CN114561033B - Garlic extract-based insect-resistant mulching film and preparation method thereof - Google Patents
Garlic extract-based insect-resistant mulching film and preparation method thereof Download PDFInfo
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- CN114561033B CN114561033B CN202210163886.6A CN202210163886A CN114561033B CN 114561033 B CN114561033 B CN 114561033B CN 202210163886 A CN202210163886 A CN 202210163886A CN 114561033 B CN114561033 B CN 114561033B
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- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- 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
- A01G13/0268—Mats or sheets, e.g. nets or fabrics
- A01G13/0275—Films
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- 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
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/023—On to modified polymers, e.g. chlorinated polymers
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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
- C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
- C08F261/02—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols
- C08F261/04—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols on to polymers of vinyl alcohol
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/003—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09D151/06—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
The invention provides a garlic extract-based insect-resistant mulching film and a preparation method thereof. The insect-resistant layer is composed of garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer. The prepared mulching film can effectively improve the effect of cabbage on resisting the invasion of plutella xylostella, has no obvious water drop formation on the surface of the mulching film facing soil, has good light transmittance, can maintain higher soil temperature, and is beneficial to agricultural production.
Description
Technical field:
the invention belongs to the technical field of agricultural mulching films, and particularly relates to a garlic extract-based insect-resistant mulching film.
The background technology is as follows:
in modern agricultural production, mulch film materials are an indispensable production tool for achieving larger crop yield in the land. The main reason that the mulching film can improve the yield of crops is that the mulching film improves the temperature and the humidity of soil and reduces the influence of cold and drought weather on the growth and the development of crops. The mulching film is of various types, wherein the light-transmitting mulching film is a main variety, the speed of lifting the ground temperature by the light-transmitting mulching film is high, the soil moisture preservation by heating is facilitated, and the light-transmitting mulching film is suitable for spring, autumn and winter with relatively low air temperature. It should be noted that in spring and autumn, the season in which pests in agricultural soil are extremely easy to grow is also considered, so that in order to ensure the harvest of crops under the mulching film, it is necessary to pay attention to not only raise the temperature and humidity of the soil, but also to prevent the pests of the crops. At present, most of traditional light-transmitting mulching films are plastic mulching films made of polyethylene or polyvinyl chloride, and when the light-transmitting mulching films are used, the whole plastic mulching films are paved on the soil surface, so that the mulching film paving operation is completed. The traditional plastic mulching film has single function, if plant diseases and insect pests occur in farmland soil, holes are needed to be broken in the traditional plastic film (sometimes the whole mulching film is lifted), and then pesticides and the like capable of inhibiting the growth of harmful bacteria or pests in the soil are applied. However, the ground film after the holes is broken is difficult to prevent the water and heat in the soil from diffusing outwards, so that the water-retaining and heat-preserving effects of the ground film on the soil are seriously weakened, and the ground film is unfavorable for increasing the yield and income of agriculture. Therefore, on the basis of the traditional mulching film, the development of a mulching film product which does not need to break holes on the mulching film to apply pesticide for deinsectization and has a certain disease and pest resistance function is significant.
The invention comprises the following steps:
the invention provides a garlic extract-based insect-resistant mulching film and a preparation method thereof, aiming at solving the problems existing in the prior art.
The garlic extract-based insect-resistant mulching film is characterized in that a mask layer (1) and an insect-resistant layer (2) are sequentially arranged from top to bottom, the insect-resistant layer is composed of a garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer, and the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer comprises the following components in parts by weight: 10-30 parts of garlic extract, 15-30 parts of hydroxypropyl acrylate, 1-5 parts of styrene, 1-5 parts of chlorosulfonated polyethylene and 20-40 parts of polyvinyl alcohol; the preparation method of the garlic extract-based insect-resistant mulching film comprises the following steps:
(1) 1-5 parts by weight of chlorosulfonated polyethylene is dissolved in 1-5 parts by weight of styrene to obtain a solution A;
(2) Dissolving 0.65 weight part of ammonium persulfate initiator in 10 weight parts of deionized water to obtain solution B;
(3) Stirring 10-30 parts by weight of the solution A obtained in the step (1), 2.9-3.2 parts by weight of sodium dodecyl sulfate, 3.9-4.3 parts by weight of OP-10 emulsifier, 20-40 parts by weight of polyvinyl alcohol and 107-258 parts by weight of deionized water at the room temperature with the rotating speed of 350-360r/min for 30-50min to obtain emulsion C;
(4) Heating a container containing emulsion C to 75-82 ℃ in a water bath, dropwise adding 15-30 parts by weight of hydroxypropyl acrylate into the emulsion C under stirring, wherein the dropwise adding speed is 1 drop per 2 seconds, the stirring speed is 200-250r/min, and meanwhile, dropwise adding the hydroxypropyl acrylate into the solution B obtained in the step (2), wherein the dropwise adding speed is 1 drop per 5 seconds;
(5) After the dripping of the hydroxypropyl acrylate and the solution B in the step (4) is finished, heating the reaction system to 85-88 ℃, and stirring at the constant temperature for reacting for 4.5-5.5 hours, wherein the stirring speed is 220-280r/min; after the constant-temperature stirring reaction is finished, cooling the obtained mixed solution to room temperature, and then adding concentrated ammonia water to adjust the pH of the mixed solution to be neutral to obtain emulsion D;
(6) Coating the emulsion D obtained in the step (5) on the surface of a mask layer, controlling the thickness of the emulsion D layer to be 0.4-0.6mm, and drying at room temperature to obtain an insect-preventing layer which is attached to the surface of the mask layer and consists of garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol;
the garlic extract-based insect-resistant mulching film can be obtained through the steps (1) - (6).
Wherein the mask layer is made of polyethylene or polyvinyl chloride.
The invention is different from the prior art in that the invention achieves the following technical effects:
The test results of the effect embodiment show that the mule film prepared by the invention can effectively improve the effect of the cabbage on resisting the invasion of plutella xylostella, has no obvious water drop formation on the surface of the mule film facing the soil, has good light transmittance and can maintain higher soil temperature. This is because of the following factors:
1. the insect-proof layer is composed of the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer, wherein the hydroxypropyl acrylate and the styrene in the copolymer can promote emulsion formation, so that the copolymer has good film forming property and adhesiveness, the copolymer can form a film-shaped coating to be adhered on the mask layer, and the stability of the insect-proof layer composed of the copolymer on the mask layer is improved. The chlorosulfonated polyethylene in the reaction raw materials can be well dissolved in the styrene, so that the chlorosulfonated polyethylene exists in a molecular form, and when the styrene monomer is subjected to copolymerization, the styrene in the copolymer can enable the chlorosulfonated polyethylene to have better compatibility with other components in the copolymer, so that the chlorosulfonated polyethylene molecular chains and other polymer chains in the copolymer are interwoven together in a molecular level to form the copolymer with more uniform distribution of the components. The chlorosulfonated polyethylene in the copolymer can improve the flexibility of the formed copolymer film and can further improve the adhesion of the copolymer, thereby further improving the stability of the insect-proof layer formed by the copolymer on the mask layer.
