CN110591310B - Modified polylactic acid foaming material and forming method thereof - Google Patents
Modified polylactic acid foaming material and forming method thereof Download PDFInfo
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Abstract
The invention belongs to the field of polylactic acid foaming materials, and relates to a modified polylactic acid foaming material and a forming method thereof, wherein PLA resin, modified resin (LDPE, EVA or POE), filler, a crosslinking agent, a foaming agent, zinc oxide, stearic acid and an antioxidant are used as raw materials, the PLA resin, the modified resin, the filler and the antioxidant are subjected to banburying mixing in an internal mixer according to a certain weight ratio for 5-10min at the temperature of 180 ℃ and 210 ℃ at the rotating speed of 30-40r/min, then the temperature is reduced to 150 ℃, the crosslinking agent dicumyl peroxide (DCP), the foaming agent, the zinc oxide and the stearic acid are added, the banburying is carried out for 3-6min to prepare a PLA pre-foaming material, and then the PLA foaming material is subjected to compression molding and foaming to obtain the PLA foaming material with uniform cells and small density, and has good comprehensive performance.
Description
Technical Field
The invention relates to a foaming material and a forming method thereof, in particular to a modified polylactic acid (PLA) foaming material and a forming method thereof.
Technical Field
The polylactic resin has no pollution in the production process, and the product can be biodegraded, thereby realizing the circulation in the nature and being an ideal green high polymer material. The density of the product is 1.20-1.30g/cm3The melting temperature is between 155-185 ℃, and the molding temperature is generally between 170-230 ℃. The product made of polylactic acid can be biodegraded, and has good biocompatibility, glossiness, transparency, hand feeling and heat resistance (can resist heat of about 120 ℃ and can be used for microwave). Polylactic acid has high tensile strength and bending strength, but pure polylactic acid has low melt strength and slow crystallization speed, and it is difficult to obtain a foamed article having a uniform cell structure. Increasing the melt strength of polylactic acid can be achieved by blending or filling methods.
At present, CN200810200437.4 discloses a preparation method of polylactic acid foaming material, which comprises mixing a tackifying modifier and polylactic acid, mixing the mixture on a mixing roll at 100 ℃ and 170 ℃, and then carrying out mould pressing foaming, wherein the mixing temperature is low, the uniform dispersion is difficult, and when the mixture is mixed at 170 ℃, foaming agent and the like are decomposed, thereby seriously affecting the foaming effect.
Therefore, the invention provides a forming method which has a clearer thought and is more beneficial to improving the foaming effect of the polylactic acid.
Disclosure of Invention
In order to solve the technical problems, polylactic acid and materials with good foaming performance such as LDPE (or EVA, POE) are mainly blended, and a certain amount of filling materials such as kaolin, calcium carbonate and the like are added, so that the viscosity and the foaming performance of the polylactic acid are improved. By utilizing the excellent biodegradability, biocompatibility, glossiness, transparency, hand feeling, heat resistance, antibacterial property, flame retardance and ultraviolet resistance, the foaming material can play an important role in the fields of clothing (underwear and coat), industry (building, agriculture, forestry and paper making), medical health and the like.
In order to achieve the purpose, the specific technical scheme is as follows:
a modified polylactic acid foam material is prepared through mixing polylactic resin, LDPE (or EVA, POE), foaming agent, cross-linking agent dicumyl peroxide (DCP), foaming assistant (Zn oxide), stearic acid and antioxidizing agent (1010) (by internal mixer) to obtain pre-foaming PLA material, and die pressing.
The foaming formula is as follows:
the raw materials of the composition are calculated according to parts by weight.
25-60 parts of PLA resin, 20-60 parts of modified resin, 10-30 parts of filler, 0.2-0.4 part of cross-linking agent, 1-6 parts of foaming agent, 1-2 parts of zinc oxide, 0.5-2 parts of stearic acid and 10100.3-0.6 part of antioxidant.
PLA resin, modified resin (LDPE, EVA or POE), blowing agent, crosslinking agent: dicumyl peroxide (DCP), filler (1000-: 100 parts of kaolin or/and calcium carbonate (subjected to surface treatment by 1% of titanate coupling agent and conventional treatment process), zinc oxide, stearic acid and antioxidant 1010.
The mesh number of the filler is limited to 1000-4500 meshes, the filler is distributed in a dendritic or network shape in a resin matrix, the heterogeneous nucleation effect of bubbles is realized, the growth of the bubbles is facilitated, and if the mesh number is too large, namely the size of inorganic particles is small, the generated cells are uneven, large and irregular. The too small mesh number means that the inorganic particles have a large size and cannot play a good role of nucleating agent, which affects the foaming growth.
