CN112063137A - Biodegradable blending material for improving crystallinity of polylactic acid and preparation method thereof - Google Patents
Biodegradable blending material for improving crystallinity of polylactic acid and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 52
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 48
- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 47
- 238000002156 mixing Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000379 polypropylene carbonate Polymers 0.000 claims abstract description 52
- -1 polypropylene carbonate Polymers 0.000 claims abstract description 37
- 239000002981 blocking agent Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 12
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 10
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 10
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 abstract description 5
- 230000008025 crystallization Effects 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 5
- 238000013508 migration Methods 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 238000006065 biodegradation reaction Methods 0.000 abstract 1
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 3
- 229910052901 montmorillonite Inorganic materials 0.000 description 3
- 229920001896 polybutyrate Polymers 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229920006126 semicrystalline polymer Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
A biodegradable blending material for improving the crystallinity of polylactic acid and a preparation method thereof relate to a biodegradable blending material and a preparation method thereof, and the blending material comprises the following raw materials: 60-90 parts of polylactic acid; 10-40 parts of polypropylene carbonate; 1-5 parts of a blocking agent; 5 parts of a compatibilizer. The preparation step 1: and (3) carrying out end capping treatment on the end capping agent and the polypropylene carbonate in a double-screw extruder. Step 2: and (3) blending the polylactic acid, the polypropylene carbonate obtained in the step (1) and the compatibilizer in a double-screw extruder to obtain the PLA/PPC blended material with high crystallinity. The blending material has better compatibility, avoids the problem of matrix migration caused by poor compatibility, has higher crystallinity compared with a single polylactic acid material, and improves the processing and forming performance of polylactic acid. The preparation method effectively improves the crystallization capacity of the polylactic acid, simultaneously reserves the characteristic of complete biodegradation, and has wide application prospect.
Description
Technical Field
The invention relates to a biodegradable blending material and a preparation method thereof, in particular to a biodegradable blending material for improving the crystallinity of polylactic acid and a preparation method thereof.
Background
Polylactic acid (PLA) is a nontoxic, completely biodegradable and renewable semi-crystalline polymer and is widely applied to the fields of biomedicine, textile, packaging and the like. However, PLA has a slow crystallization rate, a low crystallinity, poor impact resistance and poor elongation at break, which limits its further popularization and application.
PPC has the advantages of high elongation at break and good flexibility, and propylene oxide and greenhouse gas CO are adopted during synthesis2Is a raw material, and relieves the problems of greenhouse effect and white pollution. For this reason, a method of blending PPC with PLA may be employed to improve the crystallization ability and toughness of PLA. However, because the PPC and the PLA are partially compatible, the poor compatibility can obviously reduce the overall mechanical property of the material, so that the improvement of the crystallization capacity of the PLA and the guarantee of the better compatibility are very necessary for modifying the PLA material.
The invention patent application of patent publication No. CN 101724250A discloses a preparation method of blend of PPC, PBAT, PLA and PBS, the property of PPC is improved by adding PBAT, PLA and PBS, the blend takes PPC as main matrix, the addition amount of PBAT, PLA and PBS is 5% -50%, but no compatibilizer is used in the preparation process, and the blend is easy to phase separate.
Patent application publication No. CN 108359230A discloses a method for preparing degradable PLA/PPC film, which improves the mechanical property of the blend by adding montmorillonite, but improves the compatibility of montmorillonite and matrix material by polycaprolactone due to poor compatibility of montmorillonite and polymer, but does not add compatibilizer to improve the compatibility of two matrixes.
In contrast, the compatibilizer is used for improving the compatibility of the two materials, so that the matrix migration problem caused by incompatibility can not occur in the use process of the composite material, and the service life of the blending material is greatly prolonged. Meanwhile, the end capping agent is used for carrying out end capping treatment on the poly (propylene carbonate), so that the poly (propylene carbonate) is prevented from being thermally decomposed in the processing process.
The patent application for invention of patent publication No. CN 108707323A discloses a preparation method of PLA/PPC/HBP derivative blend, which uses HBP hyperbranched copolymer to increase the compatibility of two materials of PLA and PPC, but has complex operation process and higher cost.
