine, and continuously stirring and dropwise adding a certain amount of acryloyl chloride under the same reaction conditions as the first step.
The molar ratio of the triethylamine to the acryloyl chloride is 1.3: 1.
The mol ratio of the acryloyl chloride to the starch is 0.08: 1
Step three, preparation of agent C;
and (2) sequentially adding an initiator and a certain mass ratio of monomers in a system of the agent B within 30min, dropwise adding the monomers while stirring, heating in a water bath to 65-85 ℃ after the complete dropwise addition, keeping the temperature under the protection of nitrogen so as not to start the addition polymerization reaction, slowly dropwise adding the reactant solution into a mixed solution of ethanol and water for precipitation after the reaction is carried out for 24h, and precipitating the polymer agent C.
The mass ratio of the initiator to the monomer is 1.1%;
the initiator is one or a mixture of azodiisobutyronitrile, azodiisoheptonitrile, benzoyl peroxide tert-butyl peroxide and methyl ethyl ketone peroxide;
the monomer is N- (1-naphthyl) -N-phenyl acryloyl chloride and styrene;
step four, preparation of agent D;
preparing according to parts by mass: 1 part of agent C, 1.1 parts of second solvent, 0.15 part of surfactant and 7 parts of film forming agent;
the second solvent is ethanol;
the water is deionized water;
the film forming agent comprises a combination of polyvinyl alcohol, carboxymethyl cellulose, polyvinylpyrrolidone and sodium lignosulfonate;
the surfactant is sodium dodecyl sulfate;
adding a proper amount of second solvent into the reaction kettle, adding the agent C into the reaction kettle, wetting the surface, then adding water, the surfactant and the film forming agent, and stirring at a high speed of 2000r/min to obtain the agent D.
Step five, preparation of the agent E
And adding the micro-fertilizer, the pesticide and the herbicide into the agent D while stirring, and uniformly stirring.
The micro-fertilizer is a mixture of potassium fulvate, zinc fulvate, potassium dihydrogen phosphate, seaweed powder and chitin;
the pesticide is a mixture of nicotine, metalaxyl, abamectin, matrine and natural chrysanthemum-removed insect;
the herbicide is 2-4D butyl ester.
The mass ratio of the micro-fertilizer to the D agent is 0.03: 1;
the mass ratio of the pesticide to the D agent is 0.55: 1;
the mass ratio of the herbicide to the D agent is 0.65: 1.
And step six, metering and subpackaging the agent E to obtain a liquid mulching film finished product.
Example 2: functional liquid mulching film with fluorescence effect
Step one, preparing an agent A;
the prepared raw materials comprise cassava starch, coumarin 343 acyl chloride and a first solvent;
the mass ratio of the cassava starch to the first solvent is 2: 10;
the molar ratio of the coumarin 343 acyl chloride to the starch is 0.05: 1;
the molar ratio of triethylamine to coumarin 343 acyl chloride is 1.1: 1.
A first solvent, chloroform, and performing effluent treatment by the following method: adding benzophenone as a color developing agent into chloroform, adding triethylamine as an acid binding agent, adding calcium hydride at a boiling point temperature for circulating reflux, stopping reflux until the benzophenone shows blue, and separating to obtain a first solvent;
adding a first solvent into a three-neck flask with magnetic stirring, adding quantitative starch while stirring, dropwise adding coumarin 343 acyl chloride while stirring, and reacting for 24 hours under the condition of ice-water bath under the protection of nitrogen to obtain an agent A.
Step two, preparing a B agent;
and (3) after the agent A is reacted, supplementing a proper amount of triethylamine, and continuously dropwise adding quantitative methacryloyl chloride while stirring, wherein the reaction conditions are the same as those in the first step.
The molar ratio of the triethylamine to the acryloyl chloride is 1.5: 1.
The molar ratio of the methacryloyl chloride to the starch is 0.05: 1.
Step three, preparation of agent C;
and (2) sequentially adding an initiator azobisisobutyronitrile and a certain mass ratio of monomers into the system of the agent B within 30min, dropwise adding the monomers while stirring, heating in a water bath to 65-85 ℃ after the complete dropwise addition, keeping the temperature under the protection of nitrogen so as not to start the addition polymerization reaction, slowly dropwise adding the reactant solution into a mixed solution of ethanol and water for precipitation after the reaction is carried out for 24h, and precipitating the polymer C agent.
