CN111165242B - Fertilizer type biodegradable mulching film and preparation method thereof - Google Patents
Fertilizer type biodegradable mulching film and preparation method thereof Download PDFInfo
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- CN111165242B CN111165242B CN202010065238.8A CN202010065238A CN111165242B CN 111165242 B CN111165242 B CN 111165242B CN 202010065238 A CN202010065238 A CN 202010065238A CN 111165242 B CN111165242 B CN 111165242B
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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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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01C—PLANTING; SOWING; FERTILISING
- A01C15/00—Fertiliser distributors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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- C08K13/02—Organic and inorganic ingredients
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- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/3045—Sulfates
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C08K5/21—Urea; Derivatives thereof, e.g. biuret
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- Y02A40/28—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture specially adapted for farming
Abstract
The invention relates to the technical field of biodegradable mulching films, in particular to a fertilizer type biodegradable mulching film and a preparation method thereof. The fertilizer type biodegradable mulching film is prepared from the following raw materials: 70.0-95.0 parts of biodegradable plastic, 0.5-30.0 parts of fertilizer, 0-15.0 parts of lubricant, 0-2.0 parts of light stabilizer, 0-1.5 parts of antioxidant, 0-2.0 parts of chain extender and 0-6.0 parts of color master batch. The fertilizer type biodegradable mulching film can provide or supplement fertilizer for crops in a growth period, the fertilizer is released after degradation, a plurality of fine holes are formed in the mulching film, the mulching film can fully react with moisture and microorganisms in the environment, so that the degradation is accelerated, the mulching film residue in the crop harvesting period is reduced or eliminated, the crop harvesting and the straw recycling are facilitated, part of the crop film uncovering process can be omitted, and the film uncovering cost is saved.
Description
Technical Field
The invention relates to the technical field of biodegradable mulching films, in particular to a fertilizer type biodegradable mulching film and a preparation method thereof.
Background
The mulching film makes great contribution to the increase of both production and income of agriculture in China, but also causes serious white pollution. Under the premise that the mulching film covering technology cannot be replaced and a residual film recycling system is not complete, the popularization of the biodegradable mulching film is one of important technical approaches for solving the residual film pollution.
The degradable plastics which have been applied to biodegradable mulching films at present are mainly polyester products including poly (terephthalic acid)/butylene adipate (PBAT), poly (succinic acid)/butylene adipate (PBSA), poly (lactic acid) (PLA), poly (propylene carbonate) (PPC), Polyhydroxyalkanoate (PHA), poly (butylene succinate) (PBS), and the like. These materials have a fully biodegradable property and can be finally decomposed into carbon dioxide and water under the action of microorganisms under natural conditions. Compared with the traditional mulching film, the mulching film prepared from the plastic has uncontrollable degradation and higher cost, and prevents large-scale popularization and application of the mulching film.
In order to solve the problems of the biodegradable mulching film, people make efforts in various aspects such as material modification, formula and process of the biodegradable mulching film, wherein part of the efforts is to combine the fertilizer with the biodegradable mulching film so as to increase the fertilizer slow release function of the biodegradable mulching film. Patents CN 108359224 a and CN 108485207 a disclose a fully-degradable mulching film with effect of slow release of nitrogen fertilizer and a preparation method thereof, and a fully-degradable mulching film with effect of slow release of phosphate fertilizer and a preparation method thereof, respectively. The two inventions respectively utilize ammoniated lignin, phosphatized lignin and degradable plastics to synthesize the biodegradable mulching film for slowly releasing nitrogen fertilizer and phosphate fertilizer. However, the biodegradable mulching film fertilizer produced by blending lignin and degradable plastics has low utilization efficiency, poor light transmittance due to brown color and strong hydrophilicity and water permeability, and the temperature and soil moisture increasing and preserving function does not meet the growth requirements of most crops, so the biodegradable mulching film fertilizer is difficult to be practically applied; meanwhile, the method provided by the invention needs to perform ammoniation or phosphorization treatment on lignin, so that the processing cost is increased.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a fertilizer type biodegradable mulching film and a preparation method thereof. The invention mixes the fertilizer with biodegradable plastic and other additives directly after crushing and grading (coating or surface modification) to produce the biodegradable mulching film which can be completely biodegraded and can supplement the fertilizer required by the growth of crops, thereby improving the application value of the biodegradable mulching film, indirectly reducing the use cost of the biodegradable mulching film and adjusting the proportion of the fertilizer according to the requirements of the growth rules of different crops. The micro-pores created while they degrade also accelerate their degradation, allowing them to degrade almost completely at the end of the growth period. The invention is beneficial to reducing the comprehensive use cost of the biodegradable mulching film, can reduce the residue in the harvest period and promote the effective utilization of wastes such as straws and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a fertilizer type biodegradable mulching film is prepared from the following raw materials: 70.0-95.0 parts of biodegradable plastic, 0.5-30.0 parts of fertilizer, 0-15 parts of lubricant, 0-2.0 parts of light stabilizer, 0-1.5 parts of antioxidant, 0-2.0 parts of chain extender and 0-6.0 parts of color master batch.
