CN115302741A - Degradable mulching film capable of improving water blocking, heat preservation, soil moisture preservation and mechanical properties through lamination and compounding and preparation method thereof - Google Patents

Degradable mulching film capable of improving water blocking, heat preservation, soil moisture preservation and mechanical properties through lamination and compounding and preparation method thereof Download PDF

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Publication number
CN115302741A
CN115302741A CN202210865033.7A CN202210865033A CN115302741A CN 115302741 A CN115302741 A CN 115302741A CN 202210865033 A CN202210865033 A CN 202210865033A CN 115302741 A CN115302741 A CN 115302741A
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film
mulching film
micro
layers
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CN115302741B (en
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李春海
郭少云
冉澜彬
洪魏悠然
于贵营
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Sichuan University
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Sichuan University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
    • B29C55/28—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of blown tubular films, e.g. by inflation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/001—Combinations of extrusion moulding with other shaping operations
    • B29C48/0017—Combinations of extrusion moulding with other shaping operations combined with blow-moulding or thermoforming
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/09—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
    • B29C48/10—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels flexible, e.g. blown foils
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
    • B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/695—Flow dividers, e.g. breaker plates
    • B29C48/70—Flow dividers, e.g. breaker plates comprising means for dividing, distributing and recombining melt flows
    • B29C48/71—Flow dividers, e.g. breaker plates comprising means for dividing, distributing and recombining melt flows for layer multiplication
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
    • Y02A40/28—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture specially adapted for farming

Abstract

The invention provides a degradable mulching film capable of improving water blocking, heat preservation and soil moisture preservation and mechanical properties through laminated composite improvement and a preparation method thereof. The special micro-nano layer structure, the layered limited space, the abundant two-dimensional layer interface and the like can enable the micro-nano laminated film to show the advantages which are difficult to compare with the common multilayer film in the aspects of barrier, optical transparency, mechanics and the like.

Description

Degradable mulching film capable of improving water blocking, heat preservation, soil moisture preservation and mechanical properties through lamination and compounding and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of biodegradable mulching films, and relates to a degradable mulching film capable of improving water blocking, heat preservation and soil moisture preservation and mechanical properties through laminating and compounding and a preparation method thereof.
Background
The water-blocking, heat-preserving and soil moisture-preserving performance of the biodegradable mulching film is poor due to the poor water-blocking performance of the base material. The key point for improving the water resistance of the biodegradable mulching film is to reduce the water vapor transmission rate of the biodegradable mulching film, and the method mainly comprises two methods, namely surface modification and matrix modification. The surface modification is to reduce the water vapor permeability by reducing the solubility coefficient of water molecules on the surface of the membrane, and comprises methods such as surface coating, surface layer-by-layer self-assembly, vapor deposition and the like. The surface modification technologies such as vapor deposition and the like have the advantages that the water resistance of the mulching film can be obviously improved, but the lengthy process is not beneficial to controlling the processing cost of the mulching film. The matrix modification is to construct a water vapor molecular diffusion barrier in the film, reduce the water vapor transmittance of the film by reducing the diffusion coefficient, and construct the barrier in a mode of aggregation structure (crystallization) regulation, inorganic nano-filler (such as montmorillonite) filling and polymer blending and the like. However, the matrix modification technology is simple in process and easy to implement, but the improvement range of the water resistance of the degradable mulching film is limited, and the improvement of the mechanical property cannot be considered. Due to the particularity of the agricultural field, higher requirements are put on the use performance and cost control of biodegradation. Therefore, the preparation of the biodegradable mulching film with high water resistance, heat preservation and excellent mechanics is realized, the processing cost is controlled, and the method has important significance.
The existing single-layer mulching film patent, such as domestic patent CN 114106302A, discloses a carbon dioxide-based biodegradable mulching film and a preparation method thereof. The main materials are PPC and PBAT. The black and colorless biodegradable mulching film is prepared. Wherein, black color masterbatch (carbon black and the like) is added in the black film, which can provide mechanical strength for the mulching film; the colorless film can solve the problem that the middle black drip irrigation belt absorbs heat to cause premature rupture of the biodegradable mulching film, and colorless parts on two sides can still transmit a large amount of sunlight, so that the soil temperature is ensured.
The existing multilayer mulching film is basically of a two-layer or three-layer structure. For example, domestic patent CN 107933041A discloses an environment-friendly mulching film capable of sowing seeds. The mulching film structure comprises a photodegradable film layer, a compatible layer and a tackifying biodegradable film layer which are sequentially stacked. The photodegradable film layer mainly comprises a photodegradant and polyethylene resin. The polyethylene film can ensure the moisture-preserving and temperature-increasing effects of the mulching film and has better durability. Meanwhile, the addition of the photodegradable agent can promote the degradation rate of the mulching film, and degradation with controllable degradation period can be simultaneously carried out during the growth of plants. The compatible layer is compatilizer + polyethylene resin. Mainly for connecting the other two layers well and increasing the compatibility between the layer structures. The tackifying biodegradable film layer is prepared from a tackifier and aliphatic polyester resin. The used aliphatic polyester resin is biodegradable materials such as PLA, PBS, PBAT and the like, can ensure the degradation of the mulching film, and can not cause pollution to the environment and soil. The use of tackifier is for, makes this layer can carry out effective adhesion to the seed, paves through the plastic film and realizes the seeding simultaneously, not only can reduce the labour of manual seeding, has improved the regularity that the seed arranged moreover, is favorable to the growth of plant. The invention adopts the performance of the polyethylene layer material to realize the basic moisture-keeping and temperature-increasing effects of the mulching film, and the degradation of the polyethylene layer of the mulching film is promoted by using the photodegradant. However, the photodegradation process of polyolefin plastics is very slow and the decomposition rate and process are difficult to control. In areas with less solar radiation, the degradation rate is also slower, and the decomposition effect is not ideal. Due to the limitation of available environment and expensive use cost, the photodegradable plastic mulching film is not well popularized and applied.