Compared with the prior art, the invention adopts the micromolecule auxiliary agents tetrabutyl titanate and 2, 4-toluene diisocyanate as the compatibilizer, so that the cost is lower, the operation steps are simple, and the micromolecule auxiliary agents are easier to obtain.
Disclosure of Invention
The invention aims to provide a biodegradable blending material for improving the crystallinity of polylactic acid and a preparation method thereof, tetrabutyl titanate and 2, 4-toluene diisocyanate are used as a compatibilizer, after the compatibilizer is added into a PLA/PPC blending system, the hydroxyl at the end of PPC and the 4-cyanate group in TDI are dehydro-condensed, the hydroxyl at the upper end of PLA and the 2-cyanate group in TDI are dehydro-condensed, and simultaneously, the isocyanate can accelerate the ester exchange reaction rate, so that two molecular chains are chain-extended into one chain, the compatibility of PPC and PLA and the regularity of the molecular chains are improved, and the crystallinity of the material is obviously improved.
The purpose of the invention is realized by the following technical scheme:
a biodegradable blending material for improving the crystallinity of polylactic acid comprises the following raw materials:
60-90 parts of polylactic acid;
10-40 parts of polypropylene carbonate;
1-5 parts of a blocking agent;
1-5 parts of a compatibilizer.
The biodegradable blending material for improving the crystallinity of the polylactic acid is characterized in that the end-capping agent is one or more of maleic anhydride or dicumyl peroxide.
The biodegradable blending material for improving the crystallinity of the polylactic acid is characterized in that the compatibilizer is one or more of tetrabutyl titanate or 2, 4-toluene diisocyanate.
A preparation method of a biodegradable blending material for improving the crystallinity of polylactic acid comprises the following preparation processes:
(1) drying the polypropylene carbonate, uniformly mixing the dried polypropylene carbonate with a blocking agent, adding the mixture into a double-screw extruder, setting the heating temperature of the double-screw extruder at 130-150 ℃, setting the rotating speed of the double-screw extruder at 40-60 r/min, taking materials, and drying for later use;
(2) uniformly mixing the material obtained in the step (1), the dried polylactic acid and the compatibilizer, and adding the mixture into a double-screw extruder, wherein the heating temperature of the double-screw extruder is 160-200 ℃, and the rotating speed of the double-screw extruder is 40-60 r/min.
The invention has the advantages and effects that:
the two raw materials are all biodegradable materials, so that the problem of white pollution can be reduced. The addition of the micromolecular compatibilizer ensures that the compatibility of the two materials is better, the problem of matrix migration is avoided, the problems of low crystallinity and low crystallization speed of the polylactic acid are solved, and the crystallinity of the blend is successfully over 20 percent.
The product produced by the invention has low cost and simple process, is a green and environment-friendly industry, and widens the application range of the polylactic acid composite material in the industry.
Drawings
Fig. 1 and 2 are comparative images of the crystallinity enhancement of the thermal performance test in the examples of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples.
The degree of crystallinity is first measured by DSC to reflect the compatibility of the blend and the invention is described in detail below with reference to the examples.
Comparative example:
60 parts of polylactic acid
40 parts of polypropylene carbonate
Maleic anhydride 1 part
The specific implementation steps are as follows:
(1) drying the polypropylene carbonate, then uniformly mixing the dried polypropylene carbonate with maleic anhydride, adding the mixture into a double-screw extruder, setting the heating temperature to be 125 ℃ and the rotating speed to be 45 r/min, taking materials, and drying for later use;
(2) and (2) uniformly mixing the polypropylene carbonate weighed in the step (1) with the dried polylactic acid, adding the mixture into a double-screw extruder, setting the heating temperature at 180 ℃ and the rotating speed at 50 revolutions per minute, and taking the material.
The material was subjected to DSC thermal performance testing with the following results:
the crystallinity was 3.9%.