Preferably, the fertilizer type biodegradable mulching film is prepared from the following raw materials: 85-95 parts of biodegradable plastic, 5-15 parts of fertilizer, 0-2.0 parts of lubricant, 0.1-2.0 parts of light stabilizer, 0-1.5 parts of antioxidant, 0-2.0 parts of chain extender and 0-6.0 parts of color master batch.
Preferably, in the fertilizer-type biodegradable mulching film, the biodegradable plastic is selected from one or more of polybutylene adipate/terephthalate, polybutylene succinate/adipate, polylactic acid, polypropylene carbonate, polyhydroxyalkanoate and polybutylene succinate.
Preferably, in the fertilizer-type biodegradable mulching film, the fertilizer is selected from any one or more of a nitrogen fertilizer, a phosphate fertilizer, a potassium fertilizer, a boron fertilizer, a calcium fertilizer, a magnesium fertilizer, a copper fertilizer, a molybdenum fertilizer, a manganese fertilizer and an iron fertilizer, and more preferably, the fertilizer is selected from any one or more of urea, uric acid, ammonium nitrate, ammonium bicarbonate, ammonium sulfate, diammonium phosphate, ammonium dihydrogen phosphate, calcium superphosphate, triple superphosphate, potassium nitrate, potassium oxide, potassium sulfate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, zinc nitride, boron nitride and talcum powder.
Preferably, in the fertilizer type biodegradable mulching film, the fertilizer is a liquid fertilizer or a solid fertilizer, and the solid fertilizer is a 1000-5000 mesh powdery fertilizer or a flaky fertilizer with a thickness of less than or equal to 10 micrometers.
Preferably, in the fertilizer type biodegradable mulching film, the powdery fertilizer is a coated powdery fertilizer, and more preferably, the coating material used for the coated powdery fertilizer is one or more of cellulose and derivatives thereof, sodium alginate, chitosan and derivatives thereof, starch and derivatives thereof, polyethylene glycol, polyvinyl alcohol, gelatin, sodium hyaluronate or polylactic acid.
Preferably, in the fertilizer-type biodegradable mulching film, the sheet-shaped fertilizer is a coated sheet-shaped fertilizer or a sheet-shaped fertilizer modified by a silane coupling agent, and more preferably, the coating material used for the coated sheet-shaped fertilizer is one or more of cellulose and derivatives thereof, sodium alginate, chitosan and derivatives thereof, starch and derivatives thereof, polyethylene glycol, polyvinyl alcohol, gelatin, sodium hyaluronate or polylactic acid.
Preferably, in the fertilizer-type biodegradable mulching film, the lubricant is selected from one or more of talc, oleic acid, oleamide, diatomite, silicon dioxide, zinc stearate, calcium stearate, vinyl bis stearamide, soybean oil, rapeseed oil and peanut oil.
Preferably, in the fertilizer-type biodegradable mulch film, the light stabilizer is selected from one or more of salicylates, benzophenones, benzotriazoles, substituted acrylonitriles, triazines, carbon black, iron oxide red and zinc oxide.
Preferably, in the fertilizer-type biodegradable mulch film, the antioxidant is selected from any one or more of monophenol, bisphenol, triphenol, polyphenol, hydroquinone, thiobisphenol, naphthylamine, diphenylamine, p-phenylenediamine, quinoline derivatives, phosphites and thioesters.
Preferably, in the fertilizer type biodegradable mulching film, the color master is selected from any one or more of M900, 330BK and KO 3300.
The invention also provides a preparation method of the fertilizer type biodegradable mulching film, which comprises the following steps: and weighing biodegradable plastic, fertilizer and optionally added lubricant, chain extender, light stabilizer, antioxidant and color master batch according to the weight ratio, mixing, transferring the obtained mixed material into an extrusion molding machine for extrusion molding, and performing granulation and blow molding to form a film to obtain the fertilizer type biodegradable mulching film.
Preferably, the preparation method comprises the following steps:
(1) mixing the ingredients: weighing biodegradable plastic, fertilizer and selectively added lubricant, chain extender, light stabilizer, antioxidant and color master batch according to the weight ratio, putting the mixture into a stirrer for mixing, wherein the stirring speed is 1000-3500r/min, and the stirring time is 50-300 s;
(2) and (3) extruding and granulating: transferring the mixed material obtained in the step (1) into a double-screw extruder to carry out extrusion molding, wherein the extrusion temperature is 140-;
(3) and (3) blow molding to form a film: and (3) carrying out blow molding on the master batch obtained in the step (2) to form a film, so as to obtain the fertilizer type biodegradable mulching film with the width of 0.5-4.5m, and preferably, carrying out hot melt extrusion blow molding on the master batch through a single-screw or double-screw extrusion film blowing machine at the processing temperature of 120-170 ℃ to form a plastic film.
