CN112011159A - Preparation method of blend and blend - Google Patents
Preparation method of blend and blend Download PDFInfo
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- CN112011159A CN112011159A CN201910473402.6A CN201910473402A CN112011159A CN 112011159 A CN112011159 A CN 112011159A CN 201910473402 A CN201910473402 A CN 201910473402A CN 112011159 A CN112011159 A CN 112011159A
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- 239000000203 mixture Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 229920009537 polybutylene succinate adipate Polymers 0.000 claims abstract description 82
- UVCJGUGAGLDPAA-UHFFFAOYSA-N ensulizole Chemical group N1C2=CC(S(=O)(=O)O)=CC=C2N=C1C1=CC=CC=C1 UVCJGUGAGLDPAA-UHFFFAOYSA-N 0.000 claims abstract description 76
- 238000002156 mixing Methods 0.000 claims abstract description 50
- 239000004626 polylactic acid Substances 0.000 claims abstract description 39
- 239000004593 Epoxy Chemical group 0.000 claims abstract description 37
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 35
- 239000004970 Chain extender Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 27
- CKXDKAOBYWWYEK-UHFFFAOYSA-N 1,6-dioxecane-2,5-dione;hexanedioic acid Chemical compound OC(=O)CCCCC(O)=O.O=C1CCC(=O)OCCCCO1 CKXDKAOBYWWYEK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 claims description 15
- 239000000155 melt Substances 0.000 claims description 12
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 10
- 229920001897 terpolymer Polymers 0.000 claims description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 125000003700 epoxy group Chemical group 0.000 abstract description 5
- 229920002521 macromolecule Polymers 0.000 abstract description 5
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 229920005989 resin Polymers 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 12
- 238000000635 electron micrograph Methods 0.000 description 9
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- GMPCVWPKHFTZLH-UHFFFAOYSA-N butanedioic acid;1,6-dioxacyclododecane-7,12-dione Chemical compound OC(=O)CCC(O)=O.O=C1CCCCC(=O)OCCCCO1 GMPCVWPKHFTZLH-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 1
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- 229920006238 degradable plastic Polymers 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- -1 glycidyl ester Chemical class 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- 238000011056 performance test Methods 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001896 polybutyrate Polymers 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
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- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Biological Depolymerization Polymers (AREA)
Abstract
The invention provides a preparation method of a blend and the blend, wherein, firstly, poly adipic acid-butylene succinate PBSA and an epoxy chain extender are melt blended, so that the PBSA and the epoxy chain extender generate chain extension reaction, the epoxy chain extender and a multi-epoxy group thereof are introduced into a PBSA macromolecular chain to obtain epoxidized resin, and then the epoxidized PBSA and polylactic acid PLA are melt blended. The PLA/PBSA blend with the reaction compatibilization of the epoxy chain extender is obtained by a two-step blending method. In the two-step method, the epoxidized PBSA contains high-concentration epoxy groups, so that when the epoxidized PBSA is fused and blended with PLA, the epoxidized PBSA can react in situ at a PLA/PBSA two-phase interface to generate more PLA-epoxy chain extender-PBSA multi-block compatibilized macromolecules, the compatibilization effect of the blend is improved, and the impact toughness of the blend is further enhanced.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a preparation method of a blend and the blend.
Background
Plastics are high molecular compounds obtained by polyaddition or polycondensation polymerization of monomers, which are usually composed of synthetic resins and additives such as fillers, plasticizers, stabilizers, lubricants, colorants, etc. Most plastics have the characteristics of strong corrosion resistance, low manufacturing cost, water resistance and light weight, are good insulators, and are widely applied to production and life of people.
However, plastics are widely used, but are difficult to recycle, especially cannot be naturally degraded, so that a large amount of plastic wastes are accumulated, and the plastic wastes become one of important issues of environmental pollution in modern society. Therefore, the research of a new material which ensures the excellent performance of the existing plastic and can be well degraded becomes a hot spot of the current research.
Polylactic acid (PLA) has a wide application prospect as a biodegradable plastic with no pollution in the preparation process, and has excellent mechanical strength, optical property and biocompatibility, but the inherent brittleness and the lower heat resistance of the PLA limit the further application of the PLA material.
