CN113754995A - High-barrier full-biodegradable mulching film and preparation method thereof - Google Patents
High-barrier full-biodegradable mulching film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a double-layer high-barrier full-biodegradable mulching film which is of a double-layer film structure. The raw materials of polydioxanone, polylactic acid, furandicarboxylic acid-succinic acid-propylene glycol copolymer, polypropylene carbonate and the like are all biodegradable materials, and white pollution to the environment can not be brought. The first layer of film enhances and modifies the poly (p-dioxanone) with better flexibility through polylactic acid, and improves the barrier property of the poly (p-dioxanone) through the furandicarboxylic acid-succinic acid-propylene glycol copolymer. The second layer film also uses poly (p-dioxanone) as a main raw material, adopts polypropylene carbonate to improve the barrier property of the poly (propylene carbonate), simultaneously uses a water-retaining agent to improve the soil moisture preservation property, and has good associativity as the main materials of the two layers of films are the same. The mechanical properties are again improved by the combination of the two films. The first layer of film and the second layer of film both combine the use of heat stabilizers and light stabilizers to prolong the degradation time.
Description
Technical Field
The invention belongs to the technical field of agricultural mulching films, and particularly relates to a high-barrier full-biodegradable mulching film and a preparation method thereof.
Background
The agricultural mulching film has the functions of improving the ground temperature, preserving water and soil, preventing insects and inhibiting the growth of weeds, thereby increasing the yield and income of crops. However, since the mulching film is introduced in China, a large amount of Polyethylene (PE) mulching film is used in crop production, the PE mulching film brings great benefits to agriculture and serious 'white pollution' to the ecological environment, the PE mulching film is difficult to degrade because the degradation time is long, the PE mulching film still remains in the soil and the surface after the crops are harvested, pollution and damage which are difficult to estimate are caused to the soil, and the crop production is greatly reduced.
The full-biodegradable mulching film can be completely biodegraded into water, carbon dioxide, harmless substances to the environment and the like in a certain period of time under natural conditions after being paved, cannot cause pollution to soil, and belongs to a low-carbon environment-friendly material. Currently, there are dozens of biodegradable mulch film materials worldwide, such as hydroxy fatty acid ester (PHAs) polymers, polylactic acid (PLA), Polycaprolactone (PCL), polybutylene succinate (PBS), polybutylene adipate/terephthalate (PBAT), polypropylene carbonate (PPC), and the like.
The barrier property of the mulching film is an important influence factor of the soil moisture preservation property. CN106221165B discloses a high-barrier full-biodegradable mulching film, which is characterized in that PPC with excellent barrier property is added into PBAT and PHBH to improve the barrier property of the mulching film. CN110452507A discloses a high-barrier-property all-grown degradable mulching film, which adopts a mode of adding a barrier property reinforcing agent into PBAT to improve the barrier property of the PBAT. The barrier property reinforcing agent mainly comprises one or more of oxidized polyethylene wax, low molecular weight polyethylene wax, nano attapulgite, nano talcum powder, micron talcum powder, modified nano cellulose, mica sheet, vaseline and 1, 4-butanediol. CN105838048B discloses a fully biodegradable mulch film beneficial for preserving soil moisture, which is prepared by adding ethylene-vinyl alcohol copolymer to PBAT and PLA to improve the barrier property.
Aiming at the defects of the barrier property, especially the soil moisture preservation property, of the fully biodegradable mulching film, a new fully biodegradable mulching film and a corresponding preparation method thereof need to be provided.
Disclosure of Invention
The invention aims to provide a high-barrier full-biodegradable mulching film and a preparation method thereof.
The high-barrier full-biodegradable mulching film disclosed by the invention is of a double-layer structure; wherein the first layer of film comprises the following raw materials in parts by weight: 70-110 parts of poly (p-dioxanone), 1-30 parts of polylactic acid, 1-5 parts of furandicarboxylic acid-succinic acid-propylene glycol copolymer, 1-5 parts of compatilizer, 1-15 parts of inorganic filler, 0.1-2 parts of water-retaining agent, 0.1-1 part of heat stabilizer, 0.1-1 part of light stabilizer and 0.1-1 part of antioxidant; the second film comprises the following raw materials in parts by weight: 70 to 110 portions of polydioxanone, 1 to 10 portions of polypropylene carbonate, 0.1 to 1 portion of water-retaining agent, 0.1 to 1 portion of heat stabilizer, 0.1 to 1 portion of light stabilizer and 0.1 to 1 portion of antioxidant.