Domestic patent CN 113754995A discloses a double-layer high-barrier full-biodegradable mulching film, which is of a double-layer film structure. Fully biodegradable raw materials are adopted. The first layer is polylactic acid, polydioxanone and high-barrier copolymer, wherein the polylactic acid can enhance and modify the polydioxanone, and the high-barrier copolymer can improve the barrier property of the polydioxanone; the second layer is poly propylene carbonate + polydioxanone + water-retaining agent, wherein, poly propylene carbonate can promote its barrier properties, and the water-retaining agent can promote the moisture conservation ability. The two films have the same main material and good binding property. The mechanical properties are again improved by the combination of the two films. The first layer of film and the second layer of film are combined with the use of a heat stabilizer and a light stabilizer, so that the degradation time is prolonged.
Domestic patent CN 114149667A discloses a special high weather resistant biodegradable mulch film for cotton, the main material adopts biodegradable polyurethane containing carbonate structure, PPC and PBAT. And carrying out three-layer co-extrusion film blowing to prepare the mulching film with the three-layer structure of the outer layer film, the middle layer film and the bottom layer film. Outer layer film: the mulching film contains components of a coloring agent, an antioxidant and a heat preservation agent, and the damage of ultraviolet rays and oxygen to the mulching film is directly prevented on the surface of the mulching film, so that the functions of ultraviolet resistance and the like of the mulching film are effectively improved, and the problem that the components of the components influence the content of other raw materials and cannot effectively generate effects when being added into a bottom layer film and a middle layer film is also avoided; an intermediate layer: a large amount of components for increasing basic performances such as deformation, heat resistance and weather resistance and the control of the content of biodegradable polyurethane occupying most carbonate structures are added, so that the basic service performance of the mulching film as a bearing object is ensured, the control of the barrier rate to control the biodegradation time is achieved, and the problems of tensile failure, tearing, low service life and the like of the mulching film are effectively prevented; bottom layer film: the components of the scratch-resistant auxiliary agent and the antifouling auxiliary agent are utilized to directly defend soil and plant pollution and damage of scratch to the mulching film on the ground of the mulching film, so that the performances of scratch resistance and the like of the mulching film are effectively improved, and the problem that the components of the components influence the content of other raw materials and cannot effectively generate effects when being added into an outer layer film and a middle layer film is also avoided.
Domestic patent CN 113752662A discloses a three-layer co-extrusion biodegradable mulching film with a barrier structure. The first layer of film is made of PCL polycaprolactone, the degradation period of the PCL polycaprolactone is 6-12 months, the first layer of film does not pollute the environment after being decomposed, the service life of the biodegradable mulching film can be prolonged, and the planting cost is reduced; the second film is made of a polyvinyl alcohol film, the degradation period of the polyvinyl alcohol film is 50-100 days, the polyvinyl alcohol film belongs to a biodegradable polymer material, the water content of the polyvinyl alcohol film can reach 30% -50%, the moisture content in the environment of 65% RH and 25 ℃ can also reach 4.5%, and the gas barrier property is strong; the third film is made of polyamide copolymer, and the polyamide copolymer is formed by the amine transesterification of aliphatic polyester and nylon. The transparency of the aliphatic polyester is increased after the aliphatic polyester and the nylon are subjected to amine-ester exchange, the strength of the aliphatic polyester is similar to that of the main polyamide, but the elongation and the flexibility of the aliphatic polyester are increased, so that the aliphatic polyester is convenient to use and is not easy to damage. The layers are bonded by cellulose adhesive.
The biodegradable material with excellent mechanical property and the degradable material with excellent barrier property are simply blended to obtain compromise of the two properties, and the improvement effect on the prepared mulching film is not obvious enough. The barrier property reinforcing agent is added, the barrier property is improved, and the adverse effect on the mechanical property of the mulching film is also caused, the current biodegradable mulching film taking PBAT as a main material is only applied to partial crops with low water-blocking and heat-preserving requirements, and the yield-increasing effect is not as good as that of the traditional PE mulching film.
Compared with a film with a single-layer structure, the layered structure with higher phase continuity can exert the barrier property of the high-barrier polymer to the maximum extent. In addition, compared with a bicontinuous structure and the like, the layer structure is more regular and easy to obtain, and is not easily influenced by factors such as component content, viscosity, interfacial tension and the like. At present, a high-water-resistance degradable material such as PPC and the like is laminated with a degradable material with excellent mechanical property such as PBAT and the like to construct a multilayer degradable film, so that the water resistance and the mechanical property can be improved to a certain extent, but because the preparation of a higher number of layers cannot be realized, the common multilayer structure which can be realized at present and has 2-3 layers is still difficult to meet the actual application requirement.
Disclosure of Invention
In view of the above, the present invention provides a method for improving mechanical properties and water resistance of a biodegradable mulching film while maintaining original degradability of the biodegradable mulching film, and the method comprises preparing a corresponding biodegradable mulching film, preparing a degradable mulching film with improved water resistance, heat preservation, soil moisture preservation and mechanical properties by using a micro-nano lamination co-extrusion film blowing technology using a mechanical support material, a water resistance material and a functional material, and protecting the degradable mulching film by using a protective layer, wherein the preparation method of the degradable mulching film with improved water resistance, heat preservation, soil moisture preservation and mechanical properties comprises the steps of material vacuum drying → material plasticizing extrusion → layer number multiplication → enveloping ring formation → inflation molding → wind ring cooling → traction roller traction → film rolling, and the micro-nano lamination film is a film material obtained by alternately laminating and compounding dozens of or more layers of materials. The characteristics of unique micro-nano layer structure, layered limited space, rich two-dimensional layer interface and the like can enable the micro-nano laminated film to show the advantages which are difficult to compare with the common multilayer film in the aspects of barrier, optical transparency, mechanics and the like.