In the prior art, in order to improve the performance of a polylactic acid material and toughen and modify the polylactic acid material, a one-step blending method is often adopted, that is, PLA, Poly (butylene succinate-co-butylene succinate) and a multi-epoxy chain extender (ADR4370S) are mixed at the same time and put into a melt blending device for melt blending, but the blend obtained by the one-step blending method cannot fully react to generate enough PLA-ADR-PBSA compatibilized macromolecules, so that the compatibilized effect of the PLA/PBSA blend obtained by the one-step blending method needs to be improved, and the impact toughness of the PLA/PBSA blend is difficult to achieve the expected effect.
Disclosure of Invention
The invention aims to provide a preparation method of a blend and the blend, and aims to solve the problems that the compatibilization effect of a PLA/PBSA blend obtained by a one-step blending method in the prior art needs to be improved and the impact toughness is not enhanced sufficiently.
In order to solve the above problems, the present invention discloses a method for preparing a blend, which may comprise:
mixing poly adipic acid-butylene succinate PBSA with an epoxy chain extender according to a first preset proportion, and carrying out first melt blending to obtain epoxidized PBSA.
Mixing the epoxidized PBSA and polylactic acid (PLA) according to a second preset proportion, and carrying out second melt blending to obtain the blend.
Optionally, the first preset ratio includes a mass ratio of the PBSA to the epoxy chain extender being 40: 0.5-1.0.
Optionally, the second preset ratio includes a mass ratio of the PLA, the PBSA, and the epoxy chain extender is 60:40: 0.5-1.0.
Alternatively, the first melt blending has a melt temperature of 190 ℃, a rotational speed of 50 revolutions per minute, and a blending time of 15 minutes.
Optionally, the second melt blending has a melt temperature of 190 ℃, a rotational speed of 50 revolutions per minute, and a blending time of 10 minutes.
Optionally, before the step of mixing the poly (butylene adipate-succinate) PBSA with the epoxy chain extender in a first preset ratio and performing a first melt blending to obtain the epoxidized PBSA, the method further comprises:
the PLA and the PBSA were placed in a vacuum oven and dried at 50 ℃ for 5 hours.
Optionally, the epoxy chain extender is a terpolymer of styrene, methacrylic acid, and glycidyl acrylate.
The invention also discloses a blend prepared by the preparation method.
Compared with the prior art, the invention has the following advantages:
in the embodiment of the invention, the PBSA and the epoxy chain extender are firstly melt blended to obtain the epoxy chain extender reaction-compatibilized epoxidized PBSA, and then the epoxy chain extender reaction-compatibilized PBSA and the PLA are melt blended. In the two-step method, the epoxidized PBSA contains high-concentration epoxy groups, so that after PLA reaction, in-situ reaction can be carried out to generate more PLA-epoxy chain extender-PBSA compatibilized macromolecules, the compatibilization effect of the blend is improved, and the impact toughness of the blend is further enhanced.
Drawings
FIG. 1 is a flow chart of a method of making a blend according to an embodiment of the present invention;
FIG. 2 is an electron micrograph of a control 1 according to an embodiment of the present invention;
FIG. 3 is an electron micrograph of comparative example 2 of an embodiment of the present invention;
FIG. 4 is an electron micrograph of comparative example 3 according to an embodiment of the present invention;
FIG. 5 is an electron micrograph of sample 1 of an embodiment of the present invention;
FIG. 6 is an electron micrograph of sample 2 of an example of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Fig. 1 is a flow chart of a method for preparing a blend according to an embodiment of the present invention, and as shown in fig. 1, the method may include:
In the embodiment of the invention, firstly, the poly adipic acid-butylene succinate PBSA and the epoxy chain extender are mixed according to a preset proportion, and are melted and blended, so that the PBSA can be fully epoxidized to obtain the epoxidized PBSA.
Optionally, the first preset ratio includes a mass ratio of the PBSA to the epoxy chain extender being 40: 0.5-1.0.
In the embodiment of the present invention, when mixing the PBSA and the epoxy chain extender, they may be mixed in a mass ratio of 40:0.5-1.0, that is, 40 parts by mass of PBSA and 0.5-1.0 parts by mass of the epoxy chain extender are melt-blended, wherein the mass ratio may be 0.5, 0.6, 0.7, 0.8, 0.9 and 1.0 parts by mass of the epoxy chain extender, and each part by mass is the same.
