CN115785631A - Biodegradable polylactic acid toughening and reinforcing material for injection molding and injection molding product based on biodegradable polylactic acid toughening and reinforcing material - Google Patents
Biodegradable polylactic acid toughening and reinforcing material for injection molding and injection molding product based on biodegradable polylactic acid toughening and reinforcing material Download PDFInfo
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- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 7
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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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- Biological Depolymerization Polymers (AREA)
Abstract
The invention discloses a biodegradable polylactic acid toughening and reinforcing material for injection molding and an injection molding product based on the biodegradable polylactic acid toughening and reinforcing material. According to the formula of the biodegradable polylactic acid toughening and reinforcing material provided by the invention, carboxyl in maleic anhydride reacts with hydroxyl in cellulose under a high-temperature condition, and the cellulose is connected to a maleic anhydride molecular chain in a chemical bond form, so that the problem of high-temperature shearing carbonization of the cellulose can be effectively solved, the occurrence of black spots of a degradation modified material and the reduction of degradation rate can be effectively avoided, the tensile strength and toughness of a PLA blend are permanently improved, the material is endowed with lasting flexibility, and the service life and safety of a PLA product are improved.
Description
Technical Field
The invention relates to the field of preparation of biodegradable materials, in particular to a biodegradable polylactic acid toughening and reinforcing material for injection molding and a biodegradable injection molding product prepared from the biodegradable polylactic acid toughening and reinforcing material.
Background
Most of the children toys on the market at present are made of plastics, and once the toys are discarded, the plastics are difficult to degrade and can damage the environment. China owns 8000 more toy manufacturers, most of which mainly use plastic toys, and the annual output value is 500 million yuan. Nearly 75% of the toys in the world are manufactured by Chinese manufacturers, and products are sold in a plurality of countries and regions such as Europe, america, japan and the like, wherein the export of America accounts for more than 60% of the total export. Guangdong is the province with the most export of toys in China, the export accounts for more than 60% of the whole country, and the Guangdong production base is mainly in Shenzhen, dongguan and coastal areas. The polylactic acid is derived from corn plants and can be biodegraded, the playing space of the biodegradable PLA is larger, and the market prospect of the biodegradable plastic is wide in the future along with policy promotion and cost reduction.
Polylactic acid resin (PLA) itself is brittle, however, leading to the need for toughening with elastomers in injection molding systems or blending with PBAT, PBS, PPC and PLA to improve PLA brittleness problems. The petroleum-based elastomer toughening can reduce the degradation rate of a blending system, has poor compatibility with PLA and reduces the modulus and the rigidity. The degradable polyester such as PBAT is one of the common systems for PLA blending in the prior art, but PLA/PBAT physical blending is an incompatible two-phase system, and the tensile strength of PLA is reduced due to excessively high PBAT addition, so that the incompatibility problem is solved by adopting an epoxy chain extender to carry out system chain extension, but most of the epoxy chain extender has an excessive styrene content, so that the prepared plastic product does not meet the food safety contact standard. PBS, PPC, PBAT incorporation also causes PLA to lose transparency and gloss, limiting its application in transparent and high strength articles. In addition, PBS and PBAT are added into PLA to cause serious precipitation of small molecules, and the food safety contact standard is not met. At present, researchers research that in-situ copolymerization is adopted to modify PLA, a molecular chain is used for grafting a soft monomer to achieve a toughening effect, the brittleness of the PLA is improved, but the operation is complex, and the cost is increased. The systems with different processing requirements vary greatly, and different melt greases require different amounts for each copolymer, which leads to increased costs. The introduction of PBAT and PBS into PLA also necessitates a reduction in the amount of carboxyl groups in PBAT and PBS, since carboxyl groups are easily hydrolyzed leading to a reduction in the shelf life of the product.
Disclosure of Invention
Based on the problems in the prior art, the invention provides a biodegradable polylactic acid toughening and reinforcing material for injection molding, which is prepared by adding PLA coated grafted cellulose serving as a toughening and reinforcing modifier into polylactic acid resin (PLA) to reinforce, toughen and modify the PLA so as to obtain lasting flexibility.
The invention adopts the following technical scheme for realizing the purpose:
the invention firstly provides a biodegradable polylactic acid toughening and reinforcing material for injection molding, which comprises the following raw materials in parts by weight: 87.5 to 94.8 parts of PLA resin, 5 to 10 parts of PLA coated grafted cellulose, 0.1 to 2 parts of lubricant and 0.1 to 0.5 part of antioxidant.