The number average molecular weight of the poly (p-dioxanone) is 4-10 ten thousand; the number average molecular weight of the polylactic acid is 2-10 ten thousand; the number average molecular weight of the furandicarboxylic acid-succinic acid-propylene glycol copolymer is 4-8 ten thousand; the number average molecular weight of the polypropylene carbonate is 8-15 ten thousand.
The compatilizer is ethylene-acrylate-maleic anhydride copolymer.
The inorganic filler is at least one of calcium carbonate, talcum powder, silicon dioxide and hydrotalcite;
the water-retaining agent is polyacrylamide;
the heat stabilizer is at least one of barium stearate, calcium stearate, zinc stearate, copper stearate, cobalt stearate, magnesium stearate and praseodymium stearate;
the light stabilizer is at least one of 2-hydroxy-4-octoxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2, 4-dihydroxybenzophenone, methyl p-aminobenzoate, ethyl p-aminobenzoate, butyl p-aminobenzoate and glycerol p-aminobenzoate.
The antioxidant is a mixture formed by mixing a hindered phenol antioxidant and a phosphite antioxidant according to a weight ratio of 1:1, wherein the hindered phenol antioxidant is 1010, 1076, 1024 or 1520, and the phosphite antioxidant is trimethyl phosphate, triethyl phosphate, tributyl phosphate, triphenyl phosphate, triethyl phosphite, triphenyl phosphite or 168.
The preparation method of the high-barrier full-biodegradable mulching film comprises the following steps:
(1) drying the polydioxanone, polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw materials of the first membrane for 1 to 8 hours at the temperature of between 30 and 80 ℃;
(2) mixing the raw materials of poly (p-dioxanone), polylactic acid and furandicarboxylic acid-succinic acid-propylene glycol copolymer treated in the step (1) with the rest raw material compatilizer, inorganic filler, water retention agent, heat stabilizer, light stabilizer and antioxidant of the first layer of film at the rotating speed of 300 r/min-1500 r/min for 6 min-20 min, then putting into a screw extruder, and extruding and granulating at the melt temperature of 160-200 ℃ to obtain particles for the first layer of film;
(3) drying the polydioxanone and the polypropylene carbonate in the raw material of the second membrane for 1 to 8 hours at the temperature of between 30 and 80 ℃;
(4) mixing the raw materials of polydioxanone and polypropylene carbonate treated in the step (3) with the residual raw materials of the water-retaining agent, the heat stabilizer, the light stabilizer and the antioxidant of the second layer film at the rotating speed of 500 r/min-1500 r/min for 6 min-20 min, then putting into a screw extruder, and extruding and granulating at the melt temperature of 160-200 ℃ to obtain granules for the second layer film;
(5) carrying out co-extrusion blow molding on the particles for the first layer of film obtained in the step (2) and the particles for the second layer of film obtained in the step (4) in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film; the temperature of the co-extrusion blow molding is 155-200 ℃, and the screw rotating speed is 20-200 r/min.
In conclusion, the high-barrier full-biodegradable mulching film disclosed by the invention adopts the biodegradable materials such as polydioxanone, polylactic acid, furandicarboxylic acid-succinic acid-propylene glycol copolymer, polypropylene carbonate and the like, so that white pollution to the environment is avoided. The first layer of film enhances and modifies the poly (p-dioxanone) with better flexibility through polylactic acid, and improves the barrier property of the poly (p-dioxanone) through the furandicarboxylic acid-succinic acid-propylene glycol copolymer. The second layer film also uses poly (p-dioxanone) as a main raw material, adopts polypropylene carbonate to improve the barrier property of the poly (propylene carbonate), simultaneously uses a water-retaining agent to improve the soil moisture preservation property, and has good associativity as the main materials of the two layers of films are the same. The mechanical properties are again improved by the combination of the two films. The first layer of film and the second layer of film both combine the use of heat stabilizers and light stabilizers to prolong the degradation time.
Detailed Description
The high-barrier full-biodegradable mulching film and the preparation method thereof are further clearly and completely described in the following with reference to the examples.
The test mode is as follows:
the mechanical properties were measured according to GB/T35795 for the test methods in the following examples. The water vapor transmission was carried out in accordance with GB/T1037.