Alternatively, the first melt blending has a melt temperature of 190 ℃, a rotational speed of 50 revolutions per minute, and a blending time of 15 minutes.
In the embodiment of the present invention, in order to sufficiently melt and blend the PBSA and the epoxy chain extender to obtain the epoxidized PBSA better, the melt temperature of 190 ℃ and the rotation speed of 50 rpm are selected, and the blending is performed for 15 minutes, and a person skilled in the art selects an appropriate melt temperature, rotation speed and blending time according to actual materials and material ratios, which is not specifically limited in the present invention.
Step 102: mixing the epoxidized PBSA and polylactic acid (PLA) according to a second preset proportion, and carrying out second melt blending to obtain the blend.
In the embodiment of the invention, the PBSA and the epoxy chain extender are melt blended to obtain the epoxidized PBSA, and then the epoxidized PBSA and the PLA are mixed according to a second preset proportion and melt blended, so that the full reaction of the epoxidized PBSA and the PLA can be ensured, more PLA-epoxy chain extender-PBSA compatibilized macromolecules can be obtained, the compatibilization effect of the blend on the PLA can be effectively improved, and the impact toughness of the material can be further improved.
Optionally, the second preset ratio includes a mass ratio of the PLA, the PBSA, and the epoxy chain extender is 60:40: 0.5-1.0.
In the embodiment of the present invention, in the second melt blending of PLA and epoxidized PBSA, the mixing may be performed in a mass ratio of 60:40:0.5-1.0, that is, in the mixing of epoxidized PBSA and PLA, 60 parts by mass of PLA, each of which is the same, is added.
Optionally, the second melt blending has a melt temperature of 190 ℃, a rotational speed of 50 revolutions per minute, and a blending time of 10 minutes.
In the embodiment of the present invention, in order to sufficiently melt and blend PLA and epoxidized PBSA to obtain PLA-epoxy chain extender-PBSA, a melt temperature of 190 ℃ and a rotation speed of 50 rpm are selected, and blending is performed for 10 minutes, and a person skilled in the art selects an appropriate melt temperature, rotation speed and blending time according to actual materials and material ratios, which is not specifically limited in the present invention.
Optionally, before step 101, the method may further include:
the PLA and the PBSA were placed in a vacuum oven and dried at 50 ℃ for 5 hours.
In the embodiment of the invention, the PLA and the PBSA may be dried before melt blending, or alternatively, the PLA and the PBSA may be placed in a vacuum oven and dried at 50 ℃ for 5 hours, so as to sufficiently remove moisture in the raw materials, thereby preventing the problem of material hydrolysis during the processing process and affecting the preparation effect.
Optionally, the epoxy chain extender is a terpolymer of styrene, methacrylic acid, and glycidyl acrylate.
In the embodiment of the present invention, a conventional epoxy chain extender, such as a terpolymer ADR4370S of styrene, methacrylic acid and glycidyl acrylate, or other chain extenders with an epoxy group, may be selected, and a person skilled in the art may select a suitable chain extender according to actual situations, which is not specifically limited in the present invention.
The embodiment of the invention also provides a blend prepared by the preparation method.
To better illustrate the effects of the present invention, the following description is given with reference to specific examples and characterization data:
raw materials are selected:
polylactic acid (PLA 4032D), NatureWork, usa;
poly (butylene adipate-succinate) (PBSA 3001MD), japan showa;
an epoxy chain extender ADR4370S (terpolymer of styrene, methacrylic acid and glycidyl ester, hereinafter abbreviated as ADR) having a plurality of epoxy groups in the main chain and an epoxy value of 285g/mol, BASF (Badisco oil-und-Soda-Fabrik) Co., Ltd., molecular weight 6800.
And (3) drying: placing PLA and PBSA in a vacuum oven, drying for 5 hours at 50 ℃, and taking out for later use.