In order to achieve the purpose, the technical scheme is as follows:
a degradable mulching film capable of improving water blocking, heat preservation and soil moisture preservation and mechanical properties through lamination and compounding comprises the following preparation raw materials:
a mechanical support layer material A, a water-resistant layer material B and a functional layer material C;
the material A of the mechanical support layer is selected from one or more of polyethylene terephthalate-butylene terephthalate (PBAT), polylactic acid (PLA), polycaprolactone (PCL) and polybutylene succinate (PBS);
the water blocking layer material B is selected from one or more of carbon dioxide-propylene oxide copolymer PPC, polyhydroxyalkanoates PHAs and polyglycolic acid PGA;
the functional layer material C is composed of polyethylene terephthalate-butylene terephthalate (PBAT), an aging resistant agent, a hydrolysis resistant agent and an ultraviolet resistant auxiliary agent;
when the mechanical support layer material A and the water blocking layer material B are selected to prepare the degradable mulching film 1:
plasticizing a mechanical support material A and a water blocking layer material B by utilizing a micro-nano laminated co-extrusion film blowing technology to form A/B, repeatedly laminating n times to form multiple A/B layers alternately with the number of 2 x 2 n The micro-nano laminated mulching film 1 is layered, wherein n is an integer greater than or equal to 1;
when the degradable mulching film 2 is prepared by selecting a mechanical support layer material A, a water-resistant layer material B and a functional layer material C:
plasticizing a mechanical support material A, a water-resistant layer material B and a functional layer material C to form A/B/C by a micro-nano laminated co-extrusion film blowing technology, and processing for n timesRepeating the lamination to form a plurality of A/B/C layers with number of layers 3 × 2 n The micro-nano laminated mulching film 2 is layered, wherein n is an integer greater than or equal to 1.
Further, the micro-nano laminated mulching films 1 and 2 further comprise protective layers; the protective layer comprises an inner protective layer and an outer protective layer, wherein the inner protective layer is composed of a protective layer material D or a protective layer material E; the outer protective layer is composed of a protective layer material D or a protective layer material E;
the protective layer material D is composed of polylactic acid PLA, an anti-ultraviolet additive, a heat stabilizer and an antioxidant;
the protective layer material E is composed of polyethylene terephthalate-butylene terephthalate (PBAT), a heat stabilizer and an antioxidant;
and after the protective layer is plasticized, the protective layer is compounded on the inner layer and the outer layer of the micro-nano laminated mulching films 1 and 2 through a co-extrusion film blowing technology, so that the micro-nano laminated mulching film with the protective layer is formed.
Further, the aging-resistant agent is selected from 2, 6-di-tert-butyl-p-cresol.
Further, the anti-hydrolysis agent is selected from bis (2, 6-diisopropylphenyl) carbodiimide, and the anti-ultraviolet auxiliary agent is selected from 4-hydroxybenzophenone.
Further, the heat stabilizer is selected from calcium stearate, and the antioxidant is selected from dilauryl thiodipropionate.
Further, the preparation method of the degradable mulching film comprises the following steps:
s1: assembling equipment: according to the quantity of materials of the degradable mulching film, parallelly assembling a material A extruder and a material B extruder or an A extruder, a material B extruder and a material C extruder, connecting a junction station behind the extruders, connecting n layer multipliers with the junction station, sequentially connecting a film blowing die head, a cooling air ring, a traction device and a winding device behind the layer multipliers, setting the temperature and rotating speed conditions of the devices, and opening the cooling air ring, the traction device and the winding device, wherein n is more than or equal to 1;
s2: preparing layering: respectively carrying out vacuum drying on the corresponding raw material granules, respectively adding the dried raw material granules into an extruder, plasticizing the extruder, then feeding the plasticized raw material granules into a confluence device, forming an A/B or A/B/C laminated material in the confluence device, and forming the A/B laminated material after passing through n layer multipliersAlternating layers and number of layers 2 x 2 n The micro-nano laminated mulching film material of layers is formed by a plurality of A/B/C layers alternately with the number of layers being 3 x 2 n The micro-nano laminated mulching film material of the layer passes through a film blowing die head and a cooling air ring, and finally the corresponding micro-nano laminated mulching film is obtained by a traction device and a winding device.
Further, the preparation method of the degradable mulching film containing the protective layer comprises the following steps:
s1: assembling equipment: according to the quantity of materials of the degradable mulching film, parallelly assembling a material A extruder and a material B extruder or an A extruder, a material B extruder and a material C extruder, connecting a junction station behind the extruders, connecting n layer multipliers with the junction station, connecting 2 protective layer material extruders in parallel at the upper position and the lower position of an outlet of each layer multiplier, sequentially connecting a film blowing die head, a cooling air ring, a traction device and a winding device behind the 2 protective layer material extruders, setting the temperature and rotating speed conditions of each device, and opening the cooling air ring, the traction device and the winding device, wherein n is more than or equal to 1;
s2: preparing layers: respectively carrying out vacuum drying on the corresponding raw material granules, respectively adding the dried raw material granules into an extruder, plasticizing the extruder, then feeding the plasticized raw material granules into a confluence device, forming an A/B or A/B/C laminated material in the confluence device, and forming an A/B-alternated multilayer with 2 x 2 layers after n layer multipliers n The micro-nano laminated mulching film material of the layers or the micro-nano laminated mulching film material formed by a plurality of A/B/C layers in an alternating way and the number of the layers is 3 to 2 n The method comprises the steps of (1) micro-nano laminated mulching film materials on layers, then extruding protective layer materials D and E respectively by 2 protective layer material extruders, forming protective layers on the upper layer and the lower layer of the laminated mulching film materials, passing through a film blowing die head and a cooling air ring, and finally obtaining the corresponding micro-nano laminated mulching film with the protective layers by a traction device and a winding device.