Example 1:
60 parts of polylactic acid
40 parts of polypropylene carbonate
Maleic anhydride 1 part
Tetrabutyl titanate 1 part
The specific implementation steps are as follows:
(1) drying the polypropylene carbonate, then uniformly mixing the dried polypropylene carbonate with maleic anhydride, adding the mixture into a double-screw extruder, setting the heating temperature to be 130 ℃, setting the rotating speed to be 50 r/min, taking materials, and drying for later use;
(2) and (2) uniformly mixing the polypropylene carbonate weighed in the step (1) with the dried polylactic acid and tetrabutyl titanate, adding the mixture into a double-screw extruder, setting the heating temperature to be 180 ℃ and the rotating speed to be 45 revolutions per minute, and taking materials.
The material was subjected to DSC thermal performance testing with the following results:
the crystallinity is 8.19%
Example 2:
70 portions of polylactic acid
30 parts of polypropylene carbonate
Maleic anhydride 1 part
Tetrabutyl titanate 2 parts
The specific implementation steps are as follows:
(1) drying the polypropylene carbonate, then uniformly mixing the dried polypropylene carbonate with maleic anhydride, adding the mixture into a double-screw extruder, setting the heating temperature to be 135 ℃ and the rotating speed to be 55 r/min, taking materials, and drying for later use;
(2) and (2) uniformly mixing the polypropylene carbonate weighed in the step (1) with the dried polylactic acid and tetrabutyl titanate, adding the mixture into a double-screw extruder, setting the heating temperature to be 180 ℃ and the rotating speed to be 50 revolutions per minute, and taking materials.
The material was subjected to DSC thermal performance testing with the following results:
the crystallinity is 20.04%
Example 3:
70 portions of polylactic acid
30 parts of polypropylene carbonate
Dicumyl peroxide 2 parts
Tetrabutyl titanate 3 parts
The specific implementation steps are as follows:
(1) drying the polypropylene carbonate, then uniformly mixing the dried polypropylene carbonate with dicumyl peroxide, adding the mixture into a double-screw extruder, setting the heating temperature to be 130 ℃ and the rotating speed to be 55 r/min, taking materials, and drying for later use;
(2) and (2) uniformly mixing the polypropylene carbonate weighed in the step (1), the dried polylactic acid and tetrabutyl titanate, adding into a double-screw extruder, setting the heating temperature to be 175 ℃, and taking materials at the rotating speed of 50 revolutions per minute.
The material was subjected to DSC thermal performance testing with the following results:
the crystallinity is 19.64%
Example 4:
80 parts of polylactic acid
20 parts of polypropylene carbonate
Maleic anhydride 3 parts
1 part of 2, 4-toluene diisocyanate
The specific implementation steps are as follows:
(1) drying the polypropylene carbonate, then uniformly mixing the dried polypropylene carbonate with maleic anhydride, adding the mixture into a double-screw extruder, setting the heating temperature to be 130 ℃, setting the rotating speed to be 50 r/min, taking materials, and drying for later use;
(2) uniformly mixing the polypropylene carbonate weighed in the step (1), the dried polylactic acid and the dried 2, 4-toluene diisocyanate, adding the mixture into a double-screw extruder, setting the heating temperature to be 180 ℃ and the rotating speed to be 45 revolutions per minute, and taking materials.
The material was subjected to DSC thermal performance testing with the following results:
the crystallinity is 13.20%
Example 5:
70 portions of polylactic acid
30 parts of polypropylene carbonate
Dicumyl peroxide 2 parts
2 parts of 2, 4-toluene diisocyanate
The specific implementation steps are as follows:
(1) drying the polypropylene carbonate, then uniformly mixing the dried polypropylene carbonate with dicumyl peroxide, adding the mixture into a double-screw extruder, setting the heating temperature to be 130 ℃, setting the rotating speed to be 50 r/min, taking materials, and drying for later use;
(2) uniformly mixing the polypropylene carbonate weighed in the step (1), the dried polylactic acid and the dried 2, 4-toluene diisocyanate, adding the mixture into a double-screw extruder, setting the heating temperature to be 180 ℃ and the rotating speed to be 45 revolutions per minute, and taking materials.