Preparation of control: weighing PLA and PBSA in a mass ratio of 60:40 three times, wherein the sum of the parts by mass of the PLA and the parts by mass of the PBSA is 100 parts each time, setting the addition gradient of ADR, adding 0 part, 0.5 part and 1.0 part of the ADR into the three parts of the weighed PLA and PBSA respectively, mixing, and performing one-step melt blending (50 revolutions per minute at 190 ℃ for 15 minutes) respectively to obtain a reference substance 1, a reference substance 2 and a reference substance 3.
Preparation of a sample: PLA and PBSA are weighed twice according to the mass ratio of 60:40, the sum of the parts by mass of PLA and the parts by mass of PBSA is 100 parts for each time, and the addition gradient of ADR is set to be 0.5 part and 1.0 part respectively.
40 parts of PBSA were melt-blended with 0.5 parts and 1.0 part of ADR in an internal mixer at a melt temperature of 190 ℃ and a rotational speed of 50 revolutions per minute for 15 minutes to give epoxidized PBSA resins, i.e., PBSA-ADR1(40:0.5) and PBSA-ADR2(40: 1.0).
PBSA-ADR1(40:0.5) and PBSA-ADR2(40:1.0) were melt-blended with 60 parts of PLA, respectively, in an internal mixer at a melt temperature of 190 ℃ at a rotational speed of 50 rpm for 10 minutes to obtain samples 1 and 2.
Processing the components in an internal mixer for a period of time according to the mixture ratio and the melt blending condition, taking the obtained melt blend out of the internal mixer, and naturally cooling at room temperature to obtain a blank.
Preparation of the sample strips: pressing the blank in a hot press at 210 ℃ and 15MPa, wherein the thickness of a die is 4mm, the pressure and heat preservation time is 8min, and exhausting twice in the midway to remove bubbles in the sample. And (3) after 8min, quickly transferring the die from the hot press to another cold press, carrying out pressure maintaining water cooling to room temperature under 15MPa, opening the die to obtain a quenched plate with the thickness of 4mm, cutting the plate into quenched sample strips with the width of 10mm and the length of 80mm by a cutting machine, and carrying out notch treatment on the sample strips, wherein the notch depth is 2 mm.
And (5) numbering the sample strips and testing.
Testing and characterization
And (3) impact performance test:
and (4) carrying out notch impact strength test on the sample strip by using a cantilever beam impact tester, selecting at least 6 effective numerical values, and calculating the notch impact strength.
TABLE 1 notched Izod impact Strength comparison of quenched specimens
As can be seen from the data in Table 1, the impact strength of pure PLA is only 5.59kJ/m2, showing extreme brittleness. When the PBSA component was added, the notched impact strength of the control 1 specimen was only slightly increased (7.15 kJ/m)2). When 0.5 to 1.0 part of ADR was added, the impact strength of control 2 and control 3 was rapidly increased to 34.64kJ/m2And 34.34kJ/m2. However, after the preparation method provided by the embodiment of the invention is adopted, under the condition that ADR with the same quality is added, the impact strength of the sample 1 and the sample 2 prepared by the embodiment of the invention is improved more obviously, which shows that the preparation method of the embodiment of the invention has better compatibilization effect and larger impact toughness reinforcing amplitude.
Scanning Electron Microscope (SEM) testing:
and observing the micro-morphology of each sample strip quenching section by using a scanning electron microscope. The quenched sample strip is obtained by quenching a sample after soaking in liquid nitrogen for 3 minutes, and before observing the section of the sample strip, metal spraying treatment is carried out to enhance the conductivity of an interface and improve the definition, wherein the magnification is 3000 times, and the appearance of the sample is shot.
Fig. 2 is an electron microscope photograph of the comparison product 1, and it can be seen from fig. 2 that the microstructure thereof is a typical "sea-island" like structure, i.e. the PBSA dispersed phase is dispersed in the PLA matrix in granular form. Meanwhile, due to poor compatibility of PBSA and PLA, the dispersed phase of PBSA has large phase separation phenomenon, so that the particle size of the dispersed phase is large and the particle size is distributed in the range of (3-15 μm). In addition, due to poor compatibility between PLA and PBSA, the adhesion force of the two-phase interface is weak, so that the PBSA particles are obviously debonded from the PLA matrix, and the impact toughness is poor.
