CN113337013A - Cellulose nanofibril-PBAT composite film and preparation method and application thereof - Google Patents
Cellulose nanofibril-PBAT composite film and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a cellulose nanofibril-PBAT composite film, a preparation method and application thereof. The cellulose nanofibril-PBAT composite film is prepared from cellulose nanofibril, PBAT and nano soil. The preparation method of the cellulose nanofibril-PBAT composite film comprises the following steps: 1) preparing cellulose nano fibril dispersion liquid; 2) preparing a cellulose nanofibril-nano soil mixed solution; 3) preparing a cellulose nanofibril film; 4) the cellulose nanofibril film is impregnated with the PBAT dispersion. The invention takes the nano cellulose fiber as a substrate, and is compounded with the PBAT through intermolecular acting force, hydrogen bond action and interface fusion action without any chemical modification treatment, so that the obtained composite film has the advantages of good waterproof performance, large elongation at break, safety and environmental protection, and can be widely applied to the fields of agricultural mulching films, product packaging, insulating materials, packaging materials and the like.
Description
Technical Field
The invention relates to the technical field of bio-based degradable films, in particular to a cellulose nanofibril-PBAT composite film and a preparation method and application thereof.
Background
Plastics have become more and more widespread worldwide, with annual global plastic production exceeding 3 billion tons since 2014. However, plastics degrade in the environment for long periods of time, are durable, have potential negative consequences for nature and human health, and there is a need to develop sustainable alternative materials.
PBAT (a copolymer of butylene adipate and butylene terephthalate) is thermoplastic biodegradable plastic, has good ductility, high elongation at break, good heat resistance, good impact resistance and excellent biodegradability, and becomes one of research hotspots in the field of biodegradable plastics. Meanwhile, PBAT belongs to aliphatic aromatic polyester, has good biocompatibility and is one of ideal candidate materials in the fields of agriculture, packaging films, medical devices and the like. The yield of PBAT-based bioplastics was reported to be about 200 million tons in 2018, while the yield increased by two-fold in 2020, indicating a significant increase in market demand. However, PBAT has been greatly limited in its application due to its poor strength, high price, complicated production process, and the like.
Cellulose has the advantages of rich sources, environmental protection, high strength, high modulus, good heat resistance, easy degradation and the like, and is receiving more and more attention in recent years, and the application of nano cellulose as a compatibilization and reinforcement material has become a hotspot of research. The literature reports that: the cellulose micro/nano-fiber is prepared by an acid method, a wet mixed film is rolled up, and internal hydrogen bonds formed between the dried cellulose micro/nano-fibers are utilized for sealing, so that the adhesive-free all-natural degradable cellulose straw can be finally obtained (adv.funct.mater.2020,30,1910417). However, the cellulose straw prepared by the method has too many exposed hydroxyl groups and poor waterproof performance, so that the practical application of the cellulose straw is greatly limited, the cellulose is seriously degraded by an acid method, more nanocrystalline areas of the nano-cellulose cannot be reserved, the yield of the nano-cellulose is reduced, the finally formed nano-cellulose is of a one-dimensional rod-shaped structure, and the cellulose cannot form interlaced network connection.
Disclosure of Invention
The invention aims to provide a cellulose nanofibril-PBAT composite film, and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
a cellulose nanofibril-PBAT composite film is prepared from the following raw materials in percentage by mass:
cellulose nanofibrils: 51 to 99 percent;
PBAT：1％～49％；
nano soil: 0 to 8 percent.
Preferably, the cellulose nanofibril-PBAT composite film is prepared from the following raw materials in percentage by mass:
cellulose nanofibrils: 51 to 98 percent;
PBAT：1.02％～42.11％；
nano soil: 0.98-6.89%.
Preferably, the cellulose nanofibrils have a length of 200nm to 5000nm and a diameter of 1nm to 300 nm.
Preferably, the cellulose nanofibrils are made of at least one of softwood pulp, hardwood pulp, cotton pulp, bacterial cellulose.