The material was subjected to DSC thermal performance testing with the following results:
degree of crystallinity 21.00%
Example 6:
90 parts of polylactic acid
10 parts of polypropylene carbonate
Maleic anhydride 1 part
3 parts of 2, 4-toluene diisocyanate
The specific implementation steps are as follows:
(1) drying the polypropylene carbonate, then uniformly mixing the dried polypropylene carbonate with maleic anhydride, adding the mixture into a double-screw extruder, setting the heating temperature to be 130 ℃, setting the rotating speed to be 50 r/min, taking materials, and drying for later use;
(2) uniformly mixing the polypropylene carbonate weighed in the step (1), the dried polylactic acid and the dried 2, 4-toluene diisocyanate, adding the mixture into a double-screw extruder, setting the heating temperature to be 180 ℃ and the rotating speed to be 45 revolutions per minute, and taking materials.
The material was subjected to DSC thermal performance testing with the following results:
the crystallinity was 13.50%.
Degree of crystallinity
The crystallinity in the specific embodiment is obviously improved through the table data and the pictures.
Claims (4)
1. The biodegradable blending material for improving the crystallinity of the polylactic acid is characterized by comprising the following raw materials:
60-90 parts of polylactic acid;
10-40 parts of polypropylene carbonate;
1-5 parts of a blocking agent;
1-5 parts of a compatibilizer.
2. The biodegradable blending material for improving the crystallinity of the polylactic acid according to claim 1, wherein the end-capping agent is one or more of maleic anhydride or dicumyl peroxide.
3. The biodegradable blending material for improving the crystallinity of the polylactic acid as claimed in claim 1, wherein the compatibilizer is one or more of tetrabutyl titanate or 2, 4-toluene diisocyanate.
4. A preparation method of a biodegradable blending material for improving the crystallinity of polylactic acid is characterized by comprising the following preparation processes:
(1) drying the polypropylene carbonate, uniformly mixing the dried polypropylene carbonate with a blocking agent, adding the mixture into a double-screw extruder, setting the heating temperature of the double-screw extruder at 130-150 ℃, setting the rotating speed of the double-screw extruder at 40-60 r/min, taking materials, and drying for later use;
(2) uniformly mixing the material obtained in the step (1), the dried polylactic acid and the compatibilizer, and adding the mixture into a double-screw extruder, wherein the heating temperature of the double-screw extruder is 160-200 ℃, and the rotating speed of the double-screw extruder is 40-60 r/min.
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Cited By (4)
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| CN112920583A (en) * | 2021-04-14 | 2021-06-08 | 中国科学院长春应用化学研究所 | Poly-L-lactic acid foaming material with rapid crystallization capacity and preparation method thereof |
| CN113402868A (en) * | 2021-07-12 | 2021-09-17 | 北京化工大学常州先进材料研究院 | Preparation method of hyperbranched polyester modified polylactic acid/polypropylene carbonate composite material |
| CN113943406A (en) * | 2021-05-08 | 2022-01-18 | 天津科技大学 | Preparation method of intelligent temperature-control reversible light-transmitting material |
| WO2023104073A1 (en) * | 2021-12-08 | 2023-06-15 | 山东联欣环保科技有限公司 | Degradable composite polymer having high ductility, and preparation method therefor |
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Cited By (5)
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| CN112920583A (en) * | 2021-04-14 | 2021-06-08 | 中国科学院长春应用化学研究所 | Poly-L-lactic acid foaming material with rapid crystallization capacity and preparation method thereof |
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| CN113943406A (en) * | 2021-05-08 | 2022-01-18 | 天津科技大学 | Preparation method of intelligent temperature-control reversible light-transmitting material |
| CN113402868A (en) * | 2021-07-12 | 2021-09-17 | 北京化工大学常州先进材料研究院 | Preparation method of hyperbranched polyester modified polylactic acid/polypropylene carbonate composite material |
| WO2023104073A1 (en) * | 2021-12-08 | 2023-06-15 | 山东联欣环保科技有限公司 | Degradable composite polymer having high ductility, and preparation method therefor |
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