The invention has the following beneficial effects:
1. according to the fertilizer type biodegradable mulching film provided by the invention, the biodegradable plastic forms a thin protective layer around the fertilizer, once the mulching film starts to degrade, the protective layer firstly occurs around the fertilizer, so that the fertilizer is easily released, and therefore, the fertilizer can supplement required nutrition for crops in the middle and later periods of crop growth, is beneficial to crop growth, and prevents diseases or yield reduction caused by element deficiency;
2. the fertilizer type biodegradable mulching film provided by the invention is released after the degradation starts, so that a plurality of fine holes are formed in the mulching film, the mulching film can fully react with moisture and microorganisms in the environment, the degradation is accelerated, the residual mulching film in the crop harvesting period is reduced or completely eradicated, the crop harvesting and the straw recycling are facilitated, a part of crop film uncovering process can be omitted, and the film uncovering cost is effectively saved.
Drawings
Fig. 1 is a scanning electron microscope image of the fertilizer-type biodegradable mulch film prepared in example 1.
Fig. 2 is a scanning electron microscope image of the biodegradable mulch film prepared without fertilizer addition in example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited thereto.
The examples, where specific experimental procedures or conditions are not indicated, were carried out according to the procedures or conditions of the conventional experimental procedures described in the literature in the field. The reagents and instruments used are not indicated by manufacturers, and can be purchased in the market.
Example 1
A biodegradable mulching film comprises the following raw materials: 73.0 parts of PBAT, 20.0 parts of sodium alginate coated urea (2000 meshes, the content of the urea is 50%), 5.0 parts of talcum powder, 38531.0 parts of ultraviolet stabilizer UV, and 9001.0 parts of antioxidant B.
The preparation method of the sodium alginate coated urea (2000 meshes) comprises the following steps:
(1) taking a 2% sodium alginate solution as a water phase, adding urea, and uniformly stirring;
(2) adding Span-80 into isooctane solution as oil phase, stirring, and preheating in 40 deg.C water bath for 10 min;
(3) dropwise adding sodium alginate solution containing urea into oil phase while stirring, continuously stirring at high speed for 60min, and dropwise adding 8% CaCl2Stirring the solution and emulsifying for 30min, washing with anhydrous ethanol and distilled water, drying at room temperature, and filtering to obtain sodium alginate coated urea;
(4) crushing the sodium alginate coated urea by an air separation crusher, air separating to obtain granules and powder with different meshes, and taking the 2000-mesh sodium alginate coated urea for later use.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, sodium alginate coated urea, talcum powder, ultraviolet stabilizer UV3853 and antioxidant B900 according to the weight ratio, and putting the mixture into a high-speed stirrer to be mixed, wherein the stirring speed is 1500r/min, and the stirring time is 120 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be between 125 and 145 ℃, and the rotating speed of the screw is adjusted to control the feeding speed, so that the fertilizer type biodegradable mulching film with the thickness of 18 mu m is obtained.
Fig. 1 is a scanning electron microscope image of the fertilizer-type biodegradable mulch film prepared in this example, which shows that the biodegradable polyester has uniformly dispersed micron-sized fertilizer particles.
Fig. 2 is a scanning electron microscope image of the biodegradable mulch film prepared according to the preparation method of the present example, without fertilizer added to the raw materials, and it can be seen from the image that the surface is flat and uniform.
The performance of the biodegradable mulch film of this example was as follows:
(1) under the field covering condition, the covering period can reach more than 60 days (no obvious degradation occurs within 60 days), and the degradation rate of field covering for six months can reach more than 80%;
(2) calculated according to the usage amount of 15 kg per mu of land, about 1.5 kg of urea can be slowly released and supplemented in the middle growth period of crops;
(3) the biodegradable mulching film can be used for corn, vegetables, processed tomatoes, potatoes, sugar beets and other crops meeting the coverage period and nitrogen requirement required by the growth of the crops.
Example 2
A biodegradable mulching film comprises the following raw materials: 70.0 parts of PBAT, 13.0 parts of PLA, 10.0 parts of chitosan coated ammonium dihydrogen phosphate microspheres (2500 meshes, the content of ammonium dihydrogen phosphate is 20%), 5.0 parts of mica sheets, 0.5 part of oleic acid, 0.78 part of chain extender ADR-44000.5, 3260.5 parts of UV stabilizer and 2150.5 parts of antioxidant.