Preferably, the PBAT has a number average molecular weight of 40000g/mol to 80000 g/mol.
More preferably, the number average molecular weight of PBAT is 40000g/mol to 60000 g/mol.
Preferably, the particle size of the nano soil is 100nm to 1000 nm.
More preferably, the particle size of the nano-soil is 200nm to 800 nm.
The preparation method of the cellulose nanofibril-PBAT composite film comprises the following steps:
1) adding water into cellulose to prepare a cellulose suspension, and carrying out superfine grinding to obtain a cellulose nano fibril dispersion liquid;
2) dispersing nano soil in the cellulose nano fibril dispersion liquid to obtain a cellulose nano fibril-nano soil mixed liquid;
3) pouring the cellulose nanofibril-nano soil mixed solution into a film casting container for film casting to obtain a cellulose nanofibril film;
4) and (3) immersing the cellulose nanofibril film into the PBAT dispersion liquid for impregnation to obtain the cellulose nanofibril-PBAT composite film.
Preferably, the preparation method of the cellulose nanofibril-PBAT composite film comprises the following steps:
1) soaking cellulose in water to prepare a cellulose suspension, and carrying out superfine grinding to obtain a cellulose nano fibril dispersion liquid;
2) adding nano soil into the cellulose nano fibril dispersion liquid, and stirring to obtain a cellulose nano fibril-nano soil mixed solution;
3) pouring the cellulose nanofibril-nano soil mixed solution into a film casting container for film casting to obtain a cellulose nanofibril film;
4) and (3) immersing the cellulose nanofibril film into the PBAT dispersion liquid, soaking, taking out and drying to obtain the cellulose nanofibril-PBAT composite film.
Preferably, the soaking time in the step 1) is 12-48 h.
Preferably, the gap of the superfine particle crusher adopted in the superfine crushing in the step 1) is 5-60 μm, and the rotating speed is 1500-6000 r/min.
More preferably, the gap of the superfine particle crusher used for the superfine crushing in the step 1) is 5 to 20 μm, and the rotating speed is 1500 to 4500 r/min.
Preferably, the cellulose nanofibril dispersion liquid of step 2) has a mass percentage concentration of 1% to 10%.
Preferably, the stirring time in the step 2) is 0.1-3 h.
Preferably, the film casting in the step 3) is carried out at 30-80 ℃, and the film casting time is 24-240 h.
More preferably, the film casting in the step 3) is carried out at 30-50 ℃, and the film casting time is 24-168 h.
Preferably, the solvent in the PBAT dispersion of step 4) is at least one of tetrahydrofuran, acetonitrile, acetone, methanol, and ethanol.
Preferably, the drying in the step 4) is carried out at 100-300 ℃, and the drying time is 0.1-2 h.
The invention has the beneficial effects that: the invention takes the cellulose nanofibrils as the matrix, and then is compounded with the PBAT through intermolecular acting force, hydrogen bond action and interface fusion action without any chemical modification treatment, so that the obtained composite film has good waterproof performance, large elongation at break, safety and environmental protection, and can be widely applied to the fields of agricultural mulching films, product packaging, insulating materials, packaging materials and the like.
Specifically, the method comprises the following steps:
1) the invention prepares the highly devillicate fibrillar cellulose nanometer fiber by a mechanical method, and then prepares the composite film by combining the dipping method and the PBAT, the process is simple and the operation is convenient;
2) the cellulose nanofibrils used in the invention have rich surface hydroxyl groups and higher surface energy, and are firmly combined with PBAT through hydrogen bond action, intermolecular action and interface fusion action;
3) the cellulose nanofibril-PBAT composite film has the excellent performances of a nano cellulose film and a PBAT film, has good waterproof performance and large elongation at break, has adjustable light transmittance, is degradable, cannot cause damage to the environment, and can be widely applied to the fields of agricultural mulching films, product packaging, insulating materials, packaging materials and the like.