The mass ratio of the initiator to the monomer is 0.5%;
the monomers are N- (1-naphthyl) -N-phenyl acryloyl chloride and styrene;
step four, preparing a D agent;
preparing according to parts by mass: 1 part of agent C, 1.1 parts of second solvent, 0.05 part of surfactant, 3 parts of film-forming agent and water;
the second solvent is benzyl alcohol;
the water is tap water;
the film forming agent is sodium lignosulfonate;
the surfactant is a mixture of sodium stearate, sodium fatty acid methyl ester sulfate, long-chain fatty alcohol-polyoxyethylene ether, alkylphenol ethoxylates and fatty acid-polyoxyethylene ester;
adding a proper amount of second solvent into a reaction kettle, adding the agent C into the reaction kettle, carrying out surface wetting, then adding water, a surfactant and a film-forming agent, and carrying out high-speed stirring at 1000r/min to obtain the agent D.
Step five, preparation of the agent E
Preparing according to parts by mass: 1 part of D agent, 0.01 part of micro-element fertilizer, 0.01 part of insecticide and 0.01 part of herbicide;
the micro-fertilizer comprises a mixture of potassium fulvate, monopotassium phosphate, seaweed powder and chitin;
the pesticide is matrine and natural Chrysanthemum removing insect;
the herbicide is 2-4D butyl ester.
And adding the micro-fertilizer, the pesticide and the herbicide into the agent D while stirring, and uniformly stirring to obtain the agent E.
And step six, metering and subpackaging the agent E to obtain a finished product of the liquid mulching film.
Example 3: functional liquid mulching film with fluorescence effect
Step one, preparing an agent A;
the prepared raw materials comprise potato starch, coumarin 343 acyl chloride and a first solvent;
the mass ratio of the potato starch to the first solvent is 5: 10;
the molar ratio of the coumarin 343 acyl chloride to the starch is 0.3: 1;
the molar ratio of triethylamine to coumarin 343 acyl chloride is 1.5: 1.
The first solvent uses dimethyl sulfoxide, and effluent treatment is carried out by the following method: adding benzophenone serving as a color developing agent into dimethyl sulfoxide, adding triethylamine serving as an acid binding agent, adding calcium hydride at a boiling point temperature for circulating reflux, stopping reflux until the benzophenone is blue, and separating to obtain a first solvent;
adding a first solvent into a three-neck flask with magnetic stirring, adding quantitative starch while stirring, dropwise adding coumarin 343 acyl chloride while stirring, and reacting for 24 hours under the condition of ice-water bath under the protection of nitrogen to obtain an agent A.
Step two, preparing a B agent;
and (3) after the agent A is reacted, supplementing a proper amount of triethylamine, and continuously dropwise adding quantitative acryloyl chloride while stirring, wherein the reaction conditions are the same as the first step.
The molar ratio of the triethylamine to the acryloyl chloride is 1.1: 1.
The mol ratio of the acryloyl chloride to the starch is 0.1: 1
Step three, preparing a preparation C;
and (2) sequentially adding an initiator azobisisoheptonitrile and a certain mass ratio of monomers in a B agent system within 30min, dropwise adding the monomers while stirring, heating in a water bath to 65-85 ℃ after complete dropwise addition, keeping the temperature under the protection of nitrogen so as not to start addition polymerization reaction, slowly dropwise adding the reactant solution into a mixed solution of ethanol and water for precipitation after 24h of reaction, and precipitating a polymer C agent.
The mass ratio of the initiator to the monomer is 2%;
the monomer is N- (1-naphthyl) -N-phenyl acryloyl chloride and styrene;
step four, preparation of agent D;
preparing according to parts by mass: 1 part of agent C, 1.1 parts of second solvent, 0.2 part of surfactant, 10 parts of film forming agent and water;
the second solvent is a mixture of ethanol and ethylene glycol;
the water is tap water;
the film forming agent is modified starch;
the surfactant is sodium dodecyl sulfate;
adding a proper amount of second solvent into a reaction kettle, adding the agent C into the reaction kettle, carrying out surface wetting, then adding water, the surfactant and the film forming agent, and carrying out high-speed stirring at 3000r/min to obtain the agent D.
Step five, preparation of the agent E
Preparing according to parts by mass: 1 part of D agent, 0.05 part of micro-element fertilizer, 0.75 part of insecticide and 0.75 part of herbicide;
the micro-fertilizer comprises a mixture of potassium fulvate, monopotassium phosphate, seaweed powder and chitin;
the pesticide is matrine and natural Chrysanthemum removing insect;
the herbicide is 2-4D butyl ester.
And adding the micro-fertilizer, the pesticide and the herbicide into the agent D while stirring, and uniformly stirring to obtain the agent E.