Before mixing, the PLA, POE and other raw materials are crushed to make the size of the powdery raw materials close to the size of the auxiliary agent and the mesh number of the filler, namely the particle diameters of the raw materials are close to each other, so that the raw materials are easier to mix uniformly. The size (2-4mm) of the granular raw materials is much larger than that of the auxiliary agent, the difference is more than 10 times, the raw materials are not mixed uniformly, and the foaming forming is not facilitated.
The method specifically comprises the following steps: before mixing, plastic particles such as PLA, POE and the like are crushed by a plastic mill (such as a 600-disc mill manufactured by Zhang hong Kong, Libang mechanical Co., Ltd.), and after crushing, a screen is added to obtain the raw material with the mesh number similar to that of the filler.
The process comprises the following steps:
preparing a PLA pre-foaming blending material: mixing PLA resin, LDPE (or EVA, POE), filler and antioxidant 1010 in an internal mixer according to a certain weight ratio for 5-10min at the temperature of 180 ℃ and 210 ℃ and at the rotating speed of 30-40 r/min. In the temperature range of 180 ℃ to 210 ℃, LDPE (or EVA, POE) and PLA can be mixed and melted, and the filler can be uniformly dispersed in the resin matrix, and if the temperature is lower than the temperature, the mixing is difficult. After being uniformly mixed, the temperature is reduced to 150 ℃, a crosslinking agent dicumyl peroxide (DCP), a foaming agent, zinc oxide and stearic acid are added, and then banburying is carried out for 3-6min, at the temperature, LDPE (or EVA and POE) can be melted, PLA is not melted, but only the auxiliary agent needs to be uniformly dispersed into resin because the LDPE (or EVA and POE) and PLA are fully mixed in the early stage, and the foaming agent and the like are not decomposed, so that the subsequent mould pressing foaming is fully prepared. Therefore, in the invention, LDPE (or EVA, POE) plays a role of a carrier, and the LDPE (or EVA, POE) has high melt strength and good foaming performance and is a good material for improving the foaming performance of PLA. The LDPE (or EVA, POE) can also toughen the PLA. The filler plays a role of a bubble nucleating agent and improves the mechanical property of the foam. The banburying materials are taken out and flattened while hot, so that the subsequent die pressing foaming is facilitated.
Preparing a foaming material: the PLA pre-foamed blending material is foamed through mould pressing. The foaming temperature range can be 190-220 ℃, the pressure can be controlled at 1-20MPa, and the foaming time is 5-20 min. In the temperature range, PLA is melted and is fused with LDPE (or EVA and POE), a foaming agent dispersed in LDPE (or EVA and POE) is decomposed, generated bubbles expand in a PLA/LDPE (or EVA and POE) resin matrix, and meanwhile, DCP is decomposed, the resin matrix is partially crosslinked, so that the melt strength is improved, and the matching of foaming and crosslinking is facilitated.
Due to the adoption of the measures, the PLA foam material with uniform cells and low density is prepared. The PLA foaming material has good comprehensive performance, and can be used in the fields of packaging, automobiles, thermal insulation, buildings, buffer liners, sound absorption, noise reduction and the like.
Drawings
FIG. 1 is a structural diagram of a PLA foam prepared in example 1;
FIG. 2 is a structural diagram of a PLA foam prepared in example 2;
FIG. 3 is a structural diagram of a PLA foam prepared in example 3;
FIG. 4 is a structural diagram of a PLA foam prepared in comparative example 1;
FIG. 5 is a structural view of a PLA foam prepared in comparative example 2.
Detailed Description
Example 1
The foaming formula comprises (by weight parts)
50 parts of PLA resin, 30 parts of LDPE, and the following filler: 20 parts of kaolin (4000 meshes) subjected to surface treatment by 1% of titanate coupling agent, 0.3 part of dicumyl peroxide (DCP) crosslinking agent, 4 parts of foaming agent, 1 part of zinc oxide, 1 part of stearic acid and 10100.3 parts of antioxidant.
The material is available in the following brands or types:
PLA (trade name REVODE190), Zhejiang Haizhen biomaterial GmbH. LDPE (grade 2102TN26), zilu petrochemical. Dicumyl peroxide (DCP), technical grade. An AC foaming agent with the average particle size (Dn) less than or equal to 8-10 μm, Shanghai Wenhua chemical pigment Co. Zinc oxide (ZnO), analytical grade, chemical reagents ltd. Antioxidant 1010, technical grade. Stearic acid, analytically pure, chemical reagents of national drug group, ltd.
The process comprises the following steps:
firstly, the PLA resin and the LDPE are crushed by a plastic mill (such as a 600-millstone mill produced by Zhang hong Kong, Libang machinery Co., Ltd.), and then a 4000-mesh screen is added to obtain the 4000-mesh raw material.