The preparation method of the chitosan coated ammonium dihydrogen phosphate microsphere comprises the following steps:
(1) dissolving chitosan with 2% glacial acetic acid, adding ammonium monohydrogen phosphate, and stirring;
(2) adding Span-80 into liquid paraffin serving as an oil phase, uniformly stirring, slowly adding the standby mixed solution in the step (1) in a constant-temperature water bath at 40 ℃ under the stirring condition of 1500r/min, and continuously stirring for 1 h;
(3) adding a certain amount of glutaraldehyde, and continuing to stir at the speed of 1500r/min for reaction for 3 hours;
(4) standing and layering, respectively washing the lower layer mixture with petroleum ether, isopropanol and distilled water for three times, and drying to obtain chitosan coated ammonium monohydrogen phosphate;
(5) crushing chitosan-coated ammonium monohydrogen phosphate by a winnowing crusher, winnowing to obtain particles and powder with different meshes, and taking 2500-mesh chitosan-coated ammonium monohydrogen phosphate for later use.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, PLA, chitosan coated ammonium monohydrogen phosphate, mica sheets, oleic acid, chain extender ADR-4400, ultraviolet stabilizer UV326 and antioxidant B215 according to the weight ratio, putting into a high-speed stirrer, and mixing at the stirring speed of 2000r/min for 300 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be 130-150 ℃, and the rotating speed of the screw is adjusted to control the feeding speed, so that the fertilizer type biodegradable mulching film with the thickness of 15 mu m is obtained.
The performance of the biodegradable mulch film of this example was as follows:
(1) under the field covering condition, the covering period can reach more than 50 days (no obvious degradation occurs within 50 days), and the degradation rate of the field covering for six months can reach more than 90 percent;
(2) calculated according to the dosage of 12 kg per mu of land, about 0.24 kg of ammonium dihydrogen phosphate fertilizer can be supplemented in the middle growth stage of crops;
(3) the biodegradable mulching film can be used for rice, corn, potatoes, tobacco and other crops meeting the coverage period and nitrogen and phosphorus requirements needed by the growth of the crops.
Example 3
A biodegradable mulching film comprises the following raw materials: 60.0 parts of PBAT, 10.0 parts of PPC, 10.0 parts of polyvinyl alcohol coated ammonium monohydrogen phosphate microspheres (5000 meshes, the ammonium monohydrogen phosphate content is 50%), 10.0 parts of potassium sulfate (5000 meshes), 5.0 parts of modified talcum powder, 10.78 parts of ultraviolet stabilizer UV 38531.0, 2251.0 parts of antioxidant B, and 3.0 parts of carrier-free black master 330 BK.
The preparation method of the polyvinyl alcohol coated ammonium dihydrogen phosphate microspheres comprises the following steps:
(1) preparing a PVA solution with the mass fraction of 5% as a water phase, adding ammonium monohydrogen phosphate, and uniformly stirring;
(2) adding Span-80 into liquid paraffin as oil phase, and stirring;
(3) adding the water phase which is fully and uniformly mixed into the oil phase, adding 2.0g of STMP cross-linking agent, adding 1mL of NaOH as a catalyst, and reacting for 6h at the rotating speed of 2000r/min and the temperature of 50 ℃;
(4) after the reaction, the mixture was allowed to stand for 30 min. Adding small amount of anhydrous ethanol, centrifuging in a centrifuge, collecting supernatant, washing precipitate with anhydrous ethanol, isopropanol and pure water repeatedly, and drying in a forced air drying oven for 24 hr to obtain white powder.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, PPC, polyvinyl alcohol coated monoammonium phosphate microspheres, potassium sulfate, modified talcum powder, ultraviolet stabilizer UV3853, antioxidant B225 and carrier-free black master batch 330BK according to the weight ratio, and putting the mixture into a high-speed stirrer for mixing at the stirring speed of 3000r/min for 60 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 170-200 ℃, the rotating speed of screws at 180r/min, melting and blending the uniformly mixed materials by the double-screw extruder, cooling the uniformly mixed materials to 25 ℃ by air cooling or water cooling, and sealing and storing the uniformly mixed materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be 140-155 ℃, the rotating speed of the screw is adjusted to control the feeding speed, and the fertilizer type biodegradable mulching film with the thickness of 20 mu m is obtained.
The performance of the biodegradable mulch film of this example was as follows:
(1) under the field covering condition, the covering period can reach more than 80 days (no obvious degradation occurs in 80 days), and the degradation rate of the field covering for six months can reach more than 85 percent;
(2) calculated according to the dosage of 10 kilograms per mu of land, about 0.5 kilogram of ammonium dihydrogen phosphate fertilizer and 1.0 kilogram of potassium sulfate can be supplemented in the middle growth period of crops;
(3) the biodegradable mulching film can be used for crops which have a long covering period and need to be supplemented with nitrogen, phosphorus and potassium fertilizers;
(4) the biodegradable mulching film also has the effect of inhibiting weeds.
Example 4
A biodegradable mulching film comprises the following raw materials: 92.0 parts of PBAT, 5.0 parts of zinc borate (5000 meshes), 0.5 part of ethylene bis stearamide, 54111.5 parts of ultraviolet stabilizer UV, and 61.0 parts of antioxidant Irganox 10761.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, zinc borate (5000 meshes), ethylene bis stearamide, a UV stabilizer UV54111.5 and an antioxidant Irganox1076 according to the weight ratio, and putting into a high-speed stirrer for mixing at the stirring speed of 1000r/min for 240 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be between 125 and 145 ℃, and the rotating speed of the screw is adjusted to control the feeding speed, so that the fertilizer type biodegradable mulching film with the thickness of 10 mu m is obtained.