Further, the temperature of the extruder is 90-180 ℃, and the rotating speed is 200-500 r/min; the temperature of the confluence device layer, the layer multiplier and the film blowing die head area is 155-190 ℃.
Further, the working principle of the single-layer multiplier in the micro-nano lamination co-extrusion film blowing technology is as follows:
the single-layer multiplier can vertically cut the laminar polymer melt converged in the junction station into two parts, wherein one part flows into an upward fishtail-shaped runner to realize transverse widening and longitudinal thinning, the other part flows into a downward fishtail-shaped runner to realize transverse widening and longitudinal thinning, the two parts of melt after widening and thinning are overlapped again, flow and spread to a bottom channel, and the number of layers is multiplied by the cutting-widening/thinning-overlapping principle.
Further, the working principle of a film blowing die head in the micro-nano laminated co-extrusion film blowing technology is as follows:
the film blowing die head envelops the multilayer melt flow with the rectangular cross section generated by the layer multiplier into an annular multilayer melt flow, a multilayer annular fused blank with uniform wall thickness is formed at an outlet, and compressed gas can be introduced to blow the multilayer annular fused blank into a multilayer film bubble of the layer.
Has the advantages that:
the invention has the beneficial effects that:
1. the micro-nano laminated film is a film material formed by alternately laminating dozens of layers of materials to thousands of layers. The characteristics of unique micro-nano layer structure, layered limited space, rich two-dimensional layer interface and the like can enable the micro-nano laminated film to show the advantage which is difficult to compare with the common multilayer film (the number of layers is less than or equal to 13) in the aspects of barrier, optical transparency, mechanics and the like;
2. when all the components in the mulching film are arranged in parallel in a layered mode along the stress direction, the contribution of the mechanical property of the mulching film to the whole composite system is maximum. The layered arrangement not only can endow the material with high mechanical strength, but also can greatly improve the mechanical toughness of the material. The parallel arrangement of layer interfaces in an alternating layered structure is also considered to be the key to efficient barrier to small molecules of gas or liquid. The diffusion path of gas micromolecules is increased by the interface with rich high-layer system;
3. the high water-resistant material is distributed in the micro-nano laminated film in a micro-nano layer structure with thousands of layers and tens of nanometers of layer thickness, and the water-resistant performance of the composite film is improved by blocking water vapor molecules for thousands of times. Compared with a common multilayer structure, the micro-nano laminated structure can improve the barrier property through a micro-nano laminated distribution mechanism with higher barrier efficiency, and is an ideal model for constructing a high-barrier film material;
4. polymers with different mechanical properties are compounded into a multilayer film, so that the mechanical properties can be superposed. In the micro-nano laminated film, the layer structure generates a mechanical synergistic enhancement effect, and an effect of '1 +1 > 2' is generated, so that more excellent tearing strength, puncture resistance, fracture toughness and the like are comprehensively shown;
5. the barrier efficiency is improved by utilizing micro-nano laminated distribution, the barrier self-reinforcement of the material is realized by lamellar limited crystallization, and the composite mulching film is endowed with outstanding water resistance; by means of the advantages of the micro-nano laminated structure, the mechanical characteristics of 'weak and tough' of a mechanical support layer material of the material and 'strong and brittle' of a water vapor barrier layer material are fully exerted, and the composite mulching film is endowed with excellent mechanical properties such as tearing strength.
6. The thickness of a single layer in the micro-nano laminated film can be as low as tens of nanometers and is far smaller than the wavelength range (380-780 nm) of visible light, and the layer interfaces are arranged in parallel and allow the visible light to directly pass through, so that the micro-nano laminated film has outstanding optical transparency. Therefore, the micro-nano laminated structure is introduced into the degradable mulching film, the water resistance of the degradable mulching film can be greatly improved, the mechanical property is improved, the prepared mulching film has high transparency, and the advantages are very obvious.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 shows the preparation of alternating A/B multilayers with 2X 2 layers in the examples of the present application n A schematic diagram of a process of laminating the micro-nano mulching films;
FIG. 2 shows the preparation of alternating A/B/C multilayers with a number of layers 3 x 2 according to the examples of the present application n A schematic diagram of a process of laminating the micro-nano mulching films;
FIG. 3 shows the preparation of alternating A/B multilayers and D asOuter protective layer, E inner protective layer, and 2 × 2 layers n +2 layers of micro-nano laminated mulching films;
FIG. 4 shows the preparation of the present application in which A/B/C are alternately layered, D is an outer passivation layer, E is an inner passivation layer, and the number of layers is 3X 2 n +2 layers of micro-nano laminated mulching films;
FIG. 5 is a diagram illustrating a working principle of a micro-nano lamination co-extrusion film blowing technology and a layer multiplier thereof in the embodiment of the present application (taking A/B alternate layer 2 as an example);
FIG. 6 shows the preparation of alternating A/B multilayers with 2X 2 layers in the examples of the present application n A flow chart of a micro-nano laminated mulching film of the layer;
FIG. 7 shows the preparation of alternating A/B/C multilayers with a number of layers 3 x 2 according to the examples of the present application n A flow chart of a micro-nano laminated mulching film of the layer;
FIG. 8 shows the preparation of the present application in which A/B is alternately layered, D is an outer passivation layer, E is an inner passivation layer, and the number of layers is 2X 2 n +2 layers of micro-nano laminated mulching film flow chart;
FIG. 9 shows an example of the present application for preparing a multilayer with A/B/C alternation, D as an outer protective layer, E as an inner protective layer, and 3 × 2 layers n +2 layers of micro-nano laminated mulching film flow chart;
fig. 10 is an electron microscope image of a 32, 128 and 512-layer PBAT/PPC micro-nano laminated mulch film prepared in example 1 of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The material preparation in the examples was completed according to the working principle diagram of the layer multiplier shown in fig. 5.