Further, the preparation method of the PLA-coated grafted cellulose used as the modifier comprises the following steps:
s1, firstly, pouring the nano-cellulose CNF into a high-speed mixer, then adding maleic anhydride, and uniformly stirring at the speed of 300-500 r/min for 15-20 min at normal temperature to uniformly disperse the maleic anhydride; adding dicumyl peroxide into the high-speed mixer, and uniformly stirring at the speed of 300-500 r/min for 3-6 min at normal temperature to obtain a mixture A;
s2, adding PLA resin, zinc stearate, an antioxidant 1010 and an antioxidant 168 into the mixture A, and uniformly stirring at the speed of 300-500 r/min for 3-6 min at normal temperature to obtain a mixture B;
and S3, extruding and granulating the mixture B through a double-screw extruder, wherein the temperature of the extruder is 120-195 ℃, the rotating speed of the extruder is 300-350 rpm, granulating to obtain particles, and drying for 4-6 hours at 55-60 ℃ to obtain the PLA coated grafted cellulose.
Further, in the preparation method of the PLA-coated grafted cellulose: the addition amount of maleic anhydride is 3-5 wt% of the mass of the nano-cellulose, the addition amount of dicumyl peroxide is 0.5-2 wt% of the mass of the nano-cellulose, the addition amount of the nano-cellulose is 20-50 wt% of the mass of PLA, the addition amount of zinc stearate is 0.2-1 wt% of the mass of the PLA, the mass ratio of the antioxidant 1010 to the antioxidant 168 is 1:1, and the total addition amount of the antioxidant 1010 and the antioxidant 168 is 0.2-0.5 wt% of the mass of the PLA.
Further, the PLA resin is injection molding grade, and the melt index is 20-25 g/10min (190 ℃,2.16 kg).
Most preferably, the biodegradable polylactic acid toughening and reinforcing material comprises the following raw materials in parts by weight: 91.6 parts of PLA resin, 8 parts of PLA coated grafted cellulose, 0.1 part of antioxidant 1010,0.1 part of antioxidant 168 and 0.2 part of lubricant stearic acid.
The biodegradable polylactic acid toughening and reinforcing material for injection molding can be processed into required injection molding products by the following method: weighing the raw materials according to the proportion, adding the raw materials into a high-speed mixer for full mixing, sending the obtained mixture into a double-screw extruder for extrusion granulation, then sending the mixture into a dryer for repeated drying, and then sending the mixture into an injection molding machine for injection molding to obtain a biodegradable injection molding product with a certain thickness.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a formula of a biodegradable polylactic acid toughening and reinforcing material for injection molding, which is characterized in that PLA serving as a compatible modifier is added into polylactic acid resin (PLA) to coat grafted cellulose. The invention utilizes the reaction of carboxyl in maleic anhydride and hydroxyl in cellulose under the high temperature condition to connect the cellulose to a maleic anhydride molecular chain in a chemical bond form, can effectively improve the problem of high-temperature shearing carbonization of the cellulose, and effectively avoids the occurrence of black spots of degradation modified materials and the reduction of degradation rate.
2. The modified cellulose used in the invention is a non-toxic and harmless environment-friendly graft. The cellulose is a biodegradable substance, so that the environment is more environment-friendly, and the prepared product can be contacted with food. Through the extrusion reaction, toxic solvents are not introduced, the product has no residues of dimethylbenzene, methylbenzene, heavy metals and the like, and the use of various coupling agents, oily dispersing agents, surfactants and other chemical additives which cannot be in contact with food and modifiers containing metal components is avoided.
3. The biodegradable polylactic acid toughening and reinforcing material for injection molding can be widely applied to the fields of toys, tools, cups, packaging boxes and the like.
4. The biodegradable polylactic acid toughening and reinforcing material for injection molding is green and environment-friendly, has low cost, is expected to be produced industrially, and brings great economic and social benefits when being popularized and applied.
5. According to the invention, PLA coated grafted cellulose is added into PLA to be compared with pure nano cellulose, so that the tensile strength of the obtained PLA injection molding product is improved by 28%, and the bending strength is improved by 17.1%.
Drawings
Fig. 1 is an SEM picture of a nano-cellulose CNF feedstock used in example 1 of the present invention.
FIG. 2 is an SEM picture of PLA-coated grafted cellulose obtained in example 1 of the present invention.