2. The hydroxypropyl acrylate monomer in the reaction raw material has a double bond and an ester bond, and also has a hydrophilic hydroxyl group, so that the hydroxypropyl acrylate in the copolymer can endow the copolymer with better hydrophilicity. The polyvinyl alcohol in the copolymer is also a strongly hydrophilic component. Therefore, the hydroxypropyl acrylate and the polyvinyl alcohol in the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer can impart excellent hydrophilicity to the insect-repellent layer, which makes the contact angle of water drops on the surface of the insect-repellent layer smaller, and makes condensed water drops spread out and flow away rapidly on the surface of the hydrophilic insect-repellent layer. The hydrophilic insect-proof layer has the following advantages: (1) Because no (or less) water drops are formed on the surface of the hydrophilic insect prevention layer of the mulching film, the surface of the insect prevention layer is in direct contact with the crop growth environment under the mulching film, and the effect of the insect prevention layer on insect pest inhibition can be exerted greatly; if the insect-proof layer has poor hydrophilicity, a thicker water drop layer is spread on the surface of the insect-proof layer, so that the insect-proof layer cannot directly contact with the crop growing environment under the mulching film, and the insect pest inhibition effect of the insect-proof layer is difficult to be exerted. (2) The hydrophilic insect prevention layer can enable sunlight to easily penetrate through the mulching film to directly irradiate the soil surface covered by the mulching film, and reduces absorption of water drops to solar energy, so that the mulching film disclosed by the invention can efficiently utilize solar energy, and the soil covered by the mulching film is maintained at a higher temperature. The hydroxypropyl acrylate, the styrene, the chlorosulfonated polyethylene and the polyvinyl alcohol in the copolymer are transparent, so that the mulching film has good light transmittance.
3. The garlic extract in the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer is a water-soluble powdery product prepared by taking garlic bulbs of the lily family as raw materials, heating, extracting, concentrating under reduced pressure and spray drying, wherein the garlic extract keeps the original active ingredients of the plants, and is easy to dissolve in water and store. The literature ([ 1]Dougoud J,Toepfer S,Bateman M,et al.Efficacy of homemade botanical insecticides based on traditional knowledge.A review[J ]. Agronomy for Sustainable Development,2019,39,37; [2]Prowse G M,Galloway T S,Andrew F.Insecticidal activity of garlic juice in two dipteran pests[J ]. Agricultural and Forest Entomology,2006,8,1-6; [3] Wang Yunfan, wang Gang ] preliminary studies on the prevention and treatment of cabbage black spot by garlic extract [ J ]. Chongqing academy of sciences (Nature science edition), 2008,10 (5), 61-63.), all mentions that garlic extract can be used as a natural botanical pesticide in agricultural production. However, it should be noted that the garlic extract itself does not have film forming properties, and it alone cannot be covered on the soil surface as effectively as a film, so that it cannot effectively raise the temperature and humidity of the soil. Meanwhile, the garlic extract itself does not have good adhesion, and the garlic extract alone cannot be stably adhered to a polyethylene or polyvinyl chloride plastic film to form an effective insect-proof layer.
Document 4 (CN 104742459 a) reports an insect-repellent grass-repellent degradable environmental protection mulch film comprising an outer mulch film and an inner mulch film, both of which contain polyethylene, wherein the outer mulch film further contains neem oil as an insect repellent. The hydrophobic polyethylene in the inner and outer mulch film of document 4 is a main component (not less than 60 wt.%) and therefore the inner and outer mulch film has no hydrophilicity, so that water drops are liable to form on the inner and outer mulch film of document 4, and the water drops prevent the mulch film containing the insect repellent from directly contacting with the crop growing environment under the mulch film, which reduces the insect resistance of the mulch film. Unlike the mulch film of document 4, the insect-proof layer of the mulch film of the present invention has hydrophilicity, is not liable to form water drops, and can exert the insect-proof performance of the mulch film better, which can also be demonstrated by the following effect examples.
Document 5 (CN 215301950U) reports a pest-repellent garlic residue based mulch comprising a black plastic mulch layer, below which is a garlic residue layer, below which is a lignin adhesive layer. The mulching film provided in the document 5 adopts garlic residue particles, and the garlic residue particles are opaque, so that the mulching film reported in the document 5 has poor light transmittance, and the temperature rising effect of sunlight on soil under the mulching film is limited. Unlike the mulching film of document 5, the mulching film of the present invention uses garlic extract as a raw material, not garlic residue particles, and the garlic extract has water solubility, so that in the preparation step (1) of the present invention, when the garlic extract is added to a solution, the garlic extract is dissolved in the water solvent in the solution, the garlic extract exists in the solution in a molecular form, and further the garlic extract also participates in the subsequent emulsion polymerization in a molecular form, and the garlic extract component in the copolymer also exists in a molecular form, not in the form of opaque particles, and thus the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer coating (or insect-repellent layer) prepared from the garlic extract of the present invention is transparent (or light-transmitting) rather than being light-transmitting as in the mulching film of document 5.
Document 6 (CN 113563517 a) reports a liquid mulching film based on garlic residue, which is prepared by using a mixture of garlic residue slurry, pregelatinized starch and acrylic acid monomer as main raw materials, and the reaction process involves a pre-oxidation process, a pre-emulsification process and an emulsion radical polymerization process under the action of an initiator. The mulch film provided in document 6 is similar to the mulch film provided in the present invention in that: both the garlic residues and the garlic extracts are derived from garlic, a natural plant, and both use acrylic monomers. However, the mulching film provided in document 6 is significantly or distinctly different from the mulching film of the present invention in terms of the raw materials used, the method of use, the principle of film formation, the light transmittance, the range of use, and the like. Specifically: (1) The two are different in terms of raw material use, the mulching film of the document 6 uses butyl acrylate, the hydroxypropyl acrylate monomer structure is similar to the molecular structure of butyl acrylate, but the hydroxypropyl acrylate monomer has a double bond and an ester bond and also has a hydrophilic hydroxyl group, so that the copolymer can be endowed with better hydrophilicity by using the hydroxypropyl acrylate; in document 6, pregelatinized starch raw material is used, and starch is not used as raw material in the present invention; the present invention uses styrene and chlorosulfonated polyethylene as raw materials, and document 6 does not use both as raw materials; the present invention is different from document 6 in use of other materials. (2) The two are very different in terms of the use method and the film forming mechanism, the liquid mulching film used in the document 6 is formed by directly spraying liquid on the soil surface and then naturally air-drying the sprayed liquid on the soil surface, and the mulching film used in the invention is still a solid film, namely, the formed solid film material is paved on the soil surface and is not liquid; (3) The light transmittance of the mulching film is different from that of the mulching film, and the liquid mulching film obtained in the document 6 contains garlic residue particles which are not easy to transmit light, so that the mulching film in the document 6 has poor light transmittance, the garlic extract used in the invention is water-soluble, and the water-soluble garlic extract exists in a molecular form in a coating rather than in a granular form, so that the mulching film has better light transmittance than the mulching film in the document 6. (4) The liquid mulch provided in document 6 is used by tightly adhering or adhering to the soil surface, and cannot be torn off from the soil surface to form a whole film for use, i.e., is not applicable to crops grown to a certain height on the soil, because the mulch emulsion is sprayed to the surface of the crops instead of the soil surface, thereby losing the effect of the liquid mulch in raising the temperature and humidity of the soil, and the liquid mulch is mainly used for promoting germination of crop seeds and growth in an early stage; the mulching film is a whole film, can be used without being tightly attached to the ground, can be used above crops which have grown to a certain height on the soil, and is suitable for the crops in the early, middle and later stages of growth and development.