Preparing a PLA pre-foaming blending material: and carrying out banburying and mixing on the crushed PLA resin, the LDPE, the filler and the antioxidant 1010 in an internal mixer according to a certain weight ratio for 8min at the temperature of 210 ℃ and the rotating speed of 30 r/min. Then cooling to 150 ℃, adding a crosslinking agent dicumyl peroxide (DCP), a foaming agent, zinc oxide and stearic acid, and banburying for 4 min. The banburying materials are taken out and flattened while hot, so that the subsequent die pressing foaming is facilitated.
Preparing a foaming material: the PLA pre-foamed blending material is foamed through mould pressing. The foaming temperature can be 210 ℃, the pressure can be controlled at 10MPa, and the foaming time is 10 min.
And taking out the foaming material. The foam density was found to be 0.3g/cm3The tensile strength was 11.3MPa and the elongation at break was 11%. The foam structure is shown in figure 1.
Example 2
The foaming formula comprises (by weight parts)
40 parts of PLA resin, 28 parts of EVA, and the following filler: 26.4 parts of kaolin (3500 meshes) subjected to surface treatment by 1% of titanate coupling agent, 0.3 part of dicumyl peroxide (DCP) crosslinking agent, 3 parts of foaming agent, 1 part of zinc oxide, 1 part of stearic acid and 10100.3 parts of antioxidant.
The material is available in the following brands or types:
PLA (trade name REVODE190), Zhejiang Haizhen biomaterial GmbH. EVA (brand 7470M), taiwan tai-plast. Dicumyl peroxide (DCP), technical grade. An AC foaming agent with the average particle size (Dn) less than or equal to 8-10 μm, Shanghai Wenhua chemical pigment Co. Zinc oxide (ZnO), analytical grade, chemical reagents ltd. Antioxidant 1010, technical grade. Stearic acid, analytically pure, chemical reagents of national drug group, ltd.
The process comprises the following steps:
firstly, the PLA resin and the EVA are pulverized by a plastic pulverizer (such as a 600-disc pulverizer produced by Zhang hong Kong, Libang machinery Co., Ltd.), and then a screen is added to obtain 3500 mesh raw materials.
Preparing a PLA pre-foaming blending material: and (2) banburying and mixing the crushed PPLA resin, EVA, the filler and the antioxidant 1010 in an internal mixer according to a certain weight ratio for 6min at the temperature of 200 ℃ and the rotating speed of 25 r/min. Then cooling to 150 ℃, adding a crosslinking agent dicumyl peroxide (DCP), a foaming agent, zinc oxide and stearic acid, and banburying for 3 min. The banburying materials are taken out and flattened while hot, so that the subsequent die pressing foaming is facilitated.
Preparing a foaming material: the PLA pre-foamed blending material is foamed through mould pressing. The foaming temperature can be 220 ℃, the pressure can be controlled at 10MPa, and the foaming time is 10 min.
And taking out the foaming material. The foam density was found to be 0.37g/cm3The tensile strength was 15.2MPa, and the elongation at break was 14%. The foam structure is shown in figure 2.
Example 3
The foaming formula comprises (by weight parts)
60 parts of PLA resin, 25 parts of POE, and the following filler: 10.4 parts of kaolin (1250 meshes) subjected to surface treatment by 1% of titanate coupling agent, 0.3 part of dicumyl peroxide (DCP) crosslinking agent, 2 parts of foaming agent, 1 part of zinc oxide, 1 part of stearic acid and 10100.3 parts of antioxidant.
The material is available in the following brands or types:
PLA (trade name REVODE190), Zhejiang Haizhen biomaterial GmbH. POE (No. 9061), exxonmobil. Dicumyl peroxide (DCP), technical grade. An AC foaming agent with the average particle size (Dn) less than or equal to 8-10 μm, Shanghai Wenhua chemical pigment Co. Zinc oxide (ZnO), analytical grade, chemical reagents ltd. Antioxidant 1010, technical grade. Stearic acid, analytically pure, chemical reagents of national drug group, ltd.
The process comprises the following steps:
firstly, the PLA resin and POE are pulverized by a plastic pulverizer (such as a 600-millstone pulverizer produced by Zhang hong Kong, Libang machinery Co., Ltd.), and then a screen mesh is added to obtain 1250-mesh raw materials.
Preparing a PLA pre-foaming blending material: and carrying out banburying and mixing on the crushed PLA resin, the POE, the filler and the antioxidant 1010 in an internal mixer according to a certain weight ratio for 9min at the temperature of 205 ℃ and the rotating speed of 26 r/min. Then cooling to 150 ℃, adding a crosslinking agent dicumyl peroxide (DCP), a foaming agent, zinc oxide and stearic acid, and banburying for 4 min. The banburying materials are taken out and flattened while hot, so that the subsequent die pressing foaming is facilitated.