The performance of the biodegradable mulch film of this example was as follows:
(1) under the field covering condition, the covering period can reach more than 60 days (no obvious degradation occurs within 60 days), and the degradation rate of field covering for six months can reach more than 90 percent;
(2) calculated according to the dosage of 10 kilograms of fertilizer per mu of land, 0.5 kilogram of boron-zinc fertilizer can be supplemented in the middle growth stage of crops;
(3) the biodegradable mulching film can be used for corn, citrus, grape and other crops meeting the coverage period and boron and zinc requirements required by the growth of the crops;
(4) the biodegradable mulching film also has antibacterial, antiseptic and disease-resistant effects.
Example 5
A biodegradable mulching film comprises the following raw materials: 87.5 parts of PBAT, 2.0 parts of multi-element liquid fertilizer (containing nine trace elements of calcium, magnesium, iron, zinc, boron, manganese, molybdenum, copper and titanium, the manufacturer: Qingdao Jinfunongfei Co., Ltd.), 10.0 parts of talcum powder and 2150.5 parts of antioxidant B.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, a multi-element liquid fertilizer, talcum powder and an antioxidant B215 according to the weight ratio, and putting the mixture into a high-speed stirrer for mixing at the stirring speed of 2000r/min for 180 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be between 125 and 145 ℃, and the rotating speed of the screw is adjusted to control the feeding speed, so that the fertilizer type biodegradable mulching film with the thickness of 6 mu m is obtained.
The performance of the biodegradable mulch film of this example was as follows:
(1) under the field covering condition, the covering period can reach more than 40 days (no obvious degradation occurs in 40 days), and the degradation rate of the field covering for six months can reach more than 95 percent;
(2) 0.2 kg of calcium-zinc-copper-magnesium-boron compound fertilizer can be supplemented in the middle growth period of crops according to the dosage of 10 kg per mu of land;
(3) the biodegradable mulching film can be used for supplementing trace fertilizer for various crops.
Example 6
A biodegradable mulching film comprises the following raw materials: 92.0 parts of PBAT, 5.0 parts of boron nitride (manufacturer: Shanghai Longjin metal materials Co., Ltd., sheet shape, average thickness of 1 micron, controlled within 5 microns, average diameter of 20 microns, controlled within 100 microns), 2.0 parts of zinc nitride powder, 0.5 part of oleamide and 0.78 part of light stabilizer UV-3280.5.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, boron nitride, zinc nitride powder, oleamide and a light stabilizer UV-328 according to the weight ratio, and putting the PBAT, the boron nitride, the zinc nitride powder, the oleamide and the light stabilizer UV-328 into a high-speed stirrer for mixing, wherein the stirring speed is 1500r/min, and the stirring time is 240 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be between 125 and 145 ℃, and the rotating speed of the screw is adjusted to control the feeding speed, so that the fertilizer type biodegradable mulching film with the thickness of 12 mu m is obtained.
The performance of the biodegradable mulch film of this example was as follows:
(1) the longitudinal tensile load is 3.14N, and the elongation at break is 254%; the right angle tear load is 1.45N;
(2) under the field covering condition, the covering period can reach more than 50 days (no obvious degradation occurs within 50 days), and the degradation rate of the field covering for six months can reach more than 90 percent;
(3) calculated according to the dosage of 10 kilograms of fertilizer per mu of land, 0.5 kilogram of boron nitride and 0.2 kilogram of zinc nitride fertilizer can be supplemented in the middle growth period of crops;
(4) the biodegradable mulching film can be used for supplementing nitrogen, boron and zinc fertilizers for various crops.
Example 7
A biodegradable mulching film comprises the following raw materials: 92.0 parts of PBAT, 5.0 parts of polylactic acid coated boron nitride (the boron nitride content is 80 percent, the boron nitride is purchased from Shanghai Longjin metal materials Co., Ltd., sheet shape, the average thickness is 1 micron, the average diameter is controlled within 5 microns, the average diameter is 20 microns, the average diameter is controlled within 100 microns), 2.0 parts of zinc nitride powder, 0.5 part of oleamide and UV-3280.5 parts.
The preparation method of the polylactic acid coated boron nitride comprises the following steps:
(1) dissolving polylactic acid with the molecular weight of 5000 in chloroform, and adding boron nitride under the stirring condition according to the mass ratio of the polylactic acid to the boron nitride of 1: 4;
(2) subjecting the mixture to ultrasonic treatment for 5 min;
(3) and (3) carrying out spray drying on the mixture by using an organic solvent spray dryer to obtain the polylactic acid coated boron nitride fertilizer, and crushing for later use.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, polylactic acid coated boron nitride, zinc nitride powder, oleamide and a light stabilizer UV-328 according to the weight ratio, and putting the mixture into a high-speed stirrer for mixing, wherein the stirring speed is 1500r/min, and the stirring time is 240 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be between 125 and 145 ℃, and the rotating speed of the screw is adjusted to control the feeding speed, so that the fertilizer type biodegradable mulching film with the thickness of 12 mu m is obtained.
