CN115403907B - Single-layer heat-sealable biaxially oriented polylactic acid film and preparation method thereof - Google Patents
Single-layer heat-sealable biaxially oriented polylactic acid film and preparation method thereof Download PDFInfo
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- CN115403907B CN115403907B CN202211199832.1A CN202211199832A CN115403907B CN 115403907 B CN115403907 B CN 115403907B CN 202211199832 A CN202211199832 A CN 202211199832A CN 115403907 B CN115403907 B CN 115403907B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/31—Heat sealable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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Abstract
The application discloses a single-layer heat-sealable biaxially oriented polylactic acid film and a preparation method thereof. The single-layer heat-sealable biaxially oriented polylactic acid film comprises 10-40% by weight of crystalline polylactic acid and the balance of amorphous polylactic acid, wherein the crystalline polylactic acid is L-type polylactic acid, and the content of D-lactic acid is 2.5% or less than X D Less than or equal to 4.5 percent. The application ensures that the thickness of the single-layer heat-sealable BOPLA film obtained by heat setting process treatment is uniform by limiting the contents of the crystalline polylactic acid and the D-lactic acid in the formula, and still maintains higher heat sealing strength, thereby meeting the use requirement of the packaging film. In addition, the heat-sealing BOPLA film can be used as a heat-sealing film with a single-layer structure, and also can be used as a surface heat-sealing layer for a heat-sealing film with a multi-layer structure.
Description
Technical Field
The application relates to a biaxially oriented polylactic acid film, in particular to a monolayer heat-sealable biaxially oriented polylactic acid film and a preparation method thereof.
Background
Polylactic acid (PLA) is a degradable plastic which has renewable raw material sources, can be biologically degraded by 100 percent, and has high mechanical strength, good transparency and easy processing and forming. Biaxially oriented polylactic acid (BOPLA) film prepared by taking PLA as raw material is regarded as the degradable packaging material with the most development prospect under the background of increasingly serious plastic inhibition policies due to good mechanical property and optical property. When a bopa film is used as a packaging material, heat sealability is often required.
The heat sealing technology of the polylactic acid film in the prior art mainly comprises two kinds: one is to use amorphous polylactic acid (i.e. polylactic acid with amorphous structure), as disclosed in the patent publication No. CN104608448A, a biaxially oriented polylactic acid film with ABC three-layer structure capable of being directly heat-sealed is disclosed, which sequentially comprises a surface heat-sealing layer, a middle core layer and an anti-adhesion layer, wherein the surface heat-sealing layer is prepared from heat-sealing PLA slices containing 80-90 wt% of crystalline PLA and 10-20 wt% of amorphous PLA. Another technique is to add flexible molecules and tackifier to make the polylactic acid film heat-sealable, for example, the application patent with publication number CN102924883a discloses a blow-molded biodegradable polyester composition film with high heat-sealing strength, which contains flexible polymer material a (such as polybutylene succinate, etc.), substance B copolymerized with PLA, substance C containing linear PLA and branched PLA, solubilizer substance D and tackifier substance E.
The polylactic acid film has three molding methods, such as blow molding, casting and biaxial stretching. The PLA film prepared by biaxial stretching has higher mechanical strength and better optical performance, and is the first choice process of the packaging film. The existing researches show that the film which is not subjected to heat setting has serious shrinkage after heat sealing, and the heat setting treatment is carried out on the biaxially oriented film to ensure that the film has better dimensional stability, so that the existing preparation process flow of the biaxially oriented film comprises the following steps: extruding a casting sheet, longitudinally stretching, transversely stretching, heat setting, and traction and rolling.
The inventor groups find that in the production and the test, in the heat-sealing type BOPLA film, the content of the crystalline PLA and the content of the D-lactic acid in the crystalline PLA are very important, so that the heat-sealing strength of the heat-sealing type BOPLA film is greatly influenced, and the heat-sealing part film is also influenced on whether the film is shrunk or not; and the heat-sealing type BOPLA film which does not limit the D-lactic acid in the crystalline PLA even loses heat-sealing performance after heat setting treatment. None of these have been reported publicly in the prior art.