The working principle of the garlic extract-based insect-proof mulching film prepared by the invention is analyzed as follows:
the steps (1) - (5) in the preparation step of the invention are reaction steps for preparing the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer emulsion, in the emulsion preparation step, chlorosulfonated polyethylene is firstly dissolved in styrene, because the chlorosulfonated polyethylene has good solubility in styrene, the chlorosulfonated polyethylene is not easy to form particles or caking in the emulsion, and the chlorosulfonated polyethylene and other high polymer chains are crossed and interpenetrating in a molecular form to form a high polymer copolymer with uniformly distributed components. In addition, in the steps (1) - (5), the ammonium persulfate initiator can initiate the hydroxypropyl acrylate and styrene monomer molecules with double bonds in the solution to carry out polymerization reaction; sodium dodecyl sulfonate and OP-10 (an industrial raw material, alkylphenol polyoxyethylene ether obtained by condensation reaction of alkylphenol and ethylene oxide, which is a model in the OP series of emulsifiers) play the role of an emulsifier, and the copolymer generated after the polymerization reaction can be formed into oil-in-water droplets to be suspended in a solution to form emulsion. The garlic extract contained in the invention can be uniformly distributed in the emulsion, and the emulsion can exist stably and is not easy to break and delaminate; if the emulsion is unstable, demulsification layering occurs, the garlic extract components are unevenly distributed in the unstable emulsion or the demulsification layered liquid, and further the insect pest inhibition performance, the hydrophilic performance and the like of the formed insect prevention layer are affected. The preparation step (6) is to coat the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer emulsion on a polyethylene or polyvinyl chloride mask layer, wherein chlorosulfonated polyethylene derived from polyethylene has good compatibility and cohesiveness on the polyethylene or polyvinyl chloride mask layer, so that the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer emulsion is easy to adhere on the mask layer, and a solid coating containing the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer is formed on the mask layer after the moisture in the emulsion evaporates. The garlic extract component contained in the solid coating can play a role in reducing the damage effect of pests on crops. Meanwhile, the solid coating has good hydrophilicity, and water drops can be spread on the surface of the solid coating to quickly flow away, so that the surface of the insect prevention layer of the garlic extract-based insect-resistant mulching film has the property of being difficult to cause water drops to be accumulated, the surface of the hydrophilic insect prevention layer can be directly contacted with the crop growing environment below the mulching film under the condition of no blocking of the water drops, and the insect prevention layer can exert higher insect resistance efficiency.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate the invention and together with the description serve to explain, without limitation, the invention.
FIG. 1 is a perspective view of a garlic extract based insect-resistant mulch film of the present invention.
FIG. 2 is a cross-sectional view of a garlic extract based insect-resistant mulch film of the present invention.
Reference numerals in the drawings: 1-a mask layer; 2-insect prevention layer.
Detailed Description
The above and further technical features and advantages of the present invention will be described in more detail below with reference to the examples. The chemical raw materials used in the following examples are all commercially available, chemically pure reagents;
the garlic extract was purchased from Shaanxi Kang Jun Biotechnology Inc. as a water-soluble powder.
Chlorosulfonated polyethylene (model: CSM3304, production unit: jilin petrochemical company, inc.) was purchased from offshore International trade company, inc.
Polyvinyl alcohol (model: 1788) is purchased from Shanghai Chen Yi Xie Chen Co.
Example 1
Referring to the attached drawings, the garlic extract-based insect-resistant mulching film is characterized in that a mask layer (1) and an insect-resistant layer (2) are sequentially arranged from top to bottom, the insect-resistant layer is composed of a garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer, and the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer comprises the following components in parts by weight: 10 parts of garlic extract, 15 parts of hydroxypropyl acrylate, 1 part of styrene, 1 part of chlorosulfonated polyethylene and 20 parts of polyvinyl alcohol; the preparation method of the garlic extract-based insect-resistant mulching film comprises the following steps:
(1) 1 part by weight of chlorosulfonated polyethylene is dissolved in 1 part by weight of styrene to obtain a solution A;
(2) Dissolving 0.65 weight part of ammonium persulfate initiator in 10 weight parts of deionized water to obtain solution B;
(3) Stirring 10 parts by weight of the solution A obtained in the step (1), 2.9 parts by weight of sodium dodecyl sulfate, 3.9 parts by weight of OP-10 emulsifier, 20-40 parts by weight of polyvinyl alcohol and 107 parts by weight of deionized water at room temperature with the rotating speed of 350-360r/min for 30min to obtain emulsion C;
(4) Heating a container containing emulsion C to 75 ℃, dropwise adding 15 parts by weight of hydroxypropyl acrylate into the emulsion C under stirring, wherein the dripping speed is 1 drop per 2 seconds, the stirring speed is 200-220r/min, and meanwhile, dropwise adding the solution B obtained in the step (2) into the emulsion C, wherein the dripping speed is 1 drop per 5 seconds;
(5) After the dropwise addition of the hydroxypropyl acrylate and the solution B in the step (4) is finished, heating the reaction system to 85 ℃, and stirring at the constant temperature for reacting for 4.5 hours, wherein the stirring speed is 220-240r/min; after the constant-temperature stirring reaction is finished, cooling the obtained mixed solution to room temperature, and then adding concentrated ammonia water to adjust the pH of the mixed solution to be neutral to obtain emulsion D;
(6) Coating the emulsion D obtained in the step (5) on the surface of a polyvinyl chloride mask layer, controlling the thickness of the emulsion D layer to be 0.4mm, and drying at room temperature to obtain an insect-proof layer which is attached to the surface of the mask layer and consists of garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol;
the garlic extract-based insect-resistant mulching film of example 1 can be obtained through steps (1) - (6).
Example 2
Referring to the attached drawings, the garlic extract-based insect-resistant mulching film is characterized in that a mask layer (1) and an insect-resistant layer (2) are sequentially arranged from top to bottom, the insect-resistant layer is composed of a garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer, and the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer comprises the following components in parts by weight: 15 parts of garlic extract, 19 parts of hydroxypropyl acrylate, 2 parts of styrene, 2 parts of chlorosulfonated polyethylene and 25 parts of polyvinyl alcohol; the preparation method of the garlic extract-based insect-resistant mulching film comprises the following steps:
(1) 2 parts by weight of chlorosulfonated polyethylene is dissolved in 2 parts by weight of styrene to obtain a solution A;
(2) Dissolving 0.65 weight part of ammonium persulfate initiator in 10 weight parts of deionized water to obtain solution B;
(3) Stirring the solution A obtained in the step (1), 15 parts by weight of garlic extract, 3 parts by weight of sodium dodecyl sulfate, 4 parts by weight of OP-10 emulsifier, 25 parts by weight of polyvinyl alcohol and 144 parts by weight of deionized water at the room temperature with the rotating speed of 350-360r/min for 35min to obtain emulsion C;
(4) Heating a container containing emulsion C to 77 ℃, dropwise adding 19 parts by weight of hydroxypropyl acrylate into the emulsion C under stirring, wherein the dripping speed is 1 drop per 2 seconds, the stirring speed is 220-230r/min, and meanwhile, dropwise adding the solution B obtained in the step (2) into the emulsion C, wherein the dripping speed is 1 drop per 5 seconds;
(5) After the dropwise addition of the hydroxypropyl acrylate and the solution B in the step (4) is finished, heating the reaction system to 86 ℃, and stirring at the constant temperature for reacting for 4.5 hours, wherein the stirring speed is 240-250r/min; after the constant-temperature stirring reaction is finished, cooling the obtained mixed solution to room temperature, and then adding concentrated ammonia water to adjust the pH of the mixed solution to be neutral to obtain emulsion D;
(6) Coating the emulsion D obtained in the step (5) on the surface of a polyethylene mask layer, controlling the thickness of the emulsion D layer to be 0.45mm, and drying at room temperature to obtain an insect-proof layer which is attached to the surface of the mask layer and consists of garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol;
The garlic extract-based insect-resistant mulching film of example 2 was obtained through steps (1) - (6).