The performance of the biodegradable mulch film of this example was as follows:
(1) the longitudinal tensile load is 3.86N, and the elongation at break is 334 percent; right angle tear load 1.96N;
(2) under the field covering condition, the covering period can reach more than 50 days (no obvious degradation occurs within 50 days), and the degradation rate of the field covering for six months can reach more than 90 percent;
(3) calculated according to the dosage of 10 kilograms of fertilizer per mu of land, 0.4 kilogram of boron nitride and 0.2 kilogram of zinc nitride fertilizer can be supplemented in the middle growth period of crops;
(4) the biodegradable mulching film can be used for supplementing nitrogen, boron and zinc fertilizers for various crops.
In the embodiment, a low molecular weight polymer coating method is adopted, so that on one hand, polylactic acid can form a polymer coating on the surface of boron nitride to improve the compatibility of the boron nitride with degradable plastics, and on the other hand, the stacking of the lamellar boron nitride in the prepared biodegradable mulching film can be improved, and the mechanical property of the biodegradable mulching film is improved.
Example 8
A biodegradable mulching film comprises the following raw materials: 92.0 parts of PBAT, 5.0 parts of chitosan coated boron nitride (the boron nitride content is 80 percent, the boron nitride is purchased from Shanghai Longjin metal materials Co., Ltd., sheet shape, the average thickness is 1 micron, the average diameter is controlled within 5 microns, the average diameter is 20 microns, the average diameter is controlled within 100 microns), 2.0 parts of zinc nitride powder, 0.5 part of oleamide and UV-3280.5 parts of light stabilizer.
The preparation method of the chitosan coated boron nitride comprises the following steps:
(1) dissolving chitosan with 2% glacial acetic acid, adding boron nitride, and stirring;
(2) adding Span-80 into liquid paraffin serving as an oil phase, uniformly stirring, slowly adding the standby mixed solution in the step (1) in a constant-temperature water bath at 40 ℃ under the stirring condition of 2000r/min, and continuously stirring for 1 h;
(3) adding a certain amount of glutaraldehyde, and continuing stirring and reacting for 3 hours at the speed of 2000 r/min;
(4) and standing and layering, respectively washing the lower layer mixture with petroleum ether, isopropanol and distilled water for three times, and drying to obtain the chitosan coated boron nitride.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, chitosan coated boron nitride, zinc nitride powder, oleamide and a light stabilizer UV-328 according to the weight ratio, and putting the mixture into a high-speed stirrer for mixing at the stirring speed of 1500r/min for 240 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be between 125 and 145 ℃, and the rotating speed of the screw is adjusted to control the feeding speed, so that the fertilizer type biodegradable mulching film with the thickness of 12 mu m is obtained.
The performance of the biodegradable mulch film of this example was as follows:
(1) the longitudinal tensile load is 2.78N, and the elongation at break is 266 percent; right angle tear load 1.74N;
(2) under the field covering condition, the covering period can reach more than 50 days (no obvious degradation occurs within 50 days), and the degradation rate of the field covering for six months can reach more than 90 percent;
(3) calculated according to the dosage of 10 kilograms of fertilizer per mu of land, 0.4 kilogram of boron nitride and 0.2 kilogram of zinc nitride fertilizer can be supplemented in the middle growth period of crops;
(4) the biodegradable mulching film can be used for supplementing nitrogen, boron and zinc fertilizers for various crops.
Example 9
A silicon-magnesium fertilizer type biodegradable mulching film comprises the following raw materials: 89.0 parts of PBAT, 10.0 parts of surface modified talcum powder (the content of talcum powder is 95 percent, the talcum powder is purchased from Beijing Dougeny Co., Ltd, Haicheng, the average thickness is 0.5 micron, the average diameter is controlled within 2 microns, the average diameter is 20 microns, and the average diameter is controlled within 100 microns) of silane coupling agent KH560 and 7831.0 parts of light stabilizer.
The preparation method of the silane coupling agent KH560 surface modified talcum powder comprises the following steps:
(1) dispersing talcum powder with ethanol, and grinding for 0.5h at the rotation speed of 300r/min by using a ball mill;
(2) and (3) fully dissolving the silane coupling agent by using isopropanol, adding the dissolved silane coupling agent into the mixture obtained in the step (1), continuously grinding for 2 hours in the closed ball mill at the rotating speed of 300r/min, and removing the solvent to obtain the talcum powder coated by the silane coupling agent.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, a silane coupling agent KH560 surface modified talcum powder and a light stabilizer 783 according to the weight ratio, and putting into a high-speed stirrer for mixing, wherein the stirring speed is 1500r/min, and the stirring time is 240 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be between 125 and 145 ℃, and the rotating speed of the screw is adjusted to control the feeding speed, so that the fertilizer type biodegradable mulching film with the thickness of 10 mu m is obtained.