Drawings
FIG. 1 is an SEM image of the surface of a cellulose nanofibril-PBAT composite film of example 1.
FIG. 2 is a pictorial representation of a cellulose nanofibril-PBAT composite film of example 2.
FIG. 3 is an SEM image of the surface of the cellulose nanofibril-PBAT composite film of example 2.
FIG. 4 is a water drop contact angle plot of the cellulose nanofibril-PBAT composite film of example 3.
Fig. 5 is a physical representation of the cellulose nanofibril film of comparative example 1.
Fig. 6 is an SEM image of the surface of the cellulose nanofibril membrane of comparative example 1.
Fig. 7 is a diagram showing the degradation pathway of cellulose and PBAT in the cellulose nanofibril-PBAT composite film of the invention.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a preparation method of a cellulose nanofibril-PBAT composite film comprises the following steps:
1) hardwood pulp, 50g in dry weight, was added to water and soaked for 24 hours to prepare a cellulose suspension with a mass fraction of 1%, and then transferred to an ultrafine particle pulverizer (japan zengxi industrial co., model: MKCA6-2J), adjusting the rotation speed of the superfine particle pulverizer to 2000r/min, wherein the gap is 5 mu m, circularly pulverizing for 20 times, centrifuging, and re-dispersing the obtained solid product with water to obtain a cellulose nanofibril (the length is 200-1500 nm, and the diameter is 1-150 nm) dispersion liquid with the mass fraction of 1%;
2) adding 8g of nano-soil (with the particle size of 200-350 nm) dispersion with the mass fraction of 5% into 300g of cellulose nano-fibril dispersion with the mass fraction of 1%, and magnetically stirring for 1h to obtain cellulose nano-fibril-nano-soil mixed solution;
3) pouring the mixed solution of the cellulose nanofibril and the nano soil into a film casting container, and drying for 48 hours at 50 ℃ to obtain a cellulose nanofibril film;
4) and (2) immersing the cellulose nanofibril film into 40% of PBAT (number average molecular weight of 40000g/mol) acetone solution, soaking until the PBAT completely covers the surface of the cellulose nanofibril film, taking out, and drying at 200 ℃ for 0.5h to obtain the cellulose nanofibril-PBAT composite film (the mass fraction of the cellulose nanofibril is 51%, the mass fraction of the nano soil is 6.89%, and the mass fraction of the PBAT is 42.11%).
The Scanning Electron Microscope (SEM) image of the surface of the cellulose nanofibril-PBAT composite film prepared in this example is shown in fig. 1.
As can be seen from fig. 1: the cellulose nanofibril-PBAT composite film prepared by the embodiment has a smooth surface, and therefore, the interlayer spacing between the cellulose nanofibrils can be increased by the nano soil, so that the PBAT can better enter a cellulose nanofibril network structure in a heating state, the PBAT and the cellulose nanofibrils can be well combined, and the comprehensive performance of the material can be improved.
Example 2:
a preparation method of a cellulose nanofibril-PBAT composite film comprises the following steps:
1) softwood pulp with a dry weight of 100g was added to water, soaked for 36 hours, prepared into a cellulose suspension with a mass fraction of 3%, and transferred to an ultrafine particle pulverizer (japan zengxi industrial co., model: MKCA6-2J), adjusting the rotation speed of an ultrafine particle pulverizer to 4000r/min, wherein the gap is 20 microns, circularly pulverizing for 20 times, centrifuging, and re-dispersing the obtained solid product with water to obtain a cellulose nanofibril (the length is 200-2000 nm, and the diameter is 1-300 nm) dispersion liquid with the mass fraction of 3%;
2) adding 10.53g of nano-soil (with the particle size of 200 nm-500 nm) dispersion liquid with the mass fraction of 5% into 320g of cellulose nano-fibril dispersion liquid with the mass fraction of 3%, and magnetically stirring for 1h to obtain cellulose nano-fibril-nano-soil mixed liquid;
3) pouring the mixed solution of the cellulose nanofibril and the nano soil into a film casting container, and drying for 55 hours at 45 ℃ to obtain a cellulose nanofibril film;
4) soaking the cellulose nanofibril film into 30% of PBAT (number average molecular weight of 40000g/mol) tetrahydrofuran solution until the PBAT completely covers the surface of the cellulose nanofibril film, taking out the cellulose nanofibril film, and drying the cellulose nanofibril film for 1h at 130 ℃ to obtain the cellulose nanofibril-PBAT composite film (the mass fraction of the cellulose nanofibril is 73%, the mass fraction of the nano soil is 4.1%, and the mass fraction of the PBAT is 22.9%).