And step six, metering and subpackaging the agent E to obtain a finished product of the liquid mulching film.
Example 4: mulching film construction method
The mulching film product obtained in the example 1 is diluted by 50 to 100 times by adding water, and after the liquid mulching film is completely diluted in the water, the liquid mulching film can be sprayed by adopting a common agricultural spraying machine. After the film is formed, when the crops emerge, the seedlings do not need to be put artificially, and can emerge naturally, thereby saving a large amount of manpower and material resources. The mulching film can be used as a soil conditioner after being ploughed and buried, and can be degraded into nutrient substances capable of improving soil fertility. Can not only provide certain trace elements such as boron, zinc, potassium and the like for the growth of plants, improve the root system vigor of the plants, but also play a role in improving the soil fertility.
Table 2: technical indexes of the liquid mulching film
Figure BDA0003805655410000131
Figure BDA0003805655410000141
Example 5: application test of the mulching film product obtained in example 1
The first application embodiment:
planting place: potato-based land of Chifeng city in inner Mongolia autonomous region.
Planting the variety: a potato.
The planting area of the control group is: 1 mu (covered and planted by a polyethylene plastic mulching film greenhouse).
Test group planting area: 1 mu (planting by adopting a liquid mulching film cultivation technology).
Planting time: and planting potatoes of the same variety in a large bud planting manner on 1 mu of control group planting land and 1 mu of test group planting land selected in 10 days in 5 months in 2021 year.
Control group coating time: covering polyethylene plastic mulching films on the control group planting land in 2021, 5 months and 12 days;
time for spraying liquid mulching film in test group: spraying liquid mulching film on the ground of the planting field of the test group in 2021, 5 months and 12 days, which is carried out according to the following steps:
(1) leveling the ground: carrying out leveling operation on the ground of the selected test group cultivated land;
(2) preparing stock solution: before weeds in the flat test group planted farmland sprout and come out, the mulching film stock solution of the embodiment 1 is mixed according to the proportion of 1:70, diluting with water;
(3) spraying a stock solution: the liquid plastic film that will make is packed into the liquid reserve tank of atomizer, and the atomizer joins in marriage dress aperture and is 1.0 cm's nozzle, evenly sprays the liquid plastic film on planting arable land surface with the atomizer, and the spraying volume is: 2.5 kg/mu of liquid mulching film stock solution can form a cured and shaped film mulching film finished product on the surface of the cultivated land after natural air drying.
Results of the control test:
control group (using polyethylene plastic mulch): the seedlings are in poor uniformity and need to be guided and transplanted manually
The leaves of the seedlings are small, the color of the leaves is slightly dark, and the weeds in the field are more; the yield of the potatoes which are actually harvested is only 3208.3 kg/mu, and the use defects of high mulching film cost, high labor intensity, labor waste, time waste, low efficiency and field pollution caused by abandoned mulching film fragments exist.
Test group (planting by liquid mulching cultivation technology): the seedlings can naturally rupture the membranes without manual seedling leading, the emergence rate is high, the emergence is tidy and uniform, the development is normal, the seedlings grow robustly, the leaves are big and dark green, the field weeds are few, the yield of the potatoes which are actually harvested reaches 3879.6 kg/mu, and the method is observed that: the liquid mulching film is completely and naturally degraded after 100 days, has no pollution to cultivated land, no harm to people and livestock, no mulching cost, labor and time saving, and high efficiency, and is calculated according to the following steps: the yield of the potatoes planted by the liquid mulching film can be increased by 20.92 percent per mu compared with the yield of the potatoes planted by the polyethylene plastic mulching film mulching planting mode, the cost can be reduced by 20 to 40 percent, has remarkable ecological environmental protection social effect and economic benefit, and is deeply welcomed by broad growers.
The test data of the embodiment of the invention show that the liquid mulching film has less dosage and good crusting effect. The invention relates to a liquid mulching film, and most of the existing products are powder products and humic acid products: the powder product has the problems of easy agglomeration and pimple formation when diluted by water, thus uneven dispersion is caused; the humic acid products are easy to block spraying equipment. Therefore, the invention has the advantages of easy dilution and construction method, and simultaneously, the liquid mulching film with fluorescence effect can promote the growth of plants and improve the yield.

Claims (8)

1. A functional liquid mulching film with a fluorescence effect is characterized by comprising, by weight, 30-60 parts of a polymer, 5-20 parts of a second solvent, 10-20 parts of a film-forming agent, 2-5 parts of a surfactant, 1-5 parts of a micro-fertilizer, 1-5 parts of an insecticide, 1-5 parts of a herbicide and 2-15 parts of water;
the polymer is obtained by the addition polymerization of part of graft modified starch, N- (1-naphthyl) -N-phenyl acryloyl chloride and styrene.
