CN111607203B - Reinforced and toughened poly (butylene adipate)/terephthalate-polylactic acid) composite film and preparation method thereof - Google Patents
Reinforced and toughened poly (butylene adipate)/terephthalate-polylactic acid) composite film and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of agricultural high polymer materials, and particularly relates to a reinforced and toughened poly (butylene adipate)/terephthalate-polylactic acid composite film and a preparation method thereof (epoxy)8 ) Extruding the mixture by a double-screw extruder after mixing, granulating by a granulator, and blowing a film product by a film blowing machine; the provided preparation method is simple, polylactic acid and poly (butylene adipate)/terephthalate which are widely available are used as main raw materials, the excellent performances of the polylactic acid and the poly (butylene adipate)/terephthalate are combined, and films with different air permeability are prepared by adding cage-shaped polysilsesquioxane containing octaepoxy groups with different contents, so that different actual use requirements can be met; the obtained film has excellent comprehensive performance, is a full-biodegradable film and plays an important role in relieving white pollution.
Description
Technical Field
The invention belongs to the field of agricultural high polymer materials, and particularly relates to a reinforced and toughened poly (adipic acid)/polybutylene terephthalate-polylactic acid composite film and a preparation method thereof.
Background
China is a large country with 14 hundred million people, the usage amount of plastic films is increasing every day, the plastic films comprise agricultural films, food packaging films, express packaging films, household garbage bags and the like, and the plastic films bring convenience for production and life of people and bring a series of severe ecological environment problems. Most of film products are usually discarded after being used, such as incinerated, buried or directly thrown away, which causes serious harm to the environment. At present, raw materials used by plastic film products are polyolefin resin with slow degradation, the polyolefin resin is difficult to decompose by microorganisms in soil under natural conditions (about 0.2 percent in 10 years), the residual time can reach more than 200 years, the soil structure can be changed due to burying or remaining the film in the soil, the soil hardening phenomenon is serious, and the porosity and the permeability of the soil are reduced; if the polyethylene film is burnt, inhalable particles (PM <2.5) can be generated, and after the polyvinyl chloride plastic film is burnt, highly toxic substances such as dioxin, furan and the like can be generated, and the burnt toxic substances can enter the underground along with rainfall and surface water, so that underground water resources are polluted. Although the state advocates to classify and recycle plastic film products, most plastic film products are polluted to different degrees after being used, and are difficult to recycle again.
As a novel film, the completely biodegradable film can be completely degraded in the natural world and becomes a hotspot of current research, wherein the poly (butylene adipate/terephthalate) -polylactic acid (PBAT/PLA) composite film is mostly researched, a lot of patents exist for preparing films by blending the PBAT/PLA at present, and in order to improve the compatibility between the PABT and the PLA, an organic micromolecule compatilizer is mostly added; inorganic fillers are often added to improve the mechanical properties of the composite film, and organic small molecule dispersants are also used to increase the dispersibility of the inorganic fillers, but the application field of the film is limited to a certain extent because the organic small molecules are easily precipitated from the resin during the use.
Therefore, how to effectively overcome the problems in the prior art and provide a better fully biodegradable film becomes one of the problems to be solved by those skilled in the art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a reinforced and toughened polybutylene adipate/terephthalate-polylactic acid (PBAT/PLA) composite film and a preparation method thereof, and the specific scheme is that firstly, granules of the polybutylene adipate/terephthalate and the polylactic acid and cage-shaped Polysilsesquioxane (POSS) containing an octaepoxy group (epoxy)8 ) Extruding the mixture by a double-screw extruder after mixing, granulating by a granulator, and blowing a film product by a film blowing machine; the provided preparation method is simple, polylactic acid and poly (butylene adipate)/terephthalate which are widely available are used as main raw materials, the excellent performances of the polylactic acid and the poly (butylene adipate)/terephthalate are combined, and films with different air permeability are prepared by adding cage-shaped polysilsesquioxane containing octaepoxy groups with different contents, so that different actual use requirements can be met; the obtained film has excellent comprehensive performance, is a full-biodegradable film and plays an important role in relieving white pollution.