Example 1
A high-barrier full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 8 ten thousand, and 100 parts. Furan dicarboxylic acid-succinic acid-propylene glycol copolymerization with a molecular weight of 4 ten thousand, 2 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. The molecular weight of the polypropylene carbonate is 8 ten thousand, 2 parts. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) drying polydioxanone, polylactic acid and furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw materials of the first membrane at the temperature of 60 ℃ for 3 h;
(2) weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone and the polypropylene carbonate in the starting material of the second membrane were dried at a temperature of 60 ℃ for 3 h.
(4) And (4) adding the residual raw material components of the second layer of film and the raw materials treated in the step (3) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Example 2
A high-barrier full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 8 ten thousand, and 100 parts. Furan dicarboxylic acid-succinic acid-propylene glycol copolymerization with a molecular weight of 8 ten thousand, 2 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. The molecular weight of the polypropylene carbonate is 8 ten thousand, 2 parts. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) and drying the polydioxanone, the polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw material of the first membrane at 60 ℃ for 3 h.
(2) Weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone and polypropylene carbonate in the starting material of the second film were dried at 60 ℃ for 3 h.
(4) And (4) adding the residual raw material components of the second layer of film and the raw materials treated in the step (3) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Example 3
A high-barrier full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 10 ten thousand, and 100 parts. Furan dicarboxylic acid-succinic acid-propylene glycol copolymerization with a molecular weight of 4 ten thousand, 2 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. The molecular weight of the polypropylene carbonate is 8 ten thousand, 2 parts. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) and drying the polydioxanone, the polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw material of the first membrane at 60 ℃ for 3 h.
(2) Weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone and polypropylene carbonate in the starting material of the second film were dried at 60 ℃ for 3 h.
(4) And (4) adding the residual raw material components of the second layer of film and the raw materials treated in the step (3) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Example 4
A high-barrier full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 10 ten thousand, and 100 parts. Furan dicarboxylic acid-succinic acid-propylene glycol copolymerization with a molecular weight of 8 ten thousand, 2 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. The molecular weight of the polypropylene carbonate is 8 ten thousand, 2 parts. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) and drying the polydioxanone, the polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw material of the first membrane at 60 ℃ for 3 h.
(2) Weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone and the polypropylene carbonate in the starting material of the second membrane were dried at a temperature of 60 ℃ for 3 h.
(4) And (4) adding the residual raw material components of the second layer of film and the raw materials treated in the step (3) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Example 5
A high-barrier full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 8 ten thousand, and 100 parts. Furan dicarboxylic acid-succinic acid-propylene glycol copolymerization with a molecular weight of 4 ten thousand, 2 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. The molecular weight of the polypropylene carbonate is 12 ten thousand, 2 parts. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) and drying the polydioxanone, the polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw material of the first membrane at 60 ℃ for 3 h.
(2) Weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone and polypropylene carbonate in the starting material of the second film were dried at 60 ℃ for 3 h.
(4) And (4) adding the residual raw material components of the second layer of film and the raw materials treated in the step (3) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Example 6
A high-barrier full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 8 ten thousand, and 100 parts. Furan dicarboxylic acid-succinic acid-propylene glycol copolymerization with a molecular weight of 8 ten thousand, 2 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. The molecular weight of the polypropylene carbonate is 12 ten thousand, 2 parts. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) and drying the polydioxanone, the polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw material of the first membrane at 60 ℃ for 3 h.
(2) Weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone and polypropylene carbonate in the starting material of the second film were dried at 60 ℃ for 3 h.
(4) And (4) adding the residual raw material components of the second layer of film and the raw materials treated in the step (3) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Example 7
A high-barrier full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: poly-p-dioxanone with molecular weight of 10 ten thousand and 70 portions. Furan dicarboxylic acid-succinic acid-propylene glycol copolymerization with a molecular weight of 4 ten thousand, 2 parts. Polylactic acid with molecular weight of 5 ten thousand and 15 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. The molecular weight of the polypropylene carbonate is 12 ten thousand, 2 parts. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) and drying the polydioxanone, the polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw material of the first membrane at 60 ℃ for 3 h.
(2) Weighing the residual raw material components in the first layer of film material according to the equal amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone and polypropylene carbonate in the starting material of the second film were dried at 60 ℃ for 3 h.