FIG. 3 is a microscopic SEM image of a cross-section of a sample injection molded using the inventive comparative example 1 injection molding compound.
FIG. 4 is a microscopic SEM image of a cross-section of a sample injection molded using the injection molding compound of example 2 of the present invention.
Detailed Description
The present invention is described in detail below by way of examples, and it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
The polylactic acid resin used in the following examples is Anhui Feng Yuanfu Telelactic acid, inc. (FY 201).
Example 1
This example prepared PLA-coated grafted cellulose as a modifier for the subsequent examples as follows:
s1, pouring 10kg of nano cellulose CNF (10-50 nm wide and 0.5-3 microns long) (the SEM image is shown in figure 1) into a high-speed mixer, adding 0.3kg of maleic anhydride, and uniformly stirring at the normal temperature at the speed of 500r/min for 15min to uniformly disperse the maleic anhydride; then 0.1kg dicumyl peroxide is added into the high-speed mixer, and the mixture is evenly stirred for 3min at the normal temperature at the speed of 500r/min, thus obtaining a mixture A.
S2, adding 34kg of PLA resin, 0.1kg of zinc stearate, 0.05kg of antioxidant 1010 and 0.05kg of antioxidant 168 into the mixture A, and uniformly stirring at the normal temperature at the speed of 500r/min for 3min to obtain a mixture B.
And S3, extruding and granulating the mixture B through a double-screw extruder, wherein the temperature of the extruder is 120-195 ℃, the rotating speed of the extruder is 350rpm, drying the obtained particles for 4 hours at 60 ℃, and obtaining the PLA coated grafted cellulose, wherein an SEM picture of the PLA coated grafted cellulose is shown in figure 2.
Example 2
The biodegradable polylactic acid toughening and reinforcing material for injection molding in the embodiment comprises the following raw materials in parts by weight: 94.6 parts of polylactic resin, 5 parts of PLA coated grafted cellulose, 0.1 part of antioxidant 1010,0.1 parts of antioxidant 168 and 0.2 part of lubricant stearic acid.
Example 3
The biodegradable polylactic acid toughening and reinforcing material for injection molding of the embodiment comprises the following raw materials in parts by weight: 91.6 parts of polylactic acid resin, 8 parts of PLA coated grafted cellulose, 0.1 part of antioxidant 1010,0.1 parts of antioxidant 168 and 0.2 part of lubricant stearic acid.
Example 4
The biodegradable polylactic acid toughening and reinforcing material for injection molding in the embodiment comprises the following raw materials in parts by weight: 89.6 parts of polylactic resin, 10 parts of PLA coated grafted cellulose, 0.1 part of antioxidant 1010,0.1 parts of antioxidant 168 and 0.2 part of lubricant stearic acid.
Comparative example 1
The biodegradable polylactic acid toughening and reinforcing material for injection molding of the comparative example comprises the following raw materials in parts by weight: 94.6 parts of polylactic resin, 5 parts of pure nano-cellulose, 0.1 part of antioxidant 1010,0.1 part of antioxidant 168 and 0.2 part of lubricant stearic acid.
To test the properties of the biodegradable injection molding compounds of examples 2 to 4 and comparative example 1, they were injection molded into fully biodegradable sheets of 120mm × 25mm × 3mm as follows: weighing the raw materials according to the proportion, adding the raw materials into a high-speed mixer for full mixing, sending the obtained mixture into a double-screw extruder for extrusion granulation, then sending the mixture into a dryer for repeated drying, and then sending the mixture into an injection molding machine for injection molding (the temperature of the injection molding machine is 185 ℃, and the injection molding pressure is 55 MPa), thus obtaining the fully biodegradable plate.
The tensile strength, flexural strength and impact strength of the samples obtained in examples 2 to 4 and comparative example 1 were measured in accordance with GB/T1040.2-2006, GB/T9341-2000 and GB/T1843-2008, and the results are shown in Table 1.
TABLE 1
| Performance of | Tensile strength/MPa | Elongation at break/% | Flexural Strength/MPa | Notched impact strength/KJ/m 2 |
| Example 2 | 62.5 | 8.3 | 94.2 | 5.5 |
| Example 3 | 64.6 | 11.2 | 98.5 | 10.8 |
| Example 4 | 67.1 | 13.7 | 98.4 | 12.3 |
| Comparative example 1 | 52.4 | 4.8 | 84.1 | 3.7 |
As can be seen from Table 1, the biodegradable PLA products with the modifier added in examples 2-4 have better tensile strength and elongation at break, and improved toughness and bending strength, and can meet the use requirements of PLA degradable materials for toys, tools, packaging boxes, cups and plastic products.