Preparing a foaming material: the PLA pre-foamed blending material is foamed through mould pressing. The foaming temperature can be 210 ℃, the pressure can be controlled at 10MPa, and the foaming time is 10 min.
And taking out the foaming material. The foam density was found to be 0.42g/cm3The tensile strength was 15.4MPa, and the elongation at break was 12%. The foam structure is shown in figure 3.
Comparative example 1
Compared with the example 1, the formula of the comparative example 1 is the same, the difference is that the banburying process is different, and the banburying process specifically comprises the following steps:
preparing a PLA pre-foaming blending material: mixing PLA resin, LDPE, filler, antioxidant 1010, crosslinking agent dicumyl peroxide (DCP), foaming agent, zinc oxide and stearic acid in an internal mixer according to a certain weight ratio for 8min, wherein the mixing temperature is 150 ℃, and the rotating speed is 30 r/min. The banburying materials are taken out and flattened while hot, so that the subsequent die pressing foaming is facilitated.
And taking out the foaming material. The foam density was found to be 0.72g/cm3The tensile strength was 14.6MPa, and the elongation at break was 132%.
The foam structure is shown in figure 4.
Comparative example 2
Comparative example 2 is compared with example 1, except that the raw material particles were not pulverized before use, and the other were not changed, to prepare a foamed material. The foam density was found to be 0.6g/cm3The tensile strength was 16.5MPa and the elongation at break was 9%.
The foam structure is shown in figure 5.
Claims (2)
1. A molding method of a modified polylactic acid foaming material is characterized by comprising the following steps: the foaming material comprises the following raw materials in parts by weight: 25-60 parts of PLA resin, 20-60 parts of modified resin, 10-30 parts of filler, 0.2-0.4 part of cross-linking agent, 1-6 parts of foaming agent, 1-2 parts of zinc oxide, 0.5-2 parts of stearic acid and 10100.3-0.6 part of antioxidant;
100 parts of PLA resin, modified resin, filler, a crosslinking agent, a foaming agent, zinc oxide, stearic acid and an antioxidant 1010;
wherein the modified resin is LDPE, EVA or POE; the crosslinking agent is dicumyl peroxide (DCP); the foaming agent is an AC foaming agent; the antioxidant is 1010;
(1) preparing a PLA pre-foaming blending material: mixing PLA resin, modified resin, filler and antioxidant 1010 in an internal mixer according to a weight ratio for 5-10min, wherein the mixing temperature is 180-210 ℃, and the mixing speed is 30-40 r/min; reducing the temperature to 150 ℃ after banburying, adding a cross-linking agent, a foaming agent, zinc oxide and stearic acid, and banburying for 3-6min to obtain a PLA pre-foamed blending material; crushing the PLA resin and the modified resin before use;
(2) preparing a foaming material: the PLA pre-foaming blending material is foamed by mould pressing to obtain the modified polylactic acid foaming material, wherein the foaming temperature range of the mould pressing foaming is 190-220 ℃, the pressure is controlled to be 1-20MPa, and the foaming time is 5-20 min.
2. The molding method of the modified polylactic acid foamed material according to claim 1, wherein: the filler is kaolin or/and calcium carbonate which is subjected to surface treatment by 1 percent of titanate coupling agent, and the mesh number is 1000-4500 meshes.
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CN111763506B (en) * | 2020-07-09 | 2023-01-13 | 上海浦景化工技术股份有限公司 | Temporary plugging diverting agent and preparation method and application thereof |
CN112189886A (en) * | 2020-09-27 | 2021-01-08 | 河南中烟工业有限责任公司 | Preparation method of cigarette filter tip rod foaming material |
CN113912904A (en) * | 2021-10-20 | 2022-01-11 | 常州大学 | Blending filling modified PET (polyethylene terephthalate) foaming material and forming method thereof |
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JP2005002174A (en) * | 2003-06-10 | 2005-01-06 | Toray Ind Inc | Resin composition and molded article made of the same |
CN103242632A (en) * | 2012-02-14 | 2013-08-14 | 上海杰事杰新材料(集团)股份有限公司 | Polylactic acid degradable foaming material and preparation method thereof |
CN105802159A (en) * | 2014-12-29 | 2016-07-27 | 江苏华信新材料股份有限公司 | Degradable PHA/PLA mixture film and preparation method thereof |
CN104725802A (en) * | 2015-03-27 | 2015-06-24 | 北京石油化工学院 | Preparation method of polylactic acid composite material for hot-melt 3D printing |
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