Example 3
Referring to the attached drawings, the garlic extract-based insect-resistant mulching film is characterized in that a mask layer (1) and an insect-resistant layer (2) are sequentially arranged from top to bottom, the insect-resistant layer is composed of a garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer, and the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer comprises the following components in parts by weight: 20 parts of garlic extract, 22 parts of hydroxypropyl acrylate, 3 parts of styrene, 3 parts of chlorosulfonated polyethylene and 30 parts of polyvinyl alcohol; the preparation method of the garlic extract-based insect-resistant mulching film comprises the following steps:
(1) Dissolving 3 parts by weight of chlorosulfonated polyethylene in 3 parts by weight of styrene to obtain a solution A;
(2) Dissolving 0.65 weight part of ammonium persulfate initiator in 10 weight parts of deionized water to obtain solution B;
(3) Stirring the solution A obtained in the step (1), 20 parts by weight of garlic extract, 3.1 parts by weight of sodium dodecyl sulfate, 4.1 parts by weight of OP-10 emulsifier, 30 parts by weight of polyvinyl alcohol and 181 parts by weight of deionized water at a rotating speed of 350-360r/min at room temperature for 40min to obtain emulsion C;
(4) Heating a container containing the emulsion C to 80 ℃ in a water bath, dropwise adding 22 parts by weight of hydroxypropyl acrylate into the emulsion C under stirring, wherein the dripping speed is 1 drop every 2 seconds, and the stirring speed is 230-240r/min; simultaneously, dropwise adding hydroxypropyl acrylate into the emulsion C, wherein the dropwise adding speed of the solution B obtained in the step (2) is 1 drop per 5 seconds;
(5) After the dropwise addition of the hydroxypropyl acrylate and the solution B in the step (4) is finished, heating the reaction system to 87 ℃, and stirring at the constant temperature for reacting for 5 hours, wherein the stirring speed is 250-260r/min; after the constant-temperature stirring reaction is finished, cooling the obtained mixed solution to room temperature, and then adding concentrated ammonia water to adjust the pH of the mixed solution to be neutral to obtain emulsion D;
(6) Coating the emulsion D obtained in the step (5) on the surface of a polyethylene mask layer, controlling the thickness of the emulsion D layer to be 0.5mm, and drying at room temperature to obtain an insect-proof layer which is attached to the surface of the mask layer and consists of garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol;
the garlic extract-based insect-resistant mulching film of example 3 was obtained through steps (1) - (6).
Example 4
Referring to the attached drawings, the garlic extract-based insect-resistant mulching film is characterized in that a mask layer (1) and an insect-resistant layer (2) are sequentially arranged from top to bottom, the insect-resistant layer is composed of a garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer, and the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer comprises the following components in parts by weight: 25 parts of garlic extract, 26 parts of hydroxypropyl acrylate, 4 parts of styrene, 4 parts of chlorosulfonated polyethylene and 35 parts of polyvinyl alcohol; the preparation method of the garlic extract-based insect-resistant mulching film comprises the following steps:
(1) Dissolving 4 parts by weight of chlorosulfonated polyethylene in 4 parts by weight of styrene to obtain a solution A;
(2) Dissolving 0.65 weight part of ammonium persulfate initiator in 10 weight parts of deionized water to obtain solution B;
(3) Stirring the solution A obtained in the step (1), 25 parts by weight of garlic extract, 3.1 parts by weight of sodium dodecyl sulfate, 4.2 parts by weight of OP-10 emulsifier, 35 parts by weight of polyvinyl alcohol and 218 parts by weight of deionized water at the room temperature with the rotating speed of 350-360r/min for 45min to obtain emulsion C;
(4) Heating a container containing emulsion C to 80 ℃ in a water bath, dropwise adding 26 parts by weight of hydroxypropyl acrylate into the emulsion C under stirring, wherein the dripping speed is 1 drop per 2 seconds, and the stirring speed is 230-240r/min; simultaneously, dropwise adding hydroxypropyl acrylate into the emulsion C, wherein the dropwise adding speed of the solution B obtained in the step (2) is 1 drop per 5 seconds;
(5) After the dropwise addition of the hydroxypropyl acrylate and the solution B in the step (4) is finished, heating a reaction system to 87 ℃, stirring at the constant temperature for reacting for 5 hours, wherein the stirring speed is 260-270r/min, cooling the obtained mixed solution to room temperature after the constant temperature stirring reaction is finished, and adding concentrated ammonia water to adjust the pH of the mixed solution to be neutral to obtain emulsion D;
(6) Coating the emulsion D obtained in the step (5) on the surface of a polyvinyl chloride mask layer, controlling the thickness of the emulsion D layer to be 0.55mm, and drying at room temperature to obtain an insect-proof layer which is attached to the surface of the mask layer and consists of garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol;
the garlic extract-based insect-resistant mulching film of example 4 was obtained through steps (1) - (6).
Example 5
Referring to the attached drawings, the garlic extract-based insect-resistant mulching film is characterized in that a mask layer (1) and an insect-resistant layer (2) are sequentially arranged from top to bottom, the insect-resistant layer is composed of a garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer, and the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer comprises the following components in parts by weight: 30 parts of garlic extract, 30 parts of hydroxypropyl acrylate, 5 parts of styrene, 5 parts of chlorosulfonated polyethylene and 40 parts of polyvinyl alcohol; the preparation method of the garlic extract-based insect-resistant mulching film comprises the following steps:
(1) Dissolving 5 parts by weight of chlorosulfonated polyethylene in 5 parts by weight of styrene to obtain a solution A;
(2) Dissolving 0.65 weight part of ammonium persulfate initiator in 10 weight parts of deionized water to obtain solution B;
(3) Stirring 30 parts by weight of the solution A obtained in the step (1), 3.2 parts by weight of sodium dodecyl sulfate, 4.3 parts by weight of OP-10 emulsifier, 40 parts by weight of polyvinyl alcohol and 258 parts by weight of deionized water at a rotating speed of 350-360r/min at room temperature for 50min to obtain emulsion C;
(4) Heating a container containing emulsion C to 82 ℃ in a water bath, dropwise adding 30 parts by weight of hydroxypropyl acrylate into the emulsion C under stirring, wherein the dripping speed is 1 drop per 2 seconds, the stirring speed is 240-250r/min, and meanwhile, dropwise adding the solution B obtained in the step (2) into the emulsion C, wherein the dripping speed is 1 drop per 5 seconds;
(5) After the dropwise addition of the hydroxypropyl acrylate and the solution B in the step (4) is finished, heating the reaction system to 88 ℃, and stirring at the constant temperature for reacting for 5.5 hours, wherein the stirring speed is 270-280r/min; after the constant-temperature stirring reaction is finished, cooling the obtained mixed solution to room temperature, and then adding concentrated ammonia water to adjust the pH of the mixed solution to be neutral to obtain emulsion D;
(6) Coating the emulsion D obtained in the step (5) on the surface of a polyethylene mask layer, controlling the thickness of the emulsion D layer to be 0.6mm, and drying at room temperature to obtain an insect-proof layer which is attached to the surface of the mask layer and consists of garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol;
The garlic extract-based insect-resistant mulching film of example 5 was obtained through steps (1) - (6).
Comparative example 6
In this example, a mulch film was produced according to the procedure of example 3, which differs from example 3 in that the garlic extract in the production step (3) was used in an amount of 9 parts by weight, which is outside the range described in the claims, and other components, component contents, production steps and the like were the same as those of example 3.