The performance of the biodegradable mulch film of this example was as follows:
(1) the longitudinal tensile load is 3.94N, and the elongation at break is 297%; right angle tear load 2.32N;
(2) under the field covering condition, the covering period can reach more than 50 days (no obvious degradation occurs within 50 days), and the degradation rate of the field covering for six months can reach more than 90 percent;
(3) calculated according to the dosage of 10 kilograms per mu of land, about 0.95 kilogram of silicon magnesium salt fertilizer can be supplemented in the middle growth period of crops;
(4) the biodegradable mulching film can be used for supplementing nitrogen, boron and zinc fertilizers for various crops.
Comparative example 1
A biodegradable mulching film comprises the following raw materials: 73.0 parts of PBAT, 20.0 parts of sodium alginate coated urea (500 meshes, the content of the urea is 50%), 5.0 parts of talcum powder, 38531.0 parts of ultraviolet stabilizer UV, and 9001.0 parts of antioxidant B.
The preparation method of the sodium alginate coated urea comprises the following steps:
(1) taking a 2% sodium alginate solution as a water phase, adding urea, and uniformly stirring;
(2) adding Span-80 into isooctane solution as oil phase, stirring, and preheating in 40 deg.C water bath for 10 min;
(3) dropwise adding sodium alginate solution containing urea into oil phase while stirring, continuously stirring at high speed for 60min, and dropwise adding 8% CaCl2Stirring the solution and emulsifying for 30min, washing with anhydrous ethanol and distilled water, drying at room temperature, and filtering to obtain sodium alginate coated urea;
(4) crushing the sodium alginate coated urea by an air separation crusher, air separating to obtain particles and powder with different meshes, and taking the 500-mesh sodium alginate coated urea for later use.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, sodium alginate coated urea, talcum powder, ultraviolet stabilizer UV3853 and antioxidant B900 according to the weight ratio, and putting the mixture into a high-speed stirrer to be mixed, wherein the stirring speed is 1500r/min, and the stirring time is 120 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) adopts a single screw rod to form a film by single-layer extrusion blowing. And blowing the obtained degradation master batches into the full-biodegradable mulching film, wherein the processing temperature of a screw is controlled to be between 125 and 145 ℃, and the rotating speed of the screw is adjusted to control the feeding speed, so that the fertilizer type biodegradable mulching film with the thickness of 18 mu m is obtained.
The performance of the fertilizer-type biodegradable mulch film of this comparative example was as follows:
(1) the appearance of the mulching film has more and large particles, the mechanical property of the mulching film is seriously reduced, the mulching film is easy to break in the mechanical mulching process, and the efficiency is reduced and more waste materials are generated due to the fact that film bubbles are easy to break in the production and processing process.
(2) Under the field covering condition, obvious cracks or holes appear after covering for about 15 to 25 days, and the growth requirements of any crops can hardly be met.
Comparative example 2
A biodegradable mulching film comprises the following raw materials: 83.0 parts of PBAT, 10.0 parts of urea (2000 meshes), 5.0 parts of talcum powder, 38531.0 parts of ultraviolet stabilizer UV, and 9001.0 parts of antioxidant B.
The preparation method of the 2000-mesh urea comprises the following steps:
the urea is crushed by an air separation crusher, particles and powder with different meshes are obtained by air separation, and the 2000-mesh urea is taken for standby.
The preparation method of the biodegradable mulching film comprises the following steps:
(1) mixing the ingredients: weighing PBAT, urea, talcum powder, ultraviolet stabilizer UV3853 and antioxidant B900 according to the weight ratio, and putting into a high-speed stirrer for mixing, wherein the stirring speed is 1500r/min, and the stirring time is 120 s;
(2) melt blending modification extrusion granulation: putting the mixed materials into a double-screw extruder, setting the temperature of the double-screw extruder at 190 ℃, the rotating speed of screws at 120r/min, melting and blending the uniformly mixed materials by the double-screw extruder uniformly, then cooling the materials to 25 ℃ by air cooling or water cooling, and sealing and storing the materials in a dark place after the water content is less than or equal to 0.5%;
(3) the film is formed by single-layer extrusion blowing by using a single screw, wherein the processing temperature of the screw is controlled between 125 ℃ and 145 ℃, but the film cannot be formed by blowing.