The invention has the main invention point that POSS cage-shaped silane is adopted as the nucleating agent, which not only can play a role in strengthening and toughening, but also can play a role in organic compatibilizer because the POSS cage-shaped silane contains a plurality of epoxy groups, and other auxiliary agents are not required to be additionally added, so that compared with the prior art, the invention has obvious improvement on the aspect that the POSS cage-shaped Polysilsesquioxane (POSS) containing the octaepoxy groups is adopted (epoxy)8 ) The chemical formula is as follows:
the octaepoxy group cage Polysilsesquioxane (POSS) (epoxy)8 ) In the prior art, the coating is mainly applied to organic glass coating and the like; it is usually used as a 2 wt.% additive to impart coatingsLayer adhesion and durability. It can also be used as a carrier for ingredients in coatings and resins, and it can also be surface vitrified under oxygen plasma, corona, and UV to provide a tie layer for coatings or to increase scratch and mar resistance, by a mechanism of hydrogen bonding interactions.
However, before the invention appeared, the technical inspiration of applying the composite film to the composite film never appeared, and the composite film has obvious difference from the fields of the coating and the like in performance and form, and the preparation method has obvious difference.
Due to the adoption of the cage-shaped Polysilsesquioxane (POSS) containing the octaepoxy group (epoxy)8 ) Compared with the prior art, the technical scheme of the invention is greatly changed, and the method comprises the following steps:
a reinforced and toughened polylactic acid/(poly adipic acid/butylene terephthalate) composite film comprises the following main components in parts by weight:
10-20 parts of polylactic acid and 80-90 parts of poly (butylene adipate/terephthalate);
based on the two main film-forming components, 0.1-5% of cage Polysilsesquioxane (POSS) containing octaepoxy groups is added according to the total weight of the two (epoxy)8 ) (ii) a The content is too low to achieve the purposes of connecting two phases and strengthening and toughening, and the content is too high to increase the cost of the product, which is not favorable for popularization and application; thus controlling the above dosage range;
preferably, the mass ratio of polylactic acid to poly (butylene adipate)/terephthalate is 15: 85; cage Polysilsesquioxane (POSS) containing eight epoxy groups (epoxy)8 ) The addition amount of (B) is 0.1-5% of the total weight of the two, and within the addition range, the finally obtained film product can achieve the best balance state on the reverse side of the longitudinal and transverse tensile strength and the elongation at break, and belongs to the best embodiment.
Due to the addition of the cage-type silsesquioxane containing epoxy groups, the compatibility of the poly (adipic acid)/butylene terephthalate/polylactic acid is greatly improved, the mechanical property is obviously improved, the processability is better, the gas transmittance of the film can be adjusted through the proportion of various components, and the requirements on the performance of the film under different working conditions are met; the finally obtained film is a degradable film, so that the environmental pollution is reduced.
Furthermore, for better processing, the particle size of the polylactic acid and the polybutylene adipate/terephthalate as raw materials is generally controlled to be 3-6mm, and the particle size range of the finally obtained polylactic acid/polybutylene adipate/terephthalate composite material is also controlled to be 3-6 mm;
it can be seen that the technical scheme of the application only adopts three raw materials, namely, the cage-type silsesquioxane containing epoxy groups, the polylactic acid and the poly adipic acid/butylene terephthalate, which are simpler than the prior art and provide possibility for a subsequent simpler preparation method, and the preparation method comprises the following steps:
adding polylactic acid, poly (butylene adipate/terephthalate) and cage-shaped polysilsesquioxane containing an octaepoxy group into a double-screw extruder in proportion, wherein the temperature from a first zone to a head is 170-180 ℃, 180-190 ℃, 190-200 ℃, 170-185 ℃ and the rotating speed is 60-100r/min in sequence, and the granules are molten and undergo ring-opening reaction under the action of high temperature and shearing force. And extruding and cooling by an extruder, and granulating by a granulator. Blowing the mixture into a required film by a film blowing machine;
the temperature range mentioned above is a specific adjustment made by the inventors of the present invention to the composition of the present application, particularly, to the addition of the octaepoxy group-containing cage polysilsesquioxane, and the temperature range is slightly increased.