The preparation steps of this example are as follows:
the preparation steps (1) and (2) of this example are the same as steps (1) and (2) of example 3;
(3) Mixing 9 parts by weight of the solution A obtained in the step (1), 3.1 parts by weight of sodium dodecyl sulfate, 4.1 parts by weight of OP-10 emulsifier, 30 parts by weight of polyvinyl alcohol and 181 parts by weight of deionized water at a rotating speed of 350-360r/min for 40min at room temperature to obtain emulsion C;
the preparation steps (4) to (6) of this example are the same as the steps (4) to (6) of example 3.
Comparative example 7
In this example, a mulch film was produced according to the procedure of example 3, which differs from example 3 in that the garlic extract in the production step (3) was used in an amount of 31 parts by weight, which is outside the range described in the claims, and other components, component contents, production steps and the like were the same as those of example 3. The preparation steps of this example are as follows:
The preparation steps (1) and (2) of this example are the same as steps (1) and (2) of example 3;
(3) Mixing 31 parts by weight of the solution A obtained in the step (1), 3.1 parts by weight of sodium dodecyl sulfate, 4.1 parts by weight of OP-10 emulsifier, 30 parts by weight of polyvinyl alcohol and 181 parts by weight of deionized water at a rotating speed of 350-360r/min for 40min at room temperature to obtain emulsion C;
the preparation steps (4) to (6) of this example are the same as the steps (4) to (6) of example 3.
Comparative example 8
In this example, a mulch film was produced according to the procedure described in example 3, which differs from example 3 in that the garlic extract was replaced with the garlic residue particles described in document 6 in the production step (3), and other components, component contents, production steps and the like were the same as those in example 3. The preparation steps of this example are as follows:
the preparation steps (1) and (2) of this example are the same as steps (1) and (2) of example 3;
(3) Stirring 20 parts by weight of garlic residue particles smaller than 10 meshes, 3.1 parts by weight of sodium dodecyl sulfate, 4.1 parts by weight of OP-10 emulsifier, 30 parts by weight of polyvinyl alcohol and 181 parts by weight of deionized water obtained in the step (1) at room temperature at the rotating speed of 350-360r/min for 40min to obtain emulsion C;
The preparation steps (4) to (6) of this example are the same as the steps (4) to (6) of example 3.
Comparative example 9
In this example, a mulch film was produced according to the procedure described in example 3, which differs from example 3 in that the hydroxypropyl acrylate in the production step (4) was used in an amount of 14 parts by weight, which is outside the range described in the claims, and other components, component contents, production steps and the like were the same as in example 3. The preparation steps of this example are as follows:
the preparation steps (1) to (3) of this example are the same as the steps (1) to (3) of example 3;
(4) Heating a container containing emulsion C to 80 ℃, dropwise adding 14 parts by weight of hydroxypropyl acrylate into the emulsion C under stirring, wherein the dripping speed is 1 drop every 2 seconds, the stirring speed is 230-240r/min, and meanwhile, dropwise adding the solution B obtained in the step (2) into the emulsion C, wherein the dripping speed is 1 drop every 5 seconds;
the preparation steps (5) to (6) of this example are the same as the steps (5) to (6) of example 3.
Comparative example 10
In this example, a mulch film was produced according to the procedure described in example 3, which differs from example 3 in that the styrene amount in the production step (1) was 0.8 parts by weight and the chlorosulfonated polyethylene amount was 0.8 parts by weight, which were both outside the ranges described in the claims, and other components, component contents, production steps, etc. were the same as in example 3. The preparation steps of this example are as follows:
(1) Dissolving 0.8 parts by weight of chlorosulfonated polyethylene in 0.8 parts by weight of styrene to obtain a solution A;
the remaining preparation steps of this example were the same as steps (2) - (6) of example 3.
Comparative example 11
In this example, a mulch film was produced according to the procedure described in example 3, which differs from example 3 in that the polyvinyl alcohol was used in an amount of 19 parts by weight in the production step (3) and the amount was outside the range described in the claims, and other components, component contents, production steps and the like were the same as in example 3.
The preparation steps of this example are as follows:
the preparation steps (1) and (2) of this example are the same as steps (1) and (2) of example 3;
(3) Stirring the solution A obtained in the step (1), 20 parts by weight of garlic extract, 3.1 parts by weight of sodium dodecyl sulfate, 4.1 parts by weight of OP-10 emulsifier, 19 parts by weight of polyvinyl alcohol and 181 parts by weight of deionized water at a rotating speed of 350-360r/min at room temperature for 40min to obtain emulsion C;
the preparation steps (4) to (6) of this example are the same as the steps (4) to (6) of example 3.
Comparative example 12
This example was a mulch film prepared according to the procedure described in example 3, which differs from example 3 in that sodium dodecyl sulfate was used in an amount of 2.8 parts by weight and OP-10 emulsifier was used in an amount of 3.8 parts by weight in preparation step (3), which were both outside the ranges described in the claims, and other components, component contents, preparation steps, etc. were the same as in example 3. The preparation steps of this example are as follows:
The preparation steps (1) and (2) of this example are the same as steps (1) and (2) of example 3;
(3) Stirring the solution A obtained in the step (1), 20 parts by weight of garlic extract, 2.8 parts by weight of sodium dodecyl sulfate, 3.8 parts by weight of OP-10 emulsifier, 30 parts by weight of polyvinyl alcohol and 181 parts by weight of deionized water at a rotating speed of 350-360r/min at room temperature for 40min to obtain emulsion C;
the preparation steps (4) to (6) of this example are the same as the steps (4) to (6) of example 3.
Comparative example 13
This example differs from the procedure described in example 3 in that the example uses only a garlic extract solution to coat the mask layer and the mulch film is prepared without using the raw materials of hydroxypropyl acrylate, styrene, chlorosulfonated polyethylene, polyvinyl alcohol, etc. described in examples 1 to 5. The preparation steps of this example are as follows:
20 parts by weight of garlic extract is dissolved in 181 parts by weight of deionized water, and then the obtained solution is coated on the surface of a polyethylene mask layer by using a brush, and the film is obtained after drying at room temperature.
Comparative example 14
This example is a mulch film prepared according to the procedure described in example 3, which differs from the procedure described in example 3 in that the garlic extract is not added in step (3), but is mechanically mixed with emulsion D in step (6), and the resulting mixture is smeared on the mask layer, i.e., the garlic extract is not formed into a copolymer with hydroxypropyl acrylate monomer or the like, but is simply physically mixed with the copolymer. The preparation steps of this example are as follows:
The preparation steps (1) and (2) of this example are the same as steps (1) and (2) of example 3;
(3) Stirring the solution A obtained in the step (1), 3.1 parts by weight of sodium dodecyl sulfate, 4.1 parts by weight of OP-10 emulsifier, 30 parts by weight of polyvinyl alcohol and 181 parts by weight of deionized water at the room temperature with the rotating speed of 350-360r/min for 40min to obtain emulsion C;
the preparation steps (4) and (5) of this example are the same as steps (4) and (5) of example 3;
(6) And (3) physically mixing the emulsion D obtained in the step (5) with 20 parts by weight of garlic extract at normal temperature, coating the obtained mixture on the surface of a mask layer, controlling the thickness of the mixture to be 0.5mm, and drying at room temperature to obtain the mulch film of the embodiment.
Experimental phenomena: demulsification delamination occurred when emulsion D was mixed with 20 parts by weight of garlic extract, and the resulting mixture was hardly adhered to the mask layer.