Example 1
According to the drawings of fig. 1 and fig. 6, the micro-nano multilayer biodegradable mulching film comprises the following raw materials:
mechanical support layer material A: a polybutylene terephthalate (PBAT) material;
water-resistant layer material B: a carbon dioxide-propylene oxide copolymer (PPC) material.
According to the flow chart of fig. 6, the micro-nano multilayer biodegradable mulching film is prepared, which comprises the following steps:
the PPC and PBAT mass were placed in a forced air drying oven for drying.
The preparation is carried out by using a flow chart shown in fig. 6, 2, 4, 6 and 8 layer multipliers are respectively connected in series at confluence devices of two extruders, and then a film blowing die, a cooling air ring and a traction device are sequentially connected behind the layer multipliers. The series connection of 2, 4, 6, 8 layer multipliers can realize that the blown film has a multilayer structure with 8, 32, 128, 512 layers.
Extruding machine # 1 the temperature settings of a first zone, a second zone, a third zone, a fourth zone of the charging barrel and the front end zone of the junction station are respectively as follows: 125 deg.C, 170 deg.C, 180 deg.C, and 300r/min; extruding machine # 2 the temperature settings of the first zone, the second zone, the third zone, the fourth zone of the charging barrel and the front end zone of the junction station are respectively as follows: 90 ℃, 130 ℃, 165 ℃ and 300r/min of rotation speed; the temperature settings of the junction station area, the layer multiplier area, the first die head area and the second die head area are respectively as follows: 180 deg.C, 165 deg.C, 155 deg.C.
To the extruder # 1 and # 2, adding the materials of polyethylene terephthalate-butylene terephthalate (PBAT) and carbon dioxide-propylene oxide copolymer (PPC) which are baked in advance respectively for film blowing. The blown film is a multilayer biodegradable film having a structure of 32, 128 or 512 layers, as shown in fig. 10.
Example 2
According to the drawings of fig. 2 and 7, the micro-nano multilayer biodegradable mulching film comprises the following raw materials:
mechanical support layer material A: 50 parts of polyethylene terephthalate-butylene terephthalate (PBAT) material and 50 parts of polylactic acid (PLA) material;
water-resistant layer material B: a carbon dioxide-propylene oxide copolymer (PPC) material;
functional layer C: 100 parts of polyethylene terephthalate-butylene terephthalate (PBAT) material, 0.2 part of aging resistant agent 2, 6-di-tert-butyl-p-cresol, 0.2 part of hydrolysis resistant agent bis (2, 6-diisopropylphenyl) carbodiimide and 0.4 part of anti-ultraviolet auxiliary agent 4-hydroxybenzophenone.
According to the figure 7, the preparation of the micro-nano multilayer biodegradable mulching film comprises the following steps:
the material was dried in a forced air drying oven.
The preparation was carried out in an extruder using the flow chart shown in FIG. 7 # 1、 # 2 and # the junction station of 3 is connected with 4 layer multipliers in series, and then a film blowing die, a cooling air ring and a traction device are sequentially connected behind the layer multipliers. A blown film having a multilayer structure of 48 layers can be achieved by connecting 4 layer multipliers in series.
Extruding machine # 1 the temperature settings of a first zone, a second zone, a third zone, a fourth zone of the charging barrel and the front end zone of the junction station are respectively as follows: 135 deg.C, 180 deg.C, 190 deg.C, and 200r/min rotation speed; extruding machine # 2 the temperature settings of the first zone, the second zone, the third zone, the fourth zone of the charging barrel and the front end zone of the junction station are respectively as follows: 90 ℃, 130 ℃, 165 ℃ and the rotation speed of 200r/min; extruding machine # 3 the temperature settings of the first zone, the second zone, the third zone, the fourth zone of the charging barrel and the front end zone of the junction station are respectively as follows: 125 ℃, 170 ℃, 180 ℃ and the rotating speed of 200r/min; the temperature settings of the junction station area, the layer multiplier area, the first die head area and the second die head area are respectively as follows: 190 deg.C, 175 deg.C, 165 deg.C.
To the extruder # 1 adding a dried mixture material of polybutylene terephthalate (PBAT) and polylactic acid (PLA); adding the baked carbon dioxide-propylene oxide copolymer (PPC) material to extruder # 2; to the extruder # 3, adding a polybutylene terephthalate-butylene terephthalate (PBAT) material containing an anti-aging agent, a hydrolysis resistant agent and an anti-ultraviolet auxiliary agent to perform film blowing. The blown film is a multilayer biodegradable film with 48 layers of structure.