2. The functional liquid mulching film with the fluorescent effect according to claim 1, wherein the second solvent comprises one or more of ethanol, glycerol, propylene glycol, butanol, pentanol, hexanol, ethylene glycol, and benzyl alcohol;
and/or
The film forming agent is any one or combination of more of modified starch, redispersible latex powder, polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, gum arabic, guar gum, gelatin, konjac glucomannan, sodium alginate, carboxymethyl cellulose, hydroxyethyl cellulose and sodium lignosulfonate;
and/or
The surfactant is any one or a combination of more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium stearate, fatty acid methyl ester sodium sulfate, long-chain fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene, fatty acid polyoxyethylene ester, polyoxyethylene alkylamine and polyoxyethylene alkyl alcohol acyl chloride;
and/or
The micro-fertilizer is any one or combination of more of potassium fulvate, zinc fulvate, potassium dihydrogen phosphate, seaweed meal and chitin;
and/or
The pesticide is any one or combination of more of nicotine, metalaxyl, abamectin, matrine and natural chrysanthemum-removing insect;
and/or
The herbicide is any one of 2-4D butyl ester, acetochlor and butachlor;
and/or
The water is tap water or deionized water.
3. The functional liquid mulching film with the fluorescence effect according to claim 1, is prepared by the following steps:
adding the polymer and the second solvent into a reaction kettle, adding water, a surfactant and a film forming agent after the surfaces are wetted, stirring at a high speed of 1000-3000 r/min, then adding the micro-fertilizer, the pesticide and the herbicide while stirring, and uniformly stirring to obtain a finished product of the liquid mulching film.
4. The functional liquid mulching film with fluorescence effect according to claim 1, wherein the preparation method of the polymer comprises the following steps:
step one, preparation of an agent A: adding starch into a first solvent under the stirring state, continuously stirring, dropwise adding coumarin 343 acyl chloride, taking triethylamine as an acid-binding agent, and reacting for 24 hours in an ice-water bath to room temperature under the protection of nitrogen to obtain an agent A;
step two, preparing a B agent: adding triethylamine into the agent A, continuously stirring and dropwise adding acryloyl chloride or methacryloyl chloride, and reacting for 24 hours in ice water bath to room temperature under the protection of nitrogen to obtain an agent B;
step three, preparation of a preparation C: and (2) in a system of the agent B, under the protection of temperature and nitrogen, sequentially adding an initiator and monomers N- (1-naphthyl) -N-phenyl acryloyl chloride and styrene within 30min, stirring and dropwise adding the monomers, heating in a water bath to 65-85 ℃ after dropwise adding is finished, starting addition polymerization reaction, after the reaction, slowly dropwise adding the reactant solution into a mixed solution of ethanol and water for precipitation, and precipitating a polymer.
5. The functional liquid mulching film with fluorescence effect according to claim 4, wherein the first solvent is one or a combination of tetrahydrofuran, chloroform and dimethyl sulfoxide; before use, the first solvent is subjected to circulating reflux at the boiling point temperature based on benzophenone as a color developing agent, and the first solvent obtained by reflux separation is used for the reaction in the first step.
6. The functional liquid mulching film with the fluorescence effect according to claim 4, wherein the starch is any one of corn starch, tapioca starch and potato starch;
the initiator is any one or combination of a plurality of azodiisobutyronitrile, azodiisoheptonitrile, benzoyl peroxide tert-butyl peroxide and methyl ethyl ketone peroxide.
7. The functional liquid mulching film with the fluorescence effect according to claim 4, wherein the used raw materials are respectively as follows in parts by weight: 30-50 parts of starch, 10-30 parts of first solvent, 1-3 parts of coumarin 343 acyl chloride, 2-6 parts of triethylamine, 2-5 parts of acryloyl chloride or methacryloyl chloride, 0.2-0.5 part of initiator, 3-8 parts of N- (1-naphthyl) -N-phenyl acryloyl chloride and 3-6 parts of styrene.
8. The method for laying a mulching film according to claim 1, wherein the liquid mulching film according to any one of claims 1 to 7 is used in an amount of 2.5 to 3kg per mu, diluted with water by 50 to 100 times, and directly sprayed on the target soil.
CN202210996692.4A 2022-08-19 2022-08-19 Functional liquid mulching film with fluorescence effect and mulching film laying method Pending CN115216103A (en)

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