Application example 15
In this example, the mulch films obtained in example 1, example 3, example 5 and comparative examples 6 to 14 were applied to the soil surface, and the specific test procedure was as follows:
selecting a vegetable planting field, wherein the place is east longitude: 118.97539027571867 ° and north latitude: 32.066403113172214, planting Chinese cabbage in the field; in 2021, taking mulch films prepared in examples 1, 3, 5 and comparative examples 6-14 respectively, cutting the mulch films of 0.6mX0.6mX each, covering each cut mulch film over soil with the size of 0.3mX0.3mX each field, spacing 0.1m each field, uniformly sowing 30 Chinese cabbage seeds in each field, arranging the insect-preventing layer of the mulch film towards the soil, keeping the height of the mulch film from the ground by about 10cm, burying the edge of each mulch film under the ground by 2cm, compacting the edge by soil blocks, and ensuring that the enclosed space of each mulch film is a closed space.
Effect examples
This example was subjected to the following performance test for each mulch film (including the mulch films obtained in example 1, example 3, example 5, comparative examples 6 to 14) referred to in application example 15.
1. Emulsion stability test
Observing whether emulsion D formed in step 5 of each embodiment can be demulsified and layered within 3 days, if the sample is not demulsified and layered, the emulsion D is stable, and the garlic extract is uniformly distributed in the emulsion D, so that the garlic extract is uniformly distributed in an insect-preventing layer formed by the emulsion D, and the insect-preventing layer is beneficial to exerting insect-preventing effect.
2. Soil temperature test for plastic film mulching
A GPRS type soil temperature and humidity sensor (model: JXBS-7001-TR, supplier: clear-to-precision electronic technology Co., ltd.) is adopted, the sensor is used for carrying out soil temperature and humidity data transmission by means of a mobile phone signal network, the temperature of each field soil depth in application example 15 is respectively measured, the test time is 14:00-16:00 per day, the test lasts for 7 days, and the soil temperature under plastic film coverage takes the average temperature of the soil as a report value.
3. Mulch film water drop test
Selecting an area of a piece of mulching film to be 0.1m multiplied by 0.1m, and counting the average number of water drops with the inner diameter of more than 2mm in the area. The measurement time period is 2021, 11 months, 12-14 days, 3 days continuously, and the measurement time is 12 days per day: at 00 points, the average number of water droplets= (sum of 3 days of water droplet number)/3.
4. Contact angle test of mulching film facing soil
And (3) cutting 3 film samples with the same size from each example by switching on a power supply of the DSA100 optical contact angle measuring instrument, fixing the soil facing surface of the 3 film samples on a workbench upwards, forming water drops by 0.01ml of distilled water on a needle head, dripping the water drops on the surface of the film samples, standing the water drops on the film samples for 50s, rotating a cross wire in an eyepiece to serve as a tangent line at the contact point of the water drops and the film samples, and obtaining the contact angle between the tangent line and the horizontal plane of the film samples. The contact angle was measured at 3 different positions and the average value thereof was taken as the contact angle of the surface of this film sample facing the soil.
5. Light transmittance test
The size of the mulch cut specimen obtained in each example was 9.5mm×45mm. And (3) using an Shanghai prismatic light 752Pro type ultraviolet visible spectrophotometer to calibrate the baseline of the instrument, and then placing a mulching film sample on the inner wall surface of a quartz cuvette with the wavelength range of 400-800 nm and the scanning interval of 5 nm/time. Average light transmittance of mulch film samples= (sum of light transmittance of each time)/total number of tests.
6. Insect resistance experiment
The insect resistance test was performed in a greenhouse environment (25 ℃,35% humidity) and expressed as leaf breakage rate of cabbage moth on leaves of chinese cabbage. The plutella xylostella insects are collected from the farm, the collected plutella xylostella insects are firstly fed with fresh plutella xylostella for two days to eliminate the influence of original food reserves in the larvae on subsequent experiments, and then the larvae with similar body shapes are selected and divided into a plurality of groups of 10 larvae. Transplanting cabbages with similar weight and appearance into flowerpots with the same size (the diameter of each flowerpots is 10cm, the depth of each flowerpots is 5 cm), each flowerpot is provided with 450g of soil powder obtained by passing through a 5-mesh screen, 4 cabbages are transplanted into each flowerpots, each group of larvae is placed on leaf surfaces of the cabbages in each flowerpots, then the plastic films corresponding to examples 1, 3 and 5 and comparative examples 6-14 are covered on the cabbages, the distance between the top of the plastic film and the highest position of the leaf surfaces of the cabbages is 3cm, the edge of the plastic film is closed at the edge of the top of the flowerpots, and the plastic film is properly fastened by ropes, so that the experiment result is prevented from being influenced by movement of the plutella worm among cabbages in different flowerpots. After day 3, the damage of the leaf of the chinese cabbage was measured using a YMJ-a leaf surface measuring instrument. Blade breakage rate= (total damaged blade area/total original blade area) ×100%.
5. From the results in table 1, it can be seen that the performance of the mulch films of examples 1, 3, 5 was the best in each test compared to the performance of the other comparative example mulch films. The emulsion D formed in the preparation step (5) of examples 1, 3 and 5 did not undergo demulsification delamination, which indicates that the garlic extract molecules were uniformly distributed in the emulsion D, and the formed insect-repellent layer was coated with such emulsion, and the garlic extract molecules were also uniformly distributed in the formed insect-repellent layer, which enabled the prepared mulch film to have a better insect-repellent effect. The average temperature of the soil covered by the mulching films of examples 1, 3 and 5 is 0.3-7.6 ℃ higher than the average temperature of the soil covered by the mulching films of the comparative examples. The reason is that the insect-proof layers of the mulching films in the embodiments 1, 3 and 5 have high hydrophilicity (contact angle is 9-10 degrees), the number of water drops formed on the mulching films is less (1-2), no obvious water drop layer covers the waterproof layer, and therefore no water drop layer evaporates to absorb solar energy and prevent sunlight from irradiating on the soil surface; in addition, the mulch films of examples 1, 3 and 5 also have good light transmittance (70-72%), which makes sunlight more likely to penetrate through the mulch film to radiate and heat soil under the mulch film, thereby increasing the soil temperature. In the insect-resistant experiment, the damage rate (5-7%) of the mulching film of examples 1, 3 and 5 is far lower than that (15-33%) of other comparative examples, because the garlic extracts in the insect-resistant layers of the mulching films of examples 1, 3 and 5 are uniformly distributed, and no obvious water drop layer covers the insect-resistant layers, so that the insect-resistant layers can be in direct contact with the growth environment of the cabbages under the mulching films, and a better insect-resistant effect can be exerted. Obviously, the mulching films in the embodiments 1, 3 and 5 can not only raise the soil temperature, but also effectively prevent insects, and are more beneficial to agricultural production.
As for the mulch film of comparative example 6, the results in Table 1 show that the leaf breakage rate (31%) of the cabbages under the mulch film is much higher than that of examples 1, 3 and 5 by 6.2 times as much as that of example 3 (5%), because the garlic extract of comparative example 6 is used in an amount of 9 parts by weight, which is lower than the range described in the claims (10 to 30 parts by weight of garlic extract), i.e., too small an amount of garlic extract affects the insect-repellent effect of the mulch film of the present invention.