Example 3
According to the drawings of fig. 3 and fig. 8, the micro-nano multilayer biodegradable mulching film comprises the following raw materials:
mechanical support layer material A: 50 parts of polyethylene terephthalate-butylene terephthalate (PBAT) material and 50 parts of polylactic acid (PLA) material;
water-resistant layer material B: a carbon dioxide-propylene oxide copolymer (PPC) material;
outer protective layer material D: 100 parts of polylactic acid (PLA) material, 0.4 part of anti-ultraviolet auxiliary agent 4-hydroxybenzophenone, 0.2 part of heat stabilizer calcium stearate, and 0.2 part of antioxidant dilauryl thiodipropionate
Inner protective layer material E: 100 parts of polyethylene terephthalate-butylene terephthalate (PBAT) material, 0.2 part of heat stabilizer calcium stearate and 0.2 part of antioxidant dilauryl thiodipropionate
According to fig. 8, the micro-nano multilayer biodegradable mulching film comprises the following steps:
the material was placed in a forced air drying oven for drying.
The preparation was carried out according to the scheme shown in FIG. 8, in an extruder # 1 and # 2, 4 layer multipliers are connected in parallel at the junction station of the flow collectors and then connected with the extruder at the outlets of the layer multipliers # 3 and an extruder # 4, and then sequentially connecting a film blowing port die, a cooling air ring and a traction device. In principle, an interposed 4-layer multiplier makes it possible to realize a multilayer structure of 34 layers of blown film.
Extruding machine # 1 the temperature settings of a first zone, a second zone, a third zone, a fourth zone of the charging barrel and the front end zone of the junction station are respectively as follows: 135 deg.C, 180 deg.C, 190 deg.C, and 300r/min rotation speed; extruding machine # 2 the temperature settings of the first zone, the second zone, the third zone, the fourth zone of the charging barrel and the front end zone of the junction station are respectively as follows: 90 ℃, 130 ℃, 165 ℃ and 300r/min of rotation speed; extruding machine # 3 the temperature of the first zone, the second zone, the third zone and the fourth zone of the charging barrel are set as follows: 145 ℃, 180 ℃, and the rotation speed is 300r/min; extruding machine # 4 the temperature of the first zone, the second zone, the third zone and the fourth zone of the charging barrel are set as follows: 125 ℃, 170 ℃ and the rotating speed of 300r/min; the temperature settings of the junction station area, the layer multiplier area, the first die head area and the second die head area are respectively as follows: 190 deg.C, 175 deg.C, 165 deg.C.
To the extruder # 1 adding baked polybutylene terephthalate (PBAT) anda polylactic acid (PLA) blend material; adding the baked carbon dioxide-propylene oxide copolymer (PPC) material to extruder # 2; to the extruder # 3 adding a polylactic acid (PLA) material containing an anti-ultraviolet auxiliary agent, a heat stabilizer and an antioxidant; to the extruder # 4, adding polybutylene terephthalate (PBAT) material containing a heat stabilizer and an antioxidant, and blowing the film. The blown film is a multilayer biodegradable film with 34-layer structure.
Example 4
According to fig. 4 and fig. 9, the micro-nano multilayer biodegradable mulch film comprises the following raw materials:
mechanical support layer material A: 50 parts of polyethylene terephthalate-butylene terephthalate (PBAT) material and 50 parts of polylactic acid (PLA) material;
water-resistant layer material B: 50 parts of carbon dioxide-propylene oxide copolymer (PPC) material and 50 parts of polyglycolic acid (PGA) material;
functional layer material C: 100 parts of polyethylene terephthalate-butylene terephthalate (PBAT) material, 0.2 part of aging resistant agent 2, 6-di-tert-butyl-p-cresol, 0.2 part of hydrolysis resistant agent bis (2, 6-diisopropylphenyl) carbodiimide, and 0.4 part of anti-ultraviolet auxiliary agent 4-hydroxybenzophenone
Outer protective layer material D: 100 parts of polylactic acid (PLA) material, 0.4 part of anti-ultraviolet additive 4-hydroxybenzophenone, 0.2 part of heat stabilizer calcium stearate, and 0.2 part of antioxidant dilauryl thiodipropionate
Inner protective layer material E: 100 parts of polyethylene terephthalate-butylene terephthalate (PBAT) material, 0.2 part of heat stabilizer calcium stearate and 0.2 part of antioxidant dilauryl thiodipropionate
According to fig. 9, the micro-nano multilayer biodegradable mulch film comprises the following steps:
the material was dried in a forced air drying oven.
The preparation was carried out according to the scheme shown in FIG. 9, in an extruder # 1、 # 2 and # 3, connecting 4 layers of multipliers in parallel at the junction station of the flow combiner, and then connecting the outlet of the layer multipliers with an extruder # 4 and extruder # 5 connecting, and sequentially connecting the film blowingThe mouth mold, the cooling air ring and the traction device. The incorporation of a 4-layer multiplier allows the blown film to have a multilayer structure of 50 layers.
The temperature settings of the first zone, the second zone, the third zone, the fourth zone and the front end zone of the junction station of the extruder #1 charging barrel are respectively as follows: 135 deg.C, 180 deg.C, 190 deg.C, and 200r/min rotation speed; the temperature settings of the first zone, the second zone, the third zone, the fourth zone and the front end zone of the junction station of the extruder #2 charging barrel are respectively as follows: 90 ℃, 130 ℃, 165 ℃ and the rotation speed of 200r/min; the temperature settings of the first zone, the second zone, the third zone, the fourth zone of the extruder #3 charging barrel and the front end zone of the junction station are respectively as follows: 125 deg.C, 170 deg.C, 180 deg.C, and rotation speed of 200r/min; extruding machine # 4 the temperature of the first zone, the second zone, the third zone and the fourth zone of the charging barrel are set as follows: 145 ℃, 180 ℃ and 300r/min of rotation speed; extruding machine # 5 the temperature of the first zone, the second zone, the third zone and the fourth zone of the charging barrel are set as follows: 125 ℃, 170 ℃ and the rotating speed of 300r/min; the temperature settings of the junction station area, the layer multiplier area, the first die head area and the second die head area are respectively as follows: 190 deg.C, 175 deg.C, 165 deg.C.