FIG. 3 is a microscopic SEM image of a cross section of a sample injected with a comparative example 1 injection molding compound of the present invention, and FIG. 4 is a microscopic SEM image of a cross section of a sample injected with an injection molding compound of example 2 of the present invention, comparing it to see that the addition of PLA-coated grafted cellulose significantly improves the dispersion and compatibility of the PLA/nanocellulose composite system on a two-dimensional scale.
The foregoing description shows preferred embodiments of the invention, and as noted above, it is to be understood that the invention is not limited to the forms of experiments performed herein, and is not to be construed as excluding other embodiments, but is capable of numerous combinations, modifications, and environments and is capable of changes within the scope of the invention as described herein, commensurate with the skill in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the scope of the invention, which is defined by the claims appended hereto.
Claims (6)
1. The biodegradable polylactic acid toughening and reinforcing material for injection molding is characterized by comprising the following raw materials in parts by weight: 87.5 to 94.8 parts of PLA resin, 5 to 10 parts of PLA coated grafted cellulose, 0.1 to 2 parts of lubricant and 0.1 to 0.5 part of antioxidant.
2. The biodegradable polylactic acid toughening and reinforcing material for injection molding according to claim 1, wherein the preparation method of the PLA-coated grafted cellulose comprises the following steps:
s1, firstly, pouring the nano-cellulose CNF into a high-speed mixer, then adding maleic anhydride, and uniformly stirring at the speed of 300-500 r/min for 15-20 min at normal temperature to uniformly disperse the maleic anhydride; adding dicumyl peroxide into the high-speed mixer, and uniformly stirring at the speed of 300-500 r/min for 3-6 min at normal temperature to obtain a mixture A;
s2, adding PLA resin, zinc stearate, an antioxidant 1010 and an antioxidant 168 into the mixture A, and uniformly stirring at the speed of 300-500 r/min for 3-6 min at normal temperature to obtain a mixture B;
and S3, extruding and granulating the mixture B through a double-screw extruder, wherein the temperature of the extruder is 120-195 ℃, the rotating speed of the extruder is 300-350 rpm, granulating to obtain particles, and drying for 4-6 hours at 55-60 ℃ to obtain the PLA coated grafted cellulose.
3. The biodegradable polylactic acid toughening and reinforcing material for injection molding according to claim 2, wherein: the addition amount of maleic anhydride is 3-5 wt% of the mass of the nano-cellulose, the addition amount of dicumyl peroxide is 0.5-2 wt% of the mass of the nano-cellulose, the addition amount of the nano-cellulose is 20-50 wt% of the mass of PLA, the addition amount of zinc stearate is 0.2-1 wt% of the mass of the PLA, the mass ratio of the antioxidant 1010 to the antioxidant 168 is 1:1, and the total addition amount of the antioxidant 1010 and the antioxidant 168 is 0.2-0.5 wt% of the mass of the PLA.
4. The biodegradable polylactic acid toughening and reinforcing material for injection molding according to claim 1 or 2, wherein: the PLA resin is of injection molding grade, and the melt index is 20-25 g/10min (190 ℃,2.16 kg).
5. The biodegradable polylactic acid toughening and reinforcing material for injection molding according to claim 1, wherein: the biodegradable polylactic acid toughening and reinforcing material comprises the following raw materials in parts by weight: 91.6 parts of PLA resin, 8 parts of PLA coated grafted cellulose, 0.1 part of antioxidant 1010,0.1 parts of antioxidant 168 and 0.2 part of lubricant stearic acid.
6. An injection molded article characterized by: is prepared by injection molding of the biodegradable polylactic acid toughening and reinforcing material of any one of claims 1 to 5.
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| CN202211515003.XA CN115785631A (en) | 2022-11-30 | 2022-11-30 | Biodegradable polylactic acid toughening and reinforcing material for injection molding and injection molding product based on biodegradable polylactic acid toughening and reinforcing material |
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| CN103275472A (en) * | 2013-04-19 | 2013-09-04 | 中国科学院宁波材料技术与工程研究所 | All-bio-based hard polylactic acid composite material and preparation method thereof |
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| CN103275472A (en) * | 2013-04-19 | 2013-09-04 | 中国科学院宁波材料技术与工程研究所 | All-bio-based hard polylactic acid composite material and preparation method thereof |
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