(4) And (3) mixing the residual raw material components of the second film with the raw materials treated in the step (3) in a high-speed mixer for 5 minutes at the rotating speed of 800 rpm. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Example 8
A high-barrier full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 10 ten thousand, and 100 parts. Furan dicarboxylic acid-succinic acid-propylene glycol copolymerization with a molecular weight of 4 ten thousand, 2 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises poly (p-dioxanone) with a molecular weight of 8 ten thousand and 70 parts by weight. The molecular weight of the polypropylene carbonate is 12 ten thousand, 2 parts. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) and drying the polydioxanone, the polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw material of the first membrane at 60 ℃ for 3 h.
(2) Weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone and polypropylene carbonate in the starting material of the second film were dried at 60 ℃ for 3 h.
(4) And (4) adding the residual raw material components of the second layer of film and the raw materials treated in the step (3) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Comparative example 1
A full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 8 ten thousand, and 100 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. The molecular weight of the polypropylene carbonate is 8 ten thousand, 2 parts. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) the polydioxanone and polylactic acid in the raw material of the first film were dried at 60 ℃ for 3 hours.
(2) Weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone and polypropylene carbonate in the starting material of the second film were dried at 60 ℃ for 3 h.
(4) And (3) mixing the residual raw material components of the second film with the raw materials treated in the step (3) in a high-speed mixer for 5 minutes at the rotating speed of 800 rpm. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Comparative example 2
A full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 8 ten thousand, and 100 parts. Furan dicarboxylic acid-succinic acid-propylene glycol copolymerization with a molecular weight of 4 ten thousand, 2 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) and drying the polydioxanone, the polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw material of the first membrane at 60 ℃ for 3 h.
(2) Weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) The polydioxanone in the second film of material was dried at 60 ℃ for 3 h.
(4) And (3) mixing the residual raw material components of the second film with the raw materials treated in the step (3) in a high-speed mixer for 5 minutes at the rotating speed of 800 rpm. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
Comparative example 3
A full-biodegradable mulching film comprises a double-layer structure and comprises a first layer of film and a second layer of film. Wherein the raw material components of the first layer of film comprise, by weight: the molecular weight of the poly-p-dioxanone is 8 ten thousand, and 100 parts. Polylactic acid with molecular weight of 5 ten thousand, 25 portions. 0.5 part of compatilizer ethylene-acrylate-maleic anhydride copolymer. 8 parts of calcium carbonate. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion. The raw material of the second film comprises polydioxanone, 8 ten thousand of molecular weight and 100 parts by weight. 0.3 part of polyacrylamide. 0.1 part of zinc stearate. 0.2 part of 2, 4-dihydroxy benzophenone. Antioxidant 168, 0.2 portion and antioxidant 1010, 0.2 portion.
According to the raw material components, the preparation method provided by the invention is adopted to prepare the full-biodegradable mulching film:
(1) the polydioxanone and polylactic acid in the raw material of the first film were dried at 60 ℃ for 3 hours.
(2) Weighing the residual raw material components in the first layer of film material according to the amount, and adding the weighed residual raw material components and the dried material in the step (1) into a high-speed mixer to mix for 5 minutes at the rotating speed of 800 revolutions per minute. And (3) putting the mixed materials into a screw extruder for extrusion granulation, setting the melt temperature to be 170 ℃, and obtaining the granules for the first layer of film after extrusion granulation.
(3) Drying the polydioxanone in the raw material of the second membrane at a temperature of 60 ℃ for 3 h. (4) And (3) mixing the residual raw material components of the second layer of film and the raw materials treated in the step (3) in a high-speed mixer for 5 minutes at the rotating speed of 800 rpm. And then put into a screw extruder, and extruded and granulated at a melt temperature of 160 ℃ to obtain granules for a second layer film.
(5) And carrying out co-extrusion blow molding on the particles for the first layer of film and the particles for the second layer of film in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film, wherein the co-extrusion blow molding temperature is 165 ℃, and the screw rotation speed is 75 revolutions per minute. The film was blown into a film article having a thickness of 20 microns and tested for properties, the results of which are shown in table 1.
As can be seen from table 1: examples 1-8 all meet the requirements of national standard GB/T35795, and compared with comparative examples 1-3 without adding furandicarboxylic acid-succinic acid-propylene glycol copolymer and/or polypropylene carbonate, the composite material has better barrier property against water vapor. The method has important significance for the soil moisture conservation performance of the mulching film.