In conclusion, the cage-shaped polysilsesquioxane containing the octaepoxy group is creatively added into a poly adipic acid/butylene terephthalate-polylactic acid system as a raw material to obtain a master batch material which can be used as a film blowing raw material, and a film prepared from the master batch material has better performance, simple process operation, strong controllability, stable product performance, no pollutant generation in the production process, green and environment-friendly process and conforms to the green sustainable development concept.
Drawings
FIG. 1 is a schematic diagram showing the water vapor transmission rate of films of cage-like silsesquioxane with different octaepoxy groups added;
FIG. 2 shows O in films of cage-like silsesquioxane with different octaepoxy groups added 2 And CO 2 A transmittance diagram;
in the figure, the POSS-0 is the POSS addition amount of 0, the POSS-1 is the POSS addition amount of 1%, and the POSS-5 is the POSS addition amount of 5%.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The materials are commercially available from the open literature unless otherwise specified.
Example 1:
and (2) stirring dried 850g of polybutylene adipate/terephthalate granules, 150g of polylactic acid granules and 1g of cage-type silsesquioxane containing an octaepoxy group, adding the mixture into a double-screw extruder, wherein the temperature from the first zone to a machine head is 170 ℃, 180 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 180 ℃, the rotation speed of the double-screw extruder is 60r/min, cooling the materials after the materials are extruded by the machine head, and guiding the materials to a high-speed granulator by a traction device for granulation. And drying the granules again, pouring the granules into a film blowing machine for film blowing, and blowing the film with the required specification by adjusting the rotation speed, the temperature, the traction speed, the curling speed, the blowing speed and the like of the screw. The film can be packaged and stored after being cooled. The resulting film had a tensile strength of 29.71MPa in the machine direction and 19.82MPa in the transverse direction. The elongation at break was 551% and 690% in the longitudinal and transverse directions, respectively.
Example 2:
and (2) stirring dried 850g of polybutylene adipate/terephthalate granules, 150g of polylactic acid granules and 5g of cage-type silsesquioxane containing an octaepoxy group, adding the mixture into a double-screw extruder, wherein the temperature from the first zone to a machine head is 170 ℃, 180 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 180 ℃, the rotation speed of the double-screw extruder is 60r/min, cooling the material after the material is extruded by the machine head, and guiding the material to a high-speed granulator by a traction device for granulation. And drying the granules again, pouring the granules into a film blowing machine for film blowing, and blowing the film with the required specification by adjusting the rotation speed, the temperature, the traction speed, the curling speed, the blowing speed and the like of the screw. The film can be packaged and stored after being cooled. The tensile strength of the obtained film in the longitudinal direction is 30.06MPa, and the tensile strength of the film in the transverse direction is 19.40 MPa. Elongation at break was 555% and 647% in the machine and transverse directions, respectively.
Example 3:
and (2) stirring 850g of dried polybutylene adipate/terephthalate granules, 150g of polylactic acid granules and 10g of cage-type silsesquioxane containing an octaepoxy group, adding the mixture into a double-screw extruder, wherein the temperature from the first zone to a machine head is 170 ℃, 180 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 180 ℃, the rotation speed of the double-screw extruder is 60r/min, cooling the material after the material is extruded by the machine head, and guiding the material to a high-speed granulator by a traction device for granulation. And drying the granules again, pouring the granules into a film blowing machine for film blowing, and blowing the film with the required specification by adjusting the rotation speed, the temperature, the traction speed, the curling speed, the blowing speed and the like of the screw. The film can be packaged and stored after being cooled. The resulting film had a tensile strength of 29.34MPa in the machine direction and 19.46MPa in the transverse direction. Elongation at break was 564% and 667% in the machine direction and the cross direction, respectively.