An actual view of the cellulose nanofibril-PBAT composite film prepared in this example is shown in fig. 2, and an SEM view of the surface is shown in fig. 3.
As can be seen from fig. 2 and 3: the cellulose nanofibril-PBAT composite film prepared by the embodiment has uniform surface and texture, the PBAT is covered on the surface of the composite film, and the cellulose nanofibril is completely wrapped by the PBAT.
Example 3:
a preparation method of a cellulose nanofibril-PBAT composite film comprises the following steps:
1) cotton pulp, 50g in dry weight, was added to water and soaked for 48 hours to prepare a cellulose suspension with a mass fraction of 5%, and then transferred to an ultrafine particle pulverizer (japan zengxi industrial co., model: MKCA6-2J), adjusting the rotation speed of an ultrafine particle pulverizer to 2500r/min, setting the gap to be 10 mu m, circularly pulverizing for 15 times, centrifuging, and re-dispersing the obtained solid product with water to obtain cellulose nanofibril (the length is 200-4000 nm, the diameter is 1-200 nm) dispersion liquid with the mass fraction of 5%;
2) adding 6.5g of nano soil (with the particle size of 250-500 nm) dispersion liquid with the mass fraction of 5% into 100g of cellulose nano fibril dispersion liquid with the mass fraction of 5%, and magnetically stirring for 1h to obtain cellulose nano fibril-nano soil mixed liquid;
3) pouring the mixed solution of the cellulose nanofibril and the nano soil into a film casting container, and drying for 65 hours at 40 ℃ to obtain a cellulose nanofibril film;
4) soaking the cellulose nanofibril film into 35% of PBAT (number average molecular weight of 50000g/mol) tetrahydrofuran-methanol solution (the volume ratio of tetrahydrofuran to methanol is 1:1), soaking until the PBAT completely covers the surface of the cellulose nanofibril film, taking out, and drying at 200 ℃ for 0.5h to obtain the cellulose nanofibril-PBAT composite film (the mass fraction of cellulose nanofibril is 62%, the mass fraction of nano soil is 4.2%, and the mass fraction of PBAT is 33.8%).
The water drop contact angle plot of the cellulose nanofibril-PBAT composite film prepared in this example is shown in fig. 4.
As can be seen from fig. 4: the composite film prepared by the embodiment has good hydrophobic property, the contact angle of a water drop is about 86 degrees, and compared with a common nano cellulose film, the hydrophobic property is obviously improved.