Adding the baked polybutylene terephthalate (PBAT) and polylactic acid (PLA) blend material into an extruder # 1; to the extruder # 2 adding a blend material of a baked carbon dioxide-propylene oxide copolymer (PPC) material and a polyglycolic acid (PGA) material; to the extruder # 3 adding a polybutylene terephthalate-butylene terephthalate (PBAT) material containing an anti-aging agent, a hydrolysis resistant agent and an anti-ultraviolet auxiliary agent; to the extruder # 4, adding a polylactic acid (PLA) material containing an anti-ultraviolet auxiliary agent, a heat stabilizer and an antioxidant; to the extruder # 5, adding polybutylene terephthalate (PBAT) material containing a heat stabilizer and an antioxidant, and blowing the film. The blown film is a multilayer biodegradable film having a 50-layer structure.
Experimental analysis:
experimental group 1: the micro-nano multilayer biodegradable mulching film prepared in the embodiment 1 forms an experimental group 1, 8, 32, 128 and 512 layers of mulching films with alternately arranged PBAT and PPC are respectively prepared, and the film thickness is 10um;
control group 1: the other steps are the same as those of example 1, except that only the PBAT and PPC blend is used in the extruder (the ratio of PBAT to PPC is the same as that of the composite laminated mulch film prepared in example 1), and a PBAT/PPC blend mulch film control 1 having only a single-layer structure is formed.
Control group 2: the other steps are the same as the step of the embodiment 1, and the difference is that the PBAT mulching film control group 2 with a single-layer structure is prepared by using only one material of PBAT by an extruder.
The results are shown in Table 1
TABLE 1 Properties of laminated mulching film, blended mulching film, single-layered mulching film prepared (layer thickness 10 um)
Figure BDA0003758249560000151
By the above embodiment, it is possible to obtain:
according to the micro-nano multilayer co-extrusion biodegradable mulching film and the preparation method thereof, the micro-nano multilayer biodegradable mulching film prepared by the method has good water vapor barrier property and excellent mechanical property, and has unique advantages and application prospects in the field of biodegradable mulching films.
In addition, brittle fracture is carried out on the selected part of the prepared example 1 and the film, the layer structure of the film is observed through an electron microscope, as shown in fig. 10, the number of layers can reach 512 layers, the thickness of a single layer is as low as 20 nanometers, the layer structure is relatively clear, and the invention is further proved to be capable of successfully preparing the film with the micro-nano multilayer structure.
In conclusion, the invention provides a degradable mulching film for improving water-blocking, heat-preservation and soil moisture preservation and mechanical properties through laminated composite improvement and a preparation method thereof. The special characteristics of a nano-layer structure, a layered limited space, a rich two-dimensional layer interface and the like can enable the micro-nano laminated film to show the advantages which are difficult to compare with the common multilayer film in the aspects of barrier, optical transparency, mechanics and the like.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited to the above embodiments, and those skilled in the art can make various changes and modifications without departing from the scope of the present invention.

Claims (10)

1. The utility model provides a through range upon range of compound degradable plastic film that promotes heat preservation soil moisture conservation and mechanical properties that blocks water which promotes, its characterized in that, the preparation raw materials of degradable plastic film include:
a mechanical support layer material A, a water-resistant layer material B and a functional layer material C;
the material A of the mechanical support layer is selected from one or more of polyethylene terephthalate-butylene terephthalate (PBAT), polylactic acid (PLA), polycaprolactone (PCL) and polybutylene succinate (PBS);
the water blocking layer material B is selected from one or more of carbon dioxide-propylene oxide copolymer PPC, polyhydroxyalkanoates PHAs and polyglycolic acid PGA;
the functional layer material C is composed of polyethylene terephthalate-butylene terephthalate (PBAT), an aging resistant agent, a hydrolysis resistant agent and an ultraviolet resistant auxiliary agent;
when the mechanical support layer material A and the water blocking layer material B are selected to prepare the degradable mulching film 1:
mechanics by micro-nano lamination co-extrusion film blowing technologyPlasticizing the support material A and the water-blocking layer material B to form A/B, repeatedly laminating for n times to form a plurality of A/B layers with the number of layers being 2 x 2 n The micro-nano laminated mulching film 1 is layered, wherein n is an integer greater than or equal to 1;
when the mechanical support layer material A, the water-blocking layer material B and the functional layer material C are selected to prepare the degradable mulching film 2:
plasticizing a mechanical support material A, a water blocking layer material B and a functional layer material C by utilizing a micro-nano laminated co-extrusion film blowing technology to form A/B/C, repeatedly laminating for n times to form a plurality of A/B/C alternate layers with the number of layers being 3 x 2 n The micro-nano laminated mulching film 2 is layered, wherein n is an integer greater than or equal to 1.
2. The degradable mulching film capable of improving water blocking, heat preservation and soil moisture preservation and mechanical property through lamination and compounding as claimed in claim 1, wherein the micro-nano laminated mulching films 1 and 2 further comprise a protective layer; the protective layer comprises an inner protective layer and an outer protective layer, wherein the inner protective layer is composed of a protective layer material D or a protective layer material E; the outer protective layer is composed of a protective layer material D or a protective layer material E;
the protective layer material D is composed of polylactic acid PLA, an anti-ultraviolet auxiliary agent, a heat stabilizer and an antioxidant;
the protective layer material E is composed of polyethylene terephthalate-butylene terephthalate (PBAT), a heat stabilizer and an antioxidant;
and after the protective layer is plasticized, the protective layer is compounded on the inner layer and the outer layer of the micro-nano laminated mulching films 1 and 2 through a co-extrusion film blowing technology, so that the micro-nano laminated mulching film with the protective layer is formed.