With respect to the mulch film of comparative example 7, the results of table 1 show that emulsion D formed in step (5) of comparative example 7 is demulsified and delaminated; the light transmittance is 55% and lower than that of the mulching films in examples 1, 3 and 5; the damage rate (16%) of the leaf of the cabbage under the mulching film is 3.2 times higher than that of the leaf of the embodiment 1, 3 and 5 and is 3.2 times higher than that of the embodiment 3, because the garlic extract of the comparative example 7 is used in an amount of 31 parts by weight, which is higher than the range (10-30 parts by weight) of the garlic extract described in the claims, i.e., the garlic extract is used in an excessive amount, which may cause the emulsion D formed in the step (5) to have a demulsification and delamination phenomenon, which makes the molecular distribution of the garlic extract in the insect-repellent layer uneven, affects the insect-repellent performance of the mulching film, and at the same time, the excessive garlic extract also affects the light transmittance of the mulching film, which is disadvantageous for increasing the soil temperature.
With respect to the mulch film of comparative example 8, the results of table 1 show that emulsion D formed in step (5) of comparative example 8 is broken and delaminated; the average temperature of soil under the mulch film is 9.3 ℃, which is lower than that of the mulch films of examples 1, 3 and 5 and lower than that of the mulch film of example 3 by 7.6 ℃; the light transmittance of the mulch film of comparative example 8 is 32% lower than that of the mulch films of examples 1, 3 and 5; the damage rate (15%) of the cabbage leaves under the mulch film is far higher than that of the leaves of examples 1, 3 and 5, and is 3 times that of the leaves of example 3 (5%). This is because comparative example 8 replaces the garlic extract of example 3 with light-impermeable garlic residue particles, and the mixing of the granular garlic residue with other components in the amounts of the components described in example 3 results in demulsification and delamination of emulsion D, uneven distribution of the garlic residue in the insect-repellent layer, and affects the insect-repellent effect of the mulch film insect-repellent layer of comparative example 8; in addition, the opaque garlic bits make the mulch film of comparative example 8 poor in light transmission, resulting in poor ability of sunlight to heat soil under the mulch film through the mulch film, which is limited in soil temperature elevation.
With respect to the mulch film of comparative example 9, the results of table 1 show that the emulsion D formed in step (5) of comparative example 9 delaminates; the average temperature of soil under the mulch film is 9.7 ℃, which is lower than that of the mulch films of examples 1, 3 and 5 and lower than that of the mulch film of example 3 by 7.2 ℃; the number of the mulching film water drops in the comparative example 9 is 32, which is far more than that of the mulching film water drops in the examples 1, 3 and 5; the contact angle of the mulching film is 53 degrees; the damage rate (22%) of the cabbage leaves under the mulch film is much higher than that of examples 1, 3 and 5, and is 4.4 times that of example 3 (5%). This is because the amount of hydroxypropyl acrylate used in comparative example 9 is 14 parts by weight, which is lower than the range described in the claims (15 to 30 parts by weight of hydroxypropyl acrylate), i.e., a small amount of hydroxypropyl acrylate causes emulsion D to break, indicating that an appropriate amount of hydroxypropyl acrylate is also an important factor in forming stable emulsion D; in the comparative example 9, the use amount of hydroxypropyl acrylate is small, which also results in a large contact angle of the insect-proof layer, low hydrophilicity, the insect-proof layer is easy to form a water droplet layer, and the water droplet layer evaporates to absorb solar energy, so that the capability of sunlight to heat soil under the mulch film is reduced, the soil temperature is limited in lifting range, and meanwhile, the obvious water droplet layer covers the insect-proof layer, so that the insect-proof layer cannot be in direct contact with the growth environment of the cabbages under the mulch film, and the insect-proof effect of the mulch film of the comparative example 9 is reduced.
With respect to the mulch film of comparative example 10, the results of table 1 show that the average temperature of the soil under the mulch film of comparative example 10 is 10.9 ℃, lower than the average temperature of the soil under the mulch films of examples 1, 3, 5, lower than the mulch film of example 3 by 6 ℃; the number of the mulching film water drops in the comparative example 10 is 21, which is far more than that in the examples 1, 3 and 5; the contact angle of the mulching film is 37 degrees; the damage rate (20%) of the cabbage leaves under the mulch film is much higher than that of examples 1, 3 and 5, and is 4 times that of example 3 (5%). This is because the styrene amount is 0.8 weight part and the chlorosulfonated polyethylene amount is 0.8 weight part in comparative example 10, both of which are lower than the ranges described in the claims (1-5 weight parts of styrene and 1-5 weight parts of chlorosulfonated polyethylene), the styrene and chlorosulfonated polyethylene can improve the adhesion stability of the insect-repellent layer on the mask layer, and the too low amounts of styrene and chlorosulfonated polyethylene in comparative example 10 make the insect-repellent layer have a certain peeling in the use process of the mulch film, and the partially hydrophobic mask layer is exposed, so that the overall hydrophilicity of the insect-repellent layer becomes poor, so that the insect-repellent layer becomes more water droplets, and in the same way, the temperature-elevating range of soil under the mulch film and the insect-repellent effect of the insect-repellent layer are also reduced by the mulch film with poor hydrophilicity.
With respect to the mulch film of comparative example 11, the results in table 1 show that the average temperature of the soil under the mulch film of comparative example 11 is 9.9 ℃, which is lower than the average temperature of the soil under the mulch films of examples 1, 3, 5, which is lower than the mulch film of example 3 by 7 ℃; the number of the mulching film water drops in the comparative example 11 is 35, which is far more than that of the mulching film water drops in the examples 1, 3 and 5; the contact angle of the mulching film is 89 degrees; the damage rate (25%) of the cabbage leaves under the mulch film is far higher than that of the leaves of examples 1, 3 and 5, and is 5 times that of the leaves of example 3. This is because the amount of polyvinyl alcohol used in comparative example 11 is 19 parts by weight, which is lower than the range described in the claims (20 to 40 parts by weight of polyvinyl alcohol), and the amount of polyvinyl alcohol used in comparative example 11 is small, resulting in a large contact angle of the insect-repellent layer, low hydrophilicity, the insect-repellent layer being prone to water droplet formation, and the water droplet layer evaporating to absorb solar energy, reducing the ability of sunlight to heat the soil under the mulch, and the soil temperature elevation being limited, while the apparent water droplet layer covers the insect-repellent layer, so that the insect-repellent layer cannot directly contact with the growth environment of the chinese cabbage under the mulch, and the insect-repellent effect of the mulch of comparative example 11 is reduced.
With respect to the mulch film of comparative example 12, the results of table 1 show that emulsion D formed in step (5) of comparative example 12 is broken and layered; the average temperature of soil under the mulch film is 11.4 ℃, which is lower than that of the mulch films of examples 1, 3 and 5, and is 5.5 ℃ lower than that of the mulch film of example 3; the number of the mulching film water drops in the comparative example 12 is 17, which is more than that of the mulching film water drops in the examples 1, 3 and 5; the contact angle of the mulching film is 41 degrees; the damage rate (28%) of the cabbage leaves under the mulch film is far higher than that of the leaves of examples 1, 3 and 5, and is 5.6 times that of the leaves of example 3 (5%). This is because the amount of sodium dodecyl sulfate used in comparative example 12 was 2.8 parts by weight, the amount of OP-10 emulsifier used was 3.8 parts by weight, both of which were less than the ranges described in the claims (2.9 to 3.2 parts by weight of sodium dodecyl sulfate, 3.9 to 4.3 parts by weight of OP-10 emulsifier), the sodium dodecyl sulfate and OP-10 emulsifier served as surfactants so that the components could be uniformly mixed together, and further an insect-repellent layer in which the components could be uniformly distributed was obtained by emulsion polymerization; however, in comparative example 12, the amount of surfactant used was insufficient to break and delaminate the emulsion D, the components could not be uniformly distributed, and the hydrophilic components of hydroxypropyl acrylate and polyvinyl alcohol could not be uniformly distributed in the coating layer to make the insect-repellent layer have poor hydrophilicity and the surface was liable to be water-beaded, and the components of garlic extract could not be uniformly distributed, which all reduced the insect-repellent effect of the mulch film of comparative example 12.