Example 4:
and (2) stirring dried 850g of polybutylene adipate/terephthalate granules, 150g of polylactic acid granules and 30g of cage-type silsesquioxane containing an octaepoxy group, adding the mixture into a double-screw extruder, wherein the temperature from the first zone to a machine head is 170 ℃, 180 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 180 ℃, the rotation speed of the double-screw extruder is 60r/min, cooling the materials after the materials are extruded by the machine head, and guiding the materials to a high-speed granulator by a traction device for granulation. And drying the granules again, pouring the granules into a film blowing machine for film blowing, and blowing the film with the required specification by adjusting the rotation speed, the temperature, the traction speed, the curling speed, the blowing speed and the like of the screw. The film can be packaged and stored after being cooled. The tensile strength of the obtained film in the longitudinal direction is 28.00MPa, and the tensile strength of the film in the transverse direction is 18.06 MPa. The elongation at break was 598% and 698% in the longitudinal and transverse directions, respectively.
Example 5:
and (2) stirring 850g of dried polybutylene adipate/terephthalate granules, 150g of polylactic acid granules and 50g of cage-type silsesquioxane containing an octaepoxy group, adding the mixture into a double-screw extruder, wherein the temperature from the first zone to a machine head is 170 ℃, 180 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 180 ℃, the rotation speed of the double-screw extruder is 60r/min, cooling the material after the material is extruded by the machine head, and guiding the material to a high-speed granulator by a traction device for granulation. And drying the granules again, pouring the granules into a film blowing machine for film blowing, and blowing a film with a required specification by adjusting the rotation speed of a screw, the temperature, the drawing speed, the curling speed, the blowing speed and the like. The film can be packaged and stored after being cooled. The resulting film had a tensile strength of 29.06MPa in the machine direction and 17.77MPa in the transverse direction. The elongation at break was 589% and 751% in the machine and transverse directions, respectively.
Comparative example:
and (2) stirring 850g of dried polybutylene adipate/terephthalate granules, 150g of polylactic acid granules and 0g of cage-type silsesquioxane containing an octaepoxy group, adding the mixture into a double-screw extruder, wherein the temperature from the first zone to a machine head is 170 ℃, 180 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 180 ℃, the rotation speed of the double-screw extruder is 60r/min, cooling the material after the material is extruded by the machine head, and guiding the material to a high-speed granulator by a traction device for granulation. And drying the granules again, pouring the granules into a film blowing machine for film blowing, and blowing a film with a required specification by adjusting the rotation speed of a screw, the temperature, the drawing speed, the curling speed, the blowing speed and the like. The film can be packaged and stored after being cooled. The resulting film had a tensile strength of 23.92MPa in the machine direction and 12.82MPa in the transverse direction. Elongation at break 506%, 454% in the machine and transverse directions, respectively.
Besides the polylactic acid (PLA) and the polybutylene adipate/terephthalate (PBAT), other resins with hydroxyl or carboxyl end capping groups can be applied to the system of the invention, but for reasons of space, the detailed description is omitted here, and the patents extended on this basis are protected by the present invention.