On the other hand, the heat-sealing type BOPLA film generally adopts a multi-layer structure due to poor heat stability of a heat sealing layer, and at least one layer of the heat-sealing type BOPLA film has high heat stability. The heat-sealing BOPLA film disclosed in the patent publication No. CN104608448A has a three-layer structure, wherein the middle core layer is formed by slicing crystalline PLA with high heat stability, and specifically comprises 97-99% by weight of crystalline PLA and 1-3% by weight of amorphous PLA. As another patent of the application with publication number of CN 114193890A, a heat-sealable biaxially-oriented polylactic acid smoke film with degradable low water vapor permeability is disclosed, the film layer structure of the smoke film comprises a bopa film layer and a water vapor barrier layer, the bopa film layer is composed of three layers of co-extruded biaxially-oriented PLA films, a surface layer, a core layer and an inner layer are sequentially arranged from bottom to top, and the raw material components of the surface layer comprise 80.0-90.0 parts of crystalline polylactic acid slices, 9.4-18.0 parts of amorphous polylactic acid slices, 0.50-1.00 parts of opening agent and 0.10-1.00 parts of slipping agent; the core layer is composed of crystalline polylactic acid slices with higher thermal stability. At present, no report on a heat-sealable biaxially oriented polylactic acid film with a single-layer structure and good heat stability and heat sealing strength is available.
Disclosure of Invention
The application aims to solve the technical problem of providing a single-layer heat-sealable biaxially oriented polylactic acid film with a single-layer structure, uniform thickness and excellent heat sealing performance and a preparation method thereof.
In order to solve the technical problems, the application adopts the following technical scheme:
a single-layer heat-sealable biaxially oriented polylactic acid film comprises 10-40% by weight of crystalline polylactic acid and the balance of non-crystalline polylactic acid, wherein the crystalline polylactic acid is L-shaped polylactic acid, and the content of D-lactic acid in the crystalline polylactic acid is 2.5% or less than or equal to X D ≤4.5％(X D Represents the content of D-lactic acid).
The applicant found in experiments that the content of crystalline polylactic acid and the content of D-lactic acid in the crystalline polylactic acid have a very significant effect on the heat seal strength and thickness of the heat seal BOPLA film of the monolayer structure and also on whether the film is shrunk at the heat seal. When the content of the crystalline polylactic acid and the content of the D-lactic acid in the crystalline polylactic acid are within the above-mentioned limit ranges, the heat-seal type BOPLA film after heat setting treatment has no shrinkage phenomenon at the heat-seal position, and can also meet the heat-seal strength requirement of a general packaging film on the heat-seal film (the heat-seal strength requirement of the general packaging film on the heat-seal film is 2N/15 mm). The applicant also finds through experiments that when the content of the crystalline polylactic acid is too low, the thickness of the heat-sealing BOPLA film with a single-layer structure is uneven after heat setting treatment, and the thickness of the film is greatly reduced; the lower the D-lactic acid content in the crystalline polylactic acid, the higher the crystallization ability of the crystalline polylactic acid; when the single-layer heat-sealing BOPLA film is prepared, the heat-sealing strength of the heat-sealing BOPLA film is greatly reduced after heat setting treatment, and even the heat-sealing performance is lost due to the fact that the content of D-lactic acid in the crystalline polylactic acid is too low.
In order to obtain better processability, the weight average molecular weight (Mw) of the crystalline polylactic acid is preferably 14.3 to 25 ten thousand, and the weight average molecular weight of the amorphous polylactic acid is preferably 15 to 21 ten thousand.
In order to obtain a better heat seal strength of the resulting monolayer heat-sealable BOPLA film, it is preferable that the content of D-lactic acid in the crystalline polylactic acid is 3.0% or less X under other conditions D ≤4.0％。
Preferably, the monolayer heat-sealable biaxially oriented polylactic acid film of the present application comprises, by weight, 10 to 30% of crystalline polylactic acid and the balance of amorphous polylactic acid, more preferably 15 to 25% of crystalline polylactic acid and the balance of amorphous polylactic acid.
The application also provides a preparation method of the single-layer heat-sealable biaxially oriented polylactic acid film, which comprises the following steps: and (3) weighing the crystalline polylactic acid and the amorphous polylactic acid according to the formula, uniformly mixing, extruding, casting, biaxially stretching and heat setting to obtain the polylactic acid.
In the preparation method, the operations of extrusion, sheet casting, biaxial stretching, heat setting and the like are the same as those in the prior art, and specifically, a double-screw extruder is adopted for mixing, extruding and sheet casting, wherein the temperature of a charging barrel of the double-screw extruder is 130-230 ℃ during extrusion, and the temperature of a die head is 190-220 ℃; cooling the cast sheet at 30-50 ℃; the biaxial stretching is asynchronous biaxial stretching and is carried out at 50-80 ℃; the heat setting temperature is 90-110 ℃.
Furthermore, the application also discloses a multilayer heat-sealable biaxially oriented polylactic acid film, which comprises a surface heat-sealing layer, wherein the surface heat-sealing layer is made of the single-layer heat-sealable biaxially oriented polylactic acid film.
Compared with the prior art, the application is characterized in that:
1. the heat-sealing BOPLA film can be used as a heat-sealing film with a single-layer structure, and also can be used as a surface heat-sealing layer for a heat-sealing film with a multi-layer structure.