Example 4:
a preparation method of a cellulose nanofibril-PBAT composite film comprises the following steps:
1) bacterial cellulose, 50g in dry weight, was added to water and soaked for 24 hours to prepare a cellulose suspension with a mass fraction of 10%, and then transferred to an ultrafine particle pulverizer (japan zengxi industrial co., model: MKCA6-2J), adjusting the rotation speed of an ultrafine particle pulverizer to 1500r/min, adjusting the gap to 10 mu m, circularly pulverizing for 30 times, centrifuging, and re-dispersing the obtained solid product with water to obtain a cellulose nanofibril (the length is 200-4000 nm, and the diameter is 1-150 nm) dispersion liquid with the mass fraction of 10%;
2) adding 7g of nano-soil (with the particle size of 300-700 nm) dispersion with the mass fraction of 5% into 150g of cellulose nano-fibril dispersion with the mass fraction of 10%, and magnetically stirring for 1h to obtain cellulose nano-fibril-nano-soil mixed solution;
3) pouring the cellulose nanofibril-nano soil mixed solution into a film casting container, and drying for 144h at 35 ℃ to obtain a cellulose nanofibril film;
4) soaking the cellulose nanofibril film into 16% of PBAT (the number average molecular weight is 60000g/mol) tetrahydrofuran-acetonitrile solution (the volume ratio of tetrahydrofuran to acetonitrile is 2:1), soaking until the PBAT completely covers the surface of the cellulose nanofibril film, taking out, and drying at 300 ℃ for 0.5h to obtain the cellulose nanofibril-PBAT composite film (the mass fraction of cellulose nanofibril is 85%, the mass fraction of nano soil is 1.98%, and the mass fraction of PBAT is 13.02%).
Example 5:
a preparation method of a cellulose nanofibril-PBAT composite film comprises the following steps:
1) hardwood pulp (50 g by dry weight) and softwood pulp (50 g by dry weight) were added to water, soaked for 36 hours, prepared into a cellulose suspension with a mass fraction of 1%, and transferred to an ultrafine pulverizer (japan zengxi industrial co., model: MKCA6-2J), adjusting the rotation speed of the superfine particle pulverizer to 4500r/min, adjusting the gap to 10 μm, circularly pulverizing for 35 times, centrifuging, and re-dispersing the obtained solid product with water to obtain cellulose nanofibril (200-2000 nm in length and 1-200 nm in diameter) dispersion liquid with mass fraction of 8%;
2) adding 5.7g of nano soil (with the particle size of 500-800 nm) dispersion liquid with the mass fraction of 5% into 350g of cellulose nano fibril dispersion liquid with the mass fraction of 8%, and magnetically stirring for 1h to obtain cellulose nano fibril-nano soil mixed liquid;
3) pouring the mixed solution of the cellulose nanofibril and the nano soil into a film casting container, and drying for 48 hours at 50 ℃ to obtain a cellulose nanofibril film;
4) soaking the cellulose nanofibril film into 2% of PBAT (number average molecular weight is 80000g/mol) tetrahydrofuran-acetone solution (the volume ratio of tetrahydrofuran to acetone is 1:2), soaking until the PBAT completely covers the surface of the cellulose nanofibril film, taking out, and drying at 150 ℃ for 1h to obtain the cellulose nanofibril-PBAT composite film (the mass fraction of cellulose nanofibril is 98%, the mass fraction of nano soil is 0.98%, and the mass fraction of PBAT is 1.02%).
Comparative example 1:
a preparation method of a cellulose nanofiber film comprises the following steps:
1) softwood pulp with a dry weight of 100g was added to water, soaked for 36 hours, prepared into a cellulose suspension with a mass fraction of 6%, and transferred to an ultrafine particle pulverizer (japan zengxi industrial co., model: MKCA6-2J), adjusting the rotation speed of the superfine particle pulverizer to 3500r/min, the gap is 15 μm, circularly pulverizing for 25 times, centrifuging, and re-dispersing the obtained solid product with water to obtain 8% cellulose nanofibril (length 200 nm-2000 nm, diameter 1 nm-200 nm) dispersion liquid;
2) and pouring the cellulose nano fibril dispersion liquid into a film casting container, and drying at room temperature for one week to obtain the cellulose nano fibril film.
Fig. 5 shows a physical view of the cellulose nanofiber membrane prepared in this comparative example, and fig. 6 shows an SEM image of the surface.
As can be seen from fig. 5 and 6: the cellulose nanofiber membrane prepared by the comparative example is fluffy and porous in surface, obvious cellulose fiber distribution can be seen, and the structure can lead the cellulose nanofiber membrane to be hydrophilic and poor in water stability.