Experimental example 1
The data described in the above examples and comparative examples were obtained by the following experimental methods:
the composite films obtained in the examples and comparative examples on the market were subjected to the relevant mechanical property tests using an electronic universal tensile tester UTM 2502. The test contents are the transverse and longitudinal stretching performance and the transverse and longitudinal tearing performance of the composite film. The tensile test standard is in accordance with the national standard GB/T1040.3-2006. The sample used in the tensile test is cut by a special dumbbell-shaped cutter, and the tensile speed in the experimental test is 500mm min -1 . The sample used for tearing test is cut by a right-angle professional cutter, the national standard QB/T1130-91 is used, and the tearing speed is 200mm min -1 . Data were measured for 15 samples per group, and then averaged as final data. The mechanical properties are compared and referred to national standard GB13735-92, and Table 1 shows the comparison results of tensile strength and elongation at break of comparative examples and examples;
TABLE 1 comparative examples and examples tensile Strength and elongation at Break comparison results
As can be seen from the tensile strength results of the samples, the octaepoxy group-added cage-like silsesquioxane (POSS) (epoxy)8 ) The longitudinal and transverse tensile strength of the composite film is far higher than that of cage-like silsesquioxane (POSS) without added octaepoxy group (epoxy)8 ) The maximum amplification in the longitudinal direction and the transverse direction of the film is respectively 25.7 percent and 51.8 percent, and the effect is very obvious. And the difference between the longitudinal direction and the transverse direction is that octaepoxy group is added into cage-shaped silsesquioxane (POSS) (epoxy)8 ) And later, the size is reduced, so that the compatibility of the system is promoted by adding POSS, and the inorganic core of POSS plays a role in enhancing, so that the mechanical property of the film is improved as a whole. As is clear from the results of elongation at break, cage-like silsesquioxane (POSS) having an octaepoxy group added thereto (epoxy)8 ) Then, the elongation at break of the composite film in the longitudinal and transverse directions is greatly improved, and the maximum amplitudes in the longitudinal and transverse directions are respectively18.2 percent and 65.5 percent, and the effect is obvious. And the difference in elongation at break in the longitudinal and transverse directions is also decreasing. The POSS is cage-shaped siloxane, is of a hollow structure and has the function similar to an elastic ball, so that the elongation at break of the composite film is greatly improved.
Experimental example 2
The inventor adds water vapor and O of the film to the cage-shaped silsesquioxane with different octaepoxy groups according to GB/T1037-1988 test method for water vapor permeability of plastic film and sheet material-cup method 2 And CO 2 The transmittance was measured and the results are shown in FIGS. 1 and 2;
the water vapor permeability coefficient is increased along with the increase of the content of the cage-like silsesquioxane with the octaepoxy group, and the cage-like silsesquioxane composite film with the octaepoxy group has O pairs 2 And CO 2 Has selectivity for permeation of CO 2 Is more permeable than O 2 The penetration amount of the POSS is slightly more, and simultaneously, the cage-shaped hollow structure of the POSS is proved, so that reference is provided for the application expansion of the composite film.
The inventor also carried out a fresh-keeping development experiment of three foods, and found that the mushrooms, the strawberries and the bananas packaged by the Polyethylene (PE) film are rotten after eleven days; the mushrooms packaged by the PBAT/PLA composite film without POSS are browned, but the influence of bananas and strawberries is little. Therefore, the PBAT/PLA composite film also has selectivity on the fresh-keeping of food; the PBAT/PLA composite film with the POSS addition content of 1% has the best comprehensive fresh-keeping effect.
Claims (3)
1. A reinforced and toughened poly (butylene adipate/terephthalate) -polylactic acid composite film is characterized in that: the main components are as follows by weight:
10-20 parts of polylactic acid and 80-90 parts of poly (butylene adipate/terephthalate);
0.1-5% of cage polysilsesquioxane containing octaepoxy groups is added according to the total weight of the two.
2. The reinforced and toughened composite poly (butylene adipate/terephthalate) -poly (lactic acid) film as claimed in claim 1, wherein: the mass ratio of polylactic acid to poly (adipic acid)/polybutylene terephthalate is 15: 85.
3. The preparation method of the reinforced and toughened poly (butylene adipate/terephthalate) -polylactic acid composite film as claimed in claim 1, wherein: the method comprises the following specific steps:
adding polylactic acid, polybutylene adipate/terephthalate and cage polysilsesquioxane containing eight epoxy groups into a double-screw extruder according to a ratio, wherein the temperature from a first region to a machine head is sequentially 170 + 180 ℃, 180 + 190 ℃, 190 + 200 ℃, 170 + 185 ℃, the rotating speed is 60-100r/min, the granules are molten, and an open-loop reaction is carried out under the action of high temperature and shearing force; after being extruded and cooled by an extruder, the mixture is granulated by a granulator; and then blowing the mixture into a required film by a film blowing machine.
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| CN110387112A (en) * | 2019-07-23 | 2019-10-29 | 湖南工业大学 | A kind of degradable food packaging membrane material and preparation process |
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