Compared with the example 1, the comparative example has the same mesh number and weight part of urea, except that the coating treatment is not carried out, so that the urea and the PBAT undergo chemical reaction in the film blowing process, the performance of the comparative example is seriously reduced, and the film blowing and forming cannot be carried out.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The fertilizer type biodegradable mulching film is characterized by being prepared from the following raw materials: 70.0-95.0 parts of biodegradable plastic, 0.5-30.0 parts of fertilizer, 0-15 parts of lubricant, 0-2.0 parts of light stabilizer, 0-1.5 parts of antioxidant, 0-2.0 parts of chain extender and 0-6.0 parts of color master batch;
the fertilizer is a solid fertilizer, and the solid fertilizer is a flaky fertilizer with the thickness of less than or equal to 10 micrometers;
the preparation method of the fertilizer type biodegradable mulching film comprises the following steps: weighing 70.0-95.0 parts by weight of biodegradable plastic, 0.5-30.0 parts by weight of fertilizer, 0-15 parts by weight of lubricant, 0-2.0 parts by weight of chain extender, 0-2.0 parts by weight of light stabilizer, 0-1.5 parts by weight of antioxidant and 0-6.0 parts by weight of color master batch according to the weight ratio, mixing, transferring the obtained mixture into an extrusion molding machine for extrusion molding, and carrying out granulation and single-layer extrusion blow molding to form the fertilizer type biodegradable mulching film.
2. The fertilizer type biodegradable mulch film according to claim 1, wherein the biodegradable plastic is selected from any one or more of polybutylene adipate/terephthalate, polybutylene succinate/adipate, polylactic acid, polypropylene carbonate, polyhydroxyalkanoate and polybutylene succinate.
3. The fertilizer-type biodegradable mulch film according to claim 1, wherein the sheet fertilizer is a coated sheet fertilizer or a silane coupling agent-modified sheet fertilizer.
4. The biodegradable plastic film of fertilizer type as claimed in any one of claims 1-3, wherein the lubricant is selected from any one or more of talc, oleic acid, oleamide, diatomaceous earth, silica, zinc stearate, calcium stearate, vinyl bis stearamide, soybean oil, rapeseed oil and peanut oil.
5. The fertilizer-type biodegradable mulch film according to any one of claims 1-3, wherein said light stabilizer is selected from any one or more of salicylic acid esters, benzophenones, benzotriazoles, substituted acrylonitriles, triazines, carbon black, iron oxide red and zinc oxide.
6. The fertilizer-type biodegradable mulch film according to any one of claims 1-3, wherein said antioxidant is selected from any one or more of monophenols, bisphenols, triphenols, polyphenols, hydroquinones, thiobisphenols, naphthylamines, diphenylamines, p-phenylenediamines, quinoline derivatives, phosphites and thioesters.
7. The fertilizer type biodegradable mulch film according to any one of claims 1-3, wherein the color master is selected from any one or more of M900, 330BK and KO 3300.
8. The method for preparing the fertilizer-type biodegradable mulch film according to any one of claims 1-7, comprising the steps of: weighing 70.0-95.0 parts by weight of biodegradable plastic, 0.5-30.0 parts by weight of fertilizer, 0-15 parts by weight of lubricant, 0-2.0 parts by weight of chain extender, 0-2.0 parts by weight of light stabilizer, 0-1.5 parts by weight of antioxidant and 0-6.0 parts by weight of color master batch according to the weight ratio, mixing, transferring the obtained mixture into an extrusion molding machine for extrusion molding, and performing granulation and blow molding to form a film to obtain the fertilizer type biodegradable mulching film.
9. The method of claim 8, wherein the method comprises the steps of:
(1) mixing the ingredients: weighing 70.0-95.0 parts by weight of biodegradable plastic, 0.5-30.0 parts by weight of fertilizer, 0-15 parts by weight of lubricant, 0-2.0 parts by weight of chain extender, 0-2.0 parts by weight of light stabilizer, 0-1.5 parts by weight of antioxidant and 0-6.0 parts by weight of color master batch according to the weight ratio, putting into a stirrer for mixing, wherein the stirring speed is 1000-3500r/min, and the stirring time is 50-300 s;
(2) and (3) extruding and granulating: transferring the mixed material obtained in the step (1) into a double-screw extruder to carry out extrusion molding, wherein the extrusion temperature is 140-;
(3) and (3) blow molding to form a film: and (3) blowing the master batch obtained in the step (2) into a film to obtain the fertilizer type biodegradable mulching film with the width of 0.5-4.5 m.
10. The preparation method of claim 9, wherein the master batch is subjected to hot melt extrusion blow molding at a processing temperature of 120-170 ℃ by a single-screw extrusion film blowing machine to form the plastic film.
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| CN112920563B (en) * | 2021-01-28 | 2023-03-17 | 佛山(华南)新材料研究院 | Degradable plastic material, plastic product and preparation method thereof |
| CN112898744A (en) * | 2021-03-16 | 2021-06-04 | 福建星光粒子科技有限公司 | Biodegradable material containing nutrient elements, particles and mulching film |
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| CN114685955B (en) * | 2022-04-29 | 2023-03-24 | 贵州省材料产业技术研究院 | Biodegradable water seepage mulching film capable of slowly releasing fertilizer and preparation method thereof |
| CN114747347B (en) * | 2022-06-16 | 2022-09-27 | 王志红 | Front fork type sunshade covering type soil fertilizer is with machine of scattering |
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