FIG. 3 is an electron micrograph of a comparison product 2, FIG. 4 is an electron micrograph of a comparison product 3, and as shown in FIGS. 3 and 4, due to the addition of ADR4370S, the generated terpolymer PLA-ADR-PBAT plays a role in interfacial compatibilization, the interfacial tension of PLA and PBSA is reduced, and a co-continuous phase micro-phase structure is shown, which is very different from the "sea-island" micro-phase structure of a PLA/PBSA (60:40) binary blend. Numerous studies have shown that blends of co-continuous phase structures are significantly superior to "sea-island structures" in mechanical properties.
Fig. 5 is an electron micrograph of sample 1, fig. 6 is an electron micrograph of sample 2, and it is clear from fig. 5 and 6 that the two-step method sample likewise has a co-continuous phase structure. However, compared with the one-step method, the morphological structure of the co-continuous phase of the two-step method blending material is more refined, and the interfacial de-bonding phenomenon of the co-continuous phase is better inhibited and the phase interface becomes very fuzzy due to good interfacial compatibilization effect and large interfacial adhesion.
In the embodiment of the invention, the toughness enhancement effect on PLA modification is more excellent, so that the application performance and the application range of the PLA modified material in the fields of products such as packaging, films and the like are wider, and the application field of degradable plastics is further expanded.
According to the content, in the embodiment of the invention, the epoxidized PBSA is obtained by firstly carrying out melt blending and chain extension reaction on the PBSA and the epoxy chain extender, and then carrying out melt blending on the epoxidized PBSA and the PLA, because the epoxidized PBSA contains high-concentration epoxy groups in the two-step method, the epoxidized PBSA can react in situ with the PLA to generate more PLA-epoxy chain extender-PBSA compatibilized macromolecules, the compatibilization effect of the blend is improved, and the impact toughness of the blend is further enhanced.
For simplicity of description, the method embodiments are described as a series of operational combinations, but those skilled in the art will recognize that the invention is not limited by the order of operation, as some steps may occur in other orders or concurrently in accordance with the invention. Further, those skilled in the art will also appreciate that the embodiments described in the specification are presently preferred and that no requirement is necessarily placed on the invention for the exact operation and experimental conditions involved.
The blend and the preparation method of the blend provided by the invention are described in detail above, and the principle and the implementation mode of the invention are explained in the present document by applying specific examples, and the description of the above examples is only used for helping to understand the method of the invention and the core idea thereof; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (8)
1. A method of making a blend, the method comprising:
mixing poly adipic acid-butylene succinate PBSA with an epoxy chain extender according to a first preset proportion, and carrying out first melt blending to obtain epoxidized PBSA;
mixing the epoxidized PBSA and polylactic acid (PLA) according to a second preset proportion, and carrying out second melt blending to obtain the blend.
2. The method of claim 1, wherein the first predetermined ratio comprises a mass ratio of the PBSA to the epoxy chain extender of 40:0.5-1.
3. The method according to claim 1, wherein the second preset ratio comprises a mass ratio of the PLA, the PBSA and the epoxy chain extender of 60:40:0.5-1.
4. The method of claim 1, wherein the first melt blending has a melt temperature of 190 ℃, a rotational speed of 50 revolutions per minute, and a blending time of 15 minutes.
5. The method of claim 1, wherein the second melt blending has a melt temperature of 190 ℃, a rotational speed of 50 revolutions per minute, and a blending time of 10 minutes.
6. The method of claim 1, wherein prior to the step of mixing the PBSA with the chain extender epoxy in a first predetermined ratio and first melt blending to obtain the epoxidized PBSA, the method further comprises:
the PLA and the PBSA were placed in a vacuum oven and dried at 50 ℃ for 5 hours.
7. The method of claim 1, wherein the epoxy chain extender is a terpolymer of styrene, methacrylic acid, and glycidyl acrylate.
8. A blend produced by the production method according to any one of claims 1 to 7.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114605800A (en) * | 2022-03-28 | 2022-06-10 | 海南大学 | PLA/PGA/(PBAT/ADR) blended alloy and preparation method thereof |
| IT202200002468A1 (en) * | 2022-02-10 | 2023-08-10 | Novamont Spa | POLYMER COMPOSITION FOR HIGH DISINTEGRABILITY FILM IN THE MARINE ENVIRONMENT |
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