2. The application ensures that the single-layer heat-sealable BOPLA film obtained by heat setting process treatment has even thickness, no shrinkage phenomenon at the heat sealing position and still keeps higher heat sealing strength by limiting the contents of the crystalline polylactic acid and the D-lactic acid in the formula, thereby meeting the use requirement of the packaging film.
Detailed Description
In order to better explain the technical scheme of the present application, the present application will be described in further detail with reference to examples, but the embodiments of the present application are not limited thereto.
In the following examples, crystalline polylactic acid is also simply referred to as crystalline PLA, and amorphous polylactic acid is also simply referred to as amorphous PLA.
Example 1
According to weight percentage, 20 percent of crystallization type PLA (D-lactic acid content is 3.2 percent, mw is 16 ten thousand) and 80 percent of non-crystallization type PLA (Mw is 21 ten thousand) are placed in a double screw extruder to be uniformly mixed, then the mixture is extruded by the double screw extruder (the extrusion temperature is 210 ℃ and the die head temperature is 200 ℃), a casting sheet is cooled (30 ℃), and then the casting sheet is subjected to longitudinal and transverse asynchronous biaxial stretching for 4 times (50-80 ℃), and then the heat setting is carried out at 100 ℃ to obtain the single-layer heat-sealable BOPLA film.
Comparative example 1
Unlike example 1, the BOPLA film was not heat-set.
Example 2
A single layer heat sealable BOPLA film was prepared by the same process as in example 1, taking 30% crystalline PLA (D-lactic acid content 3.2%, mw 16 ten thousand) and 70% amorphous PLA (Mw 21 ten thousand) by weight percent, placing them in a twin screw extruder.
Comparative example 2-1
Unlike example 2, the D-lactic acid content in the crystalline PLA was 2.3%.
Comparative examples 2 to 2
Unlike example 2, the D-lactic acid content in the crystalline PLA was 5.2%.
Example 3
A single layer heat sealable BOPLA film was prepared by the same process as in example 1, with 40% crystalline PLA (D-lactic acid content 3.2%, mw 16 ten thousand) and 60% amorphous PLA (Mw 21 ten thousand) placed in a twin screw extruder in weight percent.
Comparative example 3
Unlike example 3, the crystalline PLA was changed to 50wt% and the amorphous PLA was changed to 50wt%.
Example 4
10% of crystalline PLA (D-lactic acid content 3.2%, mw 25 ten thousand) and 90% of amorphous PLA (Mw 15 ten thousand) were placed in a twin-screw extruder by weight percent, and a single-layer heat-sealable BOPLA film was produced by the same process as in example 1.
Comparative example 4-1
Unlike example 4, the crystalline PLA was changed to 0wt% and the amorphous PLA was changed to 100wt%.
Comparative example 4-2
Unlike example 4, the crystalline PLA was changed to 8wt% and the amorphous PLA was changed to 92wt%.
Example 5
A single layer heat sealable BOPLA film was prepared by the same process as in example 1, with 25% crystalline PLA (D-lactic acid content 4.5%, mw 20 ten thousand) and 75% amorphous PLA (Mw 18 ten thousand) placed in a twin screw extruder in weight percent.
Example 6
A single layer heat sealable BOPLA film was prepared by the same process as in example 1, taking 30% crystalline PLA (D-lactic acid content 2.5%, mw 21 ten thousand) and 70% amorphous PLA (Mw 20 ten thousand) by weight percent, placing them in a twin screw extruder.
Example 7
A single layer heat sealable BOPLA film was prepared by the same process as in example 1, taking 15% crystalline PLA (D-lactic acid content 3.5%, mw 14.3 ten thousand) and 85% amorphous PLA (Mw 18 ten thousand) by weight percent in a twin screw extruder.
The heat seal strength of the films prepared in the above examples and comparative examples was evaluated, and the heat seal conditions of the BOPLA films were unified at 85℃C 80℃C 133kPa/2s. The heat seal strength test bars were 150mm long and 15mm wide, the gap spacing was 100mm, the test speed was 100mm/min, and the maximum load of the test specimen breaking at the heat seal was read as the heat seal strength of the bars in N/15mm. The heat-seal strength of the film after heat setting is defined as losing heat-seal property which is smaller than 2N/15mm required by the heat-seal strength of the general packaging film, namely the heat-seal strength of the film after heat setting is smaller than 2N/15 mm. The results are shown in Table 1 below.