Claims (9)
1. The high-barrier full-biodegradable mulching film is characterized by being of a double-layer film structure; wherein the first layer of film comprises the following raw materials in parts by weight: 70-110 parts of poly (p-dioxanone), 1-30 parts of polylactic acid, 1-5 parts of furandicarboxylic acid-succinic acid-propylene glycol copolymer, 1-5 parts of compatilizer, 1-15 parts of inorganic filler, 0.1-2 parts of water-retaining agent, 0.1-1 part of heat stabilizer, 0.1-1 part of light stabilizer and 0.1-1 part of antioxidant; the second film comprises the following raw materials in parts by weight: 70-110 parts of poly (p-dioxanone), 1-10 parts of polypropylene carbonate, 0.1-1 part of water-retaining agent, 0.1-1 part of heat stabilizer, 0.1-1 part of light stabilizer and 0.1-1 part of antioxidant.
2. The high-barrier full-biodegradable mulch film according to claim 1, wherein the number average molecular weight of the polydioxanone is 4-10 ten thousand; the number average molecular weight of the polylactic acid is 2-10 ten thousand; the number average molecular weight of the furandicarboxylic acid-succinic acid-propylene glycol copolymer is 4-8 ten thousand; the number average molecular weight of the polypropylene carbonate is 8-15 ten thousand.
3. The high-barrier full-biodegradable mulch film according to claim 1, wherein the compatibilizer is ethylene-acrylate-maleic anhydride copolymer.
4. The high-barrier full-biodegradable mulch film according to claim 1, wherein the inorganic filler is at least one of calcium carbonate, talc, silica and hydrotalcite.
5. The high-barrier full-biodegradable mulch film according to claim 1, wherein the water retention agent is polyacrylamide.
6. The high-barrier full-biodegradable mulch film according to claim 1, wherein the heat stabilizer is at least one of barium stearate, calcium stearate, zinc stearate, copper stearate, cobalt stearate, magnesium stearate, and praseodymium stearate.
7. The high-barrier full-biodegradable mulch film according to claim 1, wherein the light stabilizer is at least one of 2-hydroxy-4-octoxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2, 4-dihydroxybenzophenone, methyl p-aminobenzoate, ethyl p-aminobenzoate, butyl p-aminobenzoate and glycerol p-aminobenzoate.
8. The high-barrier full-biodegradable mulching film according to claim 1, wherein the antioxidant is a mixture formed by mixing a hindered phenol antioxidant and a phosphite antioxidant in a weight ratio of 1:1, wherein the hindered phenol antioxidant is 1010, 1076, 1024 or 1520, and the phosphite antioxidant is trimethyl phosphate, triethyl phosphate, tributyl phosphate, triphenyl phosphate, triethyl phosphite, triphenyl phosphite or 168.
9. The preparation method of the high-barrier full-biodegradable mulch film according to claims 1-8, comprising the steps of:
(1) drying the polydioxanone, polylactic acid and the furandicarboxylic acid-succinic acid-propylene glycol copolymer in the raw materials of the first membrane for 1 to 8 hours at the temperature of between 30 and 80 ℃;
(2) mixing the raw materials of poly (p-dioxanone), polylactic acid and furandicarboxylic acid-succinic acid-propylene glycol copolymer treated in the step (1) with the rest raw material compatilizer, inorganic filler, water retention agent, heat stabilizer, light stabilizer and antioxidant of the first layer of film at the rotating speed of 300 r/min-1500 r/min for 6 min-20 min, then putting into a screw extruder, and extruding and granulating at the melt temperature of 160-200 ℃ to obtain particles for the first layer of film;
(3) drying the polydioxanone and the polypropylene carbonate in the raw material of the second membrane for 1 to 8 hours at the temperature of between 30 and 80 ℃;
(4) mixing the raw materials of polydioxanone and polypropylene carbonate treated in the step (3) with the residual raw materials of the water-retaining agent, the heat stabilizer, the light stabilizer and the antioxidant of the second layer film at the rotating speed of 500 r/min-1500 r/min for 6 min-20 min, then putting into a screw extruder, and extruding and granulating at the melt temperature of 160-200 ℃ to obtain granules for the second layer film;
(5) carrying out co-extrusion blow molding on the particles for the first layer of film obtained in the step (2) and the particles for the second layer of film obtained in the step (4) in a double-layer co-extrusion film blowing machine to obtain the high-barrier full-biodegradable mulching film; the temperature of the co-extrusion blow molding is 155-200 ℃, and the screw rotating speed is 20-200 r/min.
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