Comparative example 2:
a PBAT film, the preparation method of which comprises the following steps:
1) adding 25g of PBAT (the number average molecular weight is 60000g/mol) into 180mL of tetrahydrofuran, and stirring to prepare a PBAT tetrahydrofuran solution;
2) and pouring the PBAT tetrahydrofuran solution into a casting container, and drying for one week at 40 ℃ to obtain the PBAT film.
And (3) performance testing:
1) the cellulose nanofibril-PBAT composite films of examples 1 to 5, the cellulose nanofibril film of comparative example 1 and the PBAT film of comparative example 2 were tested for light transmittance, water drop contact angle, tensile strength and elongation at break, with reference to "determination of tensile properties of GB/T1040.1-2006, part 1: general test "test results obtained using a 500N test machine with 25mm spacing and 10mm/min pull rate using 500N sensors are shown in the following table:
TABLE 1 film light transmittance, water drop contact angle, tensile strength and elongation at break test results
As can be seen from Table 1: according to the invention, the cellulose nanofibril-PBAT composite films with different light transmittance, water resistance, tensile strength and elongation at break can be obtained by controlling the addition amounts of the cellulose nanofibril, the PBAT and the nano soil, and the actual requirements can be better met.
2) The degradation pathway of cellulose and PBAT in the cellulose nanofibril-PBAT composite film of the invention is shown in fig. 7.
As can be seen from fig. 7: the cellulose nanofibril-PBAT composite film is green and degradable, safe and environment-friendly.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The cellulose nanofibril-PBAT composite film is characterized by being prepared from the following raw materials in percentage by mass:
cellulose nanofibrils: 51 to 99 percent;
PBAT：1％～49％；
nano soil: 0 to 8 percent.
2. The cellulose nanofibril-PBAT composite film according to claim 1, characterized in that: the length of the cellulose nano-fibril is 200 nm-5000 nm, and the diameter is 1 nm-300 nm.
3. The cellulose nanofibril-PBAT composite film according to claim 1 or 2, characterized in that: the cellulose nanofibrils are made of at least one of softwood pulp, hardwood pulp, cotton pulp and bacterial cellulose.
4. The cellulose nanofibril-PBAT composite film according to claim 1 or 2, characterized in that: the number average molecular weight of the PBAT is 40000g/mol to 80000 g/mol.
5. The cellulose nanofibril-PBAT composite film according to claim 1 or 2, characterized in that: the particle size of the nano soil is 100 nm-1000 nm.
6. The method for producing a cellulose nanofibril-PBAT composite film according to any one of claims 1 to 5, comprising the steps of:
1) adding water into cellulose to prepare a cellulose suspension, and carrying out superfine grinding to obtain a cellulose nano fibril dispersion liquid;
2) dispersing nano soil in the cellulose nano fibril dispersion liquid to obtain a cellulose nano fibril-nano soil mixed liquid;
3) pouring the cellulose nanofibril-nano soil mixed solution into a film casting container for film casting to obtain a cellulose nanofibril film;
4) and (3) immersing the cellulose nanofibril film into the PBAT dispersion liquid for impregnation to obtain the cellulose nanofibril-PBAT composite film.
7. The method for producing a cellulose nanofibril-PBAT composite film according to claim 6, characterized in that: the gap of an ultrafine particle grinder adopted in the ultrafine grinding of the step 1) is 5-60 mu m, and the rotating speed is 1500-6000 r/min.
8. The method for producing a cellulose nanofibril-PBAT composite film according to claim 6 or 7, characterized in that: and 3) performing film casting at 30-80 ℃ for 24-240 h.
9. The method for producing a cellulose nanofibril-PBAT composite film according to claim 6 or 7, characterized in that: and 4) the solvent in the PBAT dispersion liquid is at least one of tetrahydrofuran, acetonitrile, acetone, methanol and ethanol.
10. Use of the cellulose nanofibril-PBAT composite film according to any one of claims 1 to 5 for the preparation of mulching films, packaging films, insulating films or encapsulation films.
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