Table 1:
it can be seen from examples 1 to 4 that the heat-seal type BOPLA film has a great influence on the heat-seal strength of the film after heat-setting, and the heat-seal strength of the film is greatly reduced with the increase of the content of the crystalline PLA. From comparison between example 1 and comparative example 1, it can be seen that the heat-setting treatment has a great influence on the flatness of the film after heat-sealing, and the film without heat-setting treatment is severely shrunk after heat-sealing. Example 2 and comparative examples 2-1 and 2-2 show that the content of D-lactic acid in crystalline PLA greatly affects the heat sealing property of a heat-sealing BOPLA film, and that the lower the content of D-lactic acid in crystalline PLA, the stronger the crystallization ability of polylactic acid, the more obviously the heat sealing strength of the heat-sealing polylactic acid is reduced, even the heat sealing property is lost; the higher the content of D-lactic acid in the crystalline PLA, the poorer the dimensional stability of the film. As can be seen from comparison of examples 1, 4 and 7, when the content of crystalline PLA in the heat-sealable BOPLA film is small, the thickness of the film after heat-setting is reduced, but the effect is not great. Example 4 and comparative examples 4-1 and 4-2 show that when the heat-seal type BOPLA film does not contain crystalline PLA, the film cannot withstand heat setting treatment, the thickness of the heat-set film is greatly reduced, even the film is broken, and normal use and test cannot be performed; the heat-sealable BOPLA film contains crystalline PLA, but even when the crystalline PLA content is low, the film cannot be given good dimensional stability.
Claims (8)
1. A single-layer heat-sealable biaxially oriented polylactic acid film is characterized by comprising 10-40% by weight of crystalline polylactic acid and the balance of non-crystalline polylactic acid, wherein the crystalline polylactic acid is L-shaped polylactic acid, and the content of D-lactic acid in the crystalline polylactic acid is 2.5% -X D ≤4.5%；
The preparation method of the single-layer heat-sealable biaxially oriented polylactic acid film comprises the following steps: and (3) weighing the crystalline polylactic acid and the amorphous polylactic acid according to the formula, uniformly mixing, extruding, casting, biaxially stretching and heat setting to obtain the polylactic acid.
2. The monolayer heat-sealable biaxially oriented polylactic acid film of claim 1, wherein the crystalline polylactic acid has a weight average molecular weight of 14.3 to 25 ten thousand.
3. The monolayer heat-sealable biaxially oriented polylactic acid film of claim 1, wherein the weight average molecular weight of the amorphous polylactic acid is 15 to 21 ten thousand.
4. The monolayer heat-sealable biaxially oriented polylactic acid film of claim 1, wherein the crystalline polylactic acid has a D-lactic acid content of 3.0% or less than X D ≤4.0%。
5. The monolayer heat-sealable biaxially oriented polylactic acid film of any of claims 1 to 4, wherein the film comprises, by weight, 10 to 30% of crystalline polylactic acid and the balance amorphous polylactic acid.
6. The monolayer heat-sealable biaxially oriented polylactic acid film of claim 5, wherein the film comprises, by weight, 15 to 25% of crystalline polylactic acid and the balance amorphous polylactic acid.
7. The method for preparing the monolayer heat-sealable biaxially oriented polylactic acid film according to claim 1, which is characterized in that the preparation method comprises the steps of weighing crystalline polylactic acid and amorphous polylactic acid according to a formula, uniformly mixing, extruding, casting, biaxially oriented drawing and heat setting.
8. A multilayer heat-sealable biaxially oriented polylactic acid film comprises a surface heat-sealing layer, and is characterized in that the surface heat-sealing layer is made of the single-layer heat-sealable biaxially oriented polylactic acid film according to claim 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104608448A (en) * | 2015-01-30 | 2015-05-13 | 山东圣和塑胶发展有限公司 | Two-way stretch polylactic acid film capable of being directly thermally sealed and preparation method of two-way stretch polylactic acid film |
| CN112297560A (en) * | 2020-10-30 | 2021-02-02 | 安徽国风塑业股份有限公司 | Antibacterial two-way stretching polylactic acid film capable of being directly heat-sealed and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US9150004B2 (en) * | 2009-06-19 | 2015-10-06 | Toray Plastics (America), Inc. | Biaxially oriented polylactic acid film with improved heat seal properties |
| US20120141766A1 (en) * | 2010-12-07 | 2012-06-07 | Toray Plastics (America), Inc. | Biaxially oriented cavitated polylactic acid film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104608448A (en) * | 2015-01-30 | 2015-05-13 | 山东圣和塑胶发展有限公司 | Two-way stretch polylactic acid film capable of being directly thermally sealed and preparation method of two-way stretch polylactic acid film |
| CN112297560A (en) * | 2020-10-30 | 2021-02-02 | 安徽国风塑业股份有限公司 | Antibacterial two-way stretching polylactic acid film capable of being directly heat-sealed and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 双向拉伸聚乳酸薄膜特性及应用前景;陈朝泉;《塑料包装》;20-21 * |
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