For the mulch of comparative example 13, which did not involve the preparation of emulsion D, the results in table 1 show that the number of mulch beads of comparative example 13 was 42, which is far greater than the number of mulch beads of examples 1, 3, 5; the contact angle of the mulching film is 106 degrees; the damage rate (33%) of the cabbage leaves under the mulch film is far higher than that of the leaves of examples 1, 3 and 5, and is 6.6 times of that of the leaves of example 3 (5%). This is because the comparative example 13 was simply coated on the mask layer with only the garlic extract solution, the other raw materials described in example 3 were not used, the garlic extract itself was not adhesive, and the solution was hardly adhered to the mask layer, which resulted in almost no garlic extract being coated on the surface of the mask layer, which resulted in exposing the hydrophobic mask layer to the outside, resulting in a large contact angle of the mulching film, poor hydrophilicity, many water drops of the mulching film, and this mulching film without an effective garlic extract coating layer had poor natural insect-resistant effect.
In the case of the mulching film of comparative example 14, in this example, the garlic extract was not added in step (3), but mechanically mixed with emulsion D in step (6), and the resulting mixture was smeared on the mask layer, i.e., the garlic extract did not form a copolymer with hydroxypropyl acrylate monomer or the like, but was simply physically mixed with the copolymer. In the embodiment, when emulsion D and 20 parts by weight of garlic extract are physically mixed, demulsification and layering occur, the obtained mixture is difficult to adhere to a mask layer, so that the emulsion stability can be destroyed due to the fact that a large amount of garlic extract which does not undergo copolymerization is in direct contact with the emulsion, the emulsion is demulsified and layered, the garlic extract is unevenly distributed in the demulsified solution, and the copolymer has a high molecular chain conformation which changes, so that the adhesiveness of the copolymer is obviously reduced; meanwhile, if the layered demulsification mixture is coated on the mask layer, the light transmittance of the mask layer is seriously reduced by the layered demulsification mixture; the layered demulsified mixture also resulted in a coating that was poor in hydrophilicity and prone to beading, which could prevent the garlic extract from directly contacting the under-film crop growth environment, which resulted in poor insect control of the mulch film of example 14. The results in Table 1 show that the average temperature of the soil under the mulch film of example 14 is 11.1 ℃ which is lower than the average temperature of the soil under the mulch films of examples 1, 3 and 5, which is lower than the average temperature of the soil under the mulch film of example 3 by 5.8 ℃; the contact angle (45 ℃) of the mulching film and the number (31) of the water drops formed in the comparison example 14 are far higher than those of the mulching films in examples 1, 3 and 5; comparative example 14 the leaf breakage rate (26%) of the cabbages under the mulch film was much higher than that of examples 1, 3 and 5, and 5.2 times the leaf breakage rate (5%) of example 3.
Table 1 experimental results in emulsion stability, soil temperature, water droplet formation, contact angle, light transmittance, and plutella xylostella resistance tests of example 1, example 3, example 5, comparative examples 6 to 14, "-" represents that the test of the corresponding item was not performed.
Claims (6)
1. The garlic extract-based insect-resistant mulching film is characterized in that a mask layer (1) and an insect-resistant layer (2) are sequentially arranged from top to bottom, the mask layer is made of polyethylene or polyvinyl chloride, the insect-resistant layer is composed of a garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer, and the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer comprises the following components in parts by weight: 10-30 parts of garlic extract, 15-30 parts of hydroxypropyl acrylate, 1-5 parts of styrene, 1-5 parts of chlorosulfonated polyethylene and 20-40 parts of polyvinyl alcohol; the garlic extract is water-soluble powder; the preparation method of the garlic extract-based insect-resistant mulching film comprises the following steps:
(1) 1-5 parts by weight of chlorosulfonated polyethylene is dissolved in 1-5 parts by weight of styrene to obtain a solution A;
(2) Dissolving 0.65 weight part of ammonium persulfate initiator in 10 weight parts of deionized water to obtain solution B;
(3) Stirring 10-30 parts by weight of the solution A obtained in the step (1), 2.9-3.2 parts by weight of sodium dodecyl sulfate, 3.9-4.3 parts by weight of OP-10 emulsifier, 20-40 parts by weight of polyvinyl alcohol and 107-258 parts by weight of deionized water at the room temperature with the rotating speed of 350-360r/min for 30-50min to obtain emulsion C;
(4) Heating a container containing emulsion C to 75-82 ℃ in a water bath, dropwise adding 15-30 parts by weight of hydroxypropyl acrylate into the emulsion C under stirring, wherein the dropwise adding speed is 1 drop per 2 seconds, the stirring speed is 200-250r/min, and meanwhile, dropwise adding the hydroxypropyl acrylate into the solution B obtained in the step (2), wherein the dropwise adding speed is 1 drop per 5 seconds;
(5) After the dripping of the hydroxypropyl acrylate and the solution B in the step (4) is finished, heating the reaction system to 85-88 ℃, and stirring at the constant temperature for reacting for 4.5-5.5 hours, wherein the stirring speed is 220-280r/min; after the constant-temperature stirring reaction is finished, cooling the obtained mixed solution to room temperature, and then adding concentrated ammonia water to adjust the pH of the mixed solution to be neutral to obtain emulsion D;
(6) Coating the emulsion D obtained in the step (5) on the surface of a mask layer, controlling the thickness of the emulsion D layer to be 0.4-0.6mm, and drying at room temperature to obtain an insect-preventing layer which is attached to the surface of the mask layer and consists of garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol;
The garlic extract-based insect-resistant mulching film can be obtained through the steps (1) - (6).
2. The garlic extract-based insect-resistant mulch film according to claim 1, wherein the garlic extract-hydroxypropyl acrylate-styrene-chlorosulfonated polyethylene-polyvinyl alcohol copolymer comprises the following components in parts by weight: 20 parts of garlic extract, 22 parts of hydroxypropyl acrylate, 3 parts of styrene, 3 parts of chlorosulfonated polyethylene and 30 parts of polyvinyl alcohol.
3. The garlic extract-based insect-resistant mulch film according to claim 1, wherein the chlorosulfonated polyethylene in the preparation step (1) is 3 parts by weight and the styrene is 3 parts by weight.
4. The garlic extract-based insect-resistant mulch film according to claim 1, wherein the container with emulsion C in the preparation step (4) is heated to 80 ℃ in a water bath.
5. The garlic extract-based insect-resistant mulch film according to claim 1, wherein the reaction system in the preparation step (5) after the completion of the dropping of the hydroxypropyl acrylate and the solution B in the step (4) is warmed to 87 ℃.
6. The garlic extract-based insect-resistant mulching film according to claim 1, wherein the thickness of the layer D of the control emulsion in the preparation step (6) is 0.5mm.
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CN202310867821.4A CN116903905A (en) | 2022-02-22 | 2022-02-22 | Preparation method of mulching film based on garlic extract and hydroxypropyl acrylate copolymer |
CN202310867819.7A CN116903904A (en) | 2022-02-22 | 2022-02-22 | Garlic extract-based insect-resistant mulching film compounded with chlorosulfonated polyethylene |
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