3. The degradable mulching film for improving water-blocking, heat preservation and soil moisture preservation and mechanical properties through lamination and compounding as claimed in claim 1, wherein the aging-resistant agent is selected from 2, 6-di-tert-butyl-p-cresol.
4. The degradable mulching film for improving water-blocking, heat preservation and soil moisture preservation and mechanical properties through lamination composite as claimed in claim 1, wherein the hydrolysis-resistant agent is selected from bis (2, 6-diisopropylphenyl) carbodiimide, and the anti-ultraviolet auxiliary agent is selected from 4-hydroxybenzophenone.
5. The degradable mulching film for improving water-blocking, heat preservation and soil moisture preservation and mechanical properties through lamination and compounding as claimed in claim 2, wherein the heat stabilizer is selected from calcium stearate, and the antioxidant is selected from dilauryl thiodipropionate.
6. The degradable mulching film for improving water blocking, heat preservation and soil moisture preservation and mechanical property through lamination and compounding as claimed in claim 1, wherein the preparation method of the degradable mulching film comprises the following steps:
s1: assembling equipment: according to the quantity of materials of the degradable mulching film, parallelly assembling a material A extruder and a material B extruder or an A extruder, a material B extruder and a material C extruder, connecting a junction station behind the extruders, connecting n layer multipliers behind the junction station, sequentially connecting a film blowing die head, a cooling air ring, a traction device and a winding device behind the layer multipliers, setting the temperature and rotating speed conditions of the devices, opening the cooling air ring, the traction device and the winding device, wherein n is more than or equal to 1;
s2: preparing layers: respectively carrying out vacuum drying on the corresponding raw material granules, respectively adding the dried raw material granules into an extruder, plasticizing the extruder, then feeding the plasticized raw material granules into a confluence device, forming an A/B or A/B/C laminated material in the confluence device, and forming an A/B-alternated multilayer with 2 x 2 layers after n layer multipliers n The micro-nano laminated mulching film material of the layers or the micro-nano laminated mulching film material formed by a plurality of A/B/C layers in an alternating way and the number of the layers is 3 to 2 n The micro-nano laminated mulching film material of the layer passes through a film blowing die head and a cooling air ring, and finally the corresponding micro-nano laminated mulching film is obtained by a traction device and a winding device.
7. The degradable mulching film for improving water blocking, heat preservation and soil moisture preservation and mechanical property through lamination and compounding as claimed in claim 2, wherein the preparation method of the degradable mulching film comprises the following steps:
s1: assembling equipment: according to the quantity of materials of the degradable mulching film, parallelly assembling a material A extruder and a material B extruder or an A extruder, a material B extruder and a material C extruder, connecting a junction station behind the extruders, connecting n layer multipliers with the junction station, connecting 2 protective layer material extruders in parallel at the upper position and the lower position of an outlet of each layer multiplier, sequentially connecting a film blowing die head, a cooling air ring, a traction device, a winding device behind the 2 protective layer material extruders, setting the temperature and rotating speed conditions of each device, opening the cooling air ring, the traction device and the winding device, wherein n is more than or equal to 1;
s2: preparing layers: respectively carrying out vacuum drying on the corresponding raw material granules, respectively adding the dried raw material granules into an extruder, plasticizing the extruder, then feeding the plasticized raw material granules into a confluence device, forming an A/B or A/B/C laminated material in the confluence device, and forming an A/B-alternated multilayer with 2 x 2 layers after n layer multipliers n The micro-nano laminated mulching film material of layers is formed by a plurality of A/B/C layers alternately with the number of layers being 3 x 2 n The method comprises the steps of micro-nano laminated mulching film materials on layers, extruding protective layer materials D and E respectively by 2 protective layer material extruders, forming protective layers on the upper layer and the lower layer of the laminated mulching film materials, passing through a film blowing die head and a cooling air ring, and finally obtaining the corresponding micro-nano laminated mulching film with the protective layers by a traction device and a winding device.
8. The degradable mulching film for improving water blocking, heat preservation and soil moisture preservation and mechanical property through lamination and compounding as claimed in claim 7, wherein the temperature of the extruder is 90-180 ℃, and the rotation speed is 200-500 r/min; the temperature of the confluence device layer, the layer multiplier and the film blowing die head area is 155-190 ℃.
9. The degradable mulching film capable of improving water blocking, heat preservation and soil moisture preservation and mechanical property through lamination and composite lifting according to claims 7-8, wherein a single-layer multiplier in the micro-nano lamination co-extrusion film blowing technology has the working principle that:
the single-layer multiplier can vertically cut the laminar polymer melt converged in the junction station into two parts, wherein one part flows into an upward fishtail-shaped runner to realize transverse widening and longitudinal thinning, the other part flows into a downward fishtail-shaped runner to realize transverse widening and longitudinal thinning, the two parts of melt after widening and thinning are overlapped again, flow and spread to a bottom channel, and the number of layers is multiplied by the cutting-widening/thinning-overlapping principle.
10. The degradable mulching film capable of improving water blocking, heat preservation and soil moisture preservation and mechanical property through lamination and composite lifting according to claims 7-8, wherein a film blowing die head in the micro-nano lamination co-extrusion film blowing technology has the working principle that:
the film blowing die head envelops the multilayer melt flow with the rectangular cross section generated by the layer multiplier into an annular multilayer melt flow, a multilayer annular fused blank with uniform wall thickness is formed at an outlet, and compressed gas can be introduced to blow the multilayer annular fused blank into a multilayer film bubble of the layer.
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CN101947841A (en) * 2010-08-06 2011-01-19 北京化工大学 Device and method for preparing micro-nano laminated composite material with high barrier proper
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