CN105885368A - Highly heat-resistant polylactic acid/thermoplastic starch composite material and preparation method thereof - Google Patents
Highly heat-resistant polylactic acid/thermoplastic starch composite material and preparation method thereof Download PDFInfo
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- CN105885368A CN105885368A CN201410755949.2A CN201410755949A CN105885368A CN 105885368 A CN105885368 A CN 105885368A CN 201410755949 A CN201410755949 A CN 201410755949A CN 105885368 A CN105885368 A CN 105885368A
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Abstract
The invention is aimed at providing a highly heat-resistant polylactic acid/thermoplastic starch composite material and a preparation method thereof. When poly(L-lactic acid) PLLA and poly(D-lactic acid) PDLA coexist, due to the hydrogen bond acting force of special molecular chains between two molecular chains, a stereocomplex (SC) is generated at the time of polymer crystallization; and the SC and homopolymer both have relatively high melting point (230 DEG C) and play a role of nucleating agent in the product forming process. A little PDLA is added into PLLA, and the SC can serve as a nucleating agent for PLA crystallization so as to improve the crystallization property; during preparation of a blend of PLA and starch, the crystallization speed of the product can be increased by adding appropriate PDLA; and due to the rigidity of the PLA molecular chain, by adding proper plasticizer, the crystallization speed and product crystallinity can be remarkably increased, and the heat resistance is improved.
Description
Technical field
The present invention relates to a kind of high heat-proof polylactic acid/thermoplastic starch powder composite material and tool preparation method.
Background technology
Plastics are most widely used materials, and substantial amounts of use causes very important negative effect to natural environment.Biodegradated polymer materal refers to make to have by nature microorganism (bacterium, fungi etc.) and the macromolecule of degraded occurs.Different with manufacturing process according to raw material composition, natural macromolecular material, chemosynthetic organism degraded macromolecular material, Microbe synthesis macromolecular material can be divided into.PLA is considered as one of the most promising material, has excellent biodegradability and biocompatibility, and raw material can be obtained on a large scale by cereal crops, is a kind of low energy consumption product, and is independent of petroleum resources.But, owing to the price comparison of PLA product is high, product is thermo-labile, causes the application of PLA to be very limited.
Starch and biodegradable polymers its mix, the composite of complete biodegradable can be obtained, when starch and these polymer its mixed time, starch uses as a kind of filler, and they mix with PLA.Improve its mixed thing crystallization rate when normal production and can improve the degree of crystallinity of product, to reach heat-resisting effect.Starch source is extensive, cheap, and high heat-resisting PLA and its mixed thing of starch are also a kind of environmental friendliness and nontoxic thermoplastic, and price is relatively low, and therefore the application prospect in packaging for foodstuff and other consumer product area is boundless.
Patent CN 102268144 A propose a kind of by add thermal distoftion modifying agent improve PLA and the method for starch composite material heat resistance, this patent uses a methyl styrene based polyalcohol as thermal distoftion modifying agent, make PLA improve with the heat resistance of starch composite material, but this heat-proof modifier has to be solved with the consistency problem of starch.
Patent CN 03149911.2 is taken off the inorganic filler including first-class by selection strengthen the heat resistance of PLA include mica, talcum powder, illiteracy, but increase rate is limited, it is impossible to meet some products higher to heat resistant requirements, such as the service plate used in hot food and drink.
Summary of the invention
The defect that the present invention is directed to prior art provides a kind of high heat-proof polylactic acid/thermoplastic starch powder composite material and preparation method thereof.
The present invention, for realizing object above, uses following scheme: a kind of high heat-proof polylactic acid/thermoplastic starch powder composite material, following components and weight portion mix: PLA 20-60 part, starch 20-60 part, plasticiser 5-20 part, coupling agent 5-20 part, nucleator 5-10 part, grafting agent 2-5 part, lubricant 2-5 part, antioxidant 2-5 part, antistatic additive 1-2 part, wherein said PLA is injection grade poly (l-lactic acid) and poly-D-ALPHA-Hydroxypropionic acid, and its molecular weight is 1-20 ten thousand dalton；The addition of described poly-D-ALPHA-Hydroxypropionic acid is 0.1%-10%.
Further, described starch is the mixture of one or more in cornstarch, wheat starch, potato starch, sorghum starch, bean starch, described grafting agent is maleic anhydride, diphenylmethane diisocyanate, formamide and the one with epoxy functional compounds, and described plasticizer is one or more in glycerine, polyethylene glycol, polypropylene glycol, acetic acid tributyl, ATBC, neck dibatyl phithalate, mineral oil, urea.
Further, described coupling agent is usual auxiliaries, one or more mixtures in silane coupler or titanate coupling agent.
Further, described nucleator includes talcum powder, montmorillonite, nanometer SO2, CNT, rare earth, N, N '-ethylene bis stearamide, tert-butyl-calix aromatic hydrocarbons.
Further, described antioxidant is antioxidant 1010 or irgasfos 168.
Further, one or more during described lubricant is fatty acid, fatty acid ester.
Further, described antistatic additive is one or more in alkylsulfonate, alkyl sulfate and quaternary ammonium salt.
The preparation method of a kind of high heat-proof polylactic acid/thermoplastic starch powder composite material, comprises the following steps:
(1), by 50-80% starch, 5%-20% glycerine, additive, 5%-20% silane coupler or titanate coupling agent, 2%-5% maleic anhydride, grafting agent, 2%-5% fatty acid or fatty acid ester add stirring in high speed mixing smelting machine, time is 10-50 minute, and normal temperature mixes, stand-by；
(2), poly (l-lactic acid) and poly-D-ALPHA-Hydroxypropionic acid are mixed by same ratio, use its mixed method of solution to prepare polylactic acid stereoscopic composite；
(3) mixture that, by step (1) obtains and after double screw extruder extruding pelletization, mixes granulation again with the stereoscopic composite obtained in 20%-60% PLA, 0.1-2% antistatic additive, 1%-3% antioxidant and 1 part of step (2).
Further, the high speed muller in step (1) is banbury, Haake torque rheometer, double screw extruder, and operating temperature is at 20-120 DEG C.
Further, the draw ratio of described double screw extruder is 25: 1-40: 1, and from feeding section to die face, each district temperature controls to be 150 to 230 DEG C.
Beneficial effects of the present invention: the addition of nucleator and PDLA is made PLA crystallization rate when producing product accelerate by the present invention, and the degree of crystallinity of product improves, and makes have preferable heat resistance, card softening temperature can reach 90-140 DEG C；The tableware requirement used in food and drink can be met completely.
Detailed description of the invention
A kind of high heat-proof polylactic acid/thermoplastic starch powder composite material, mixed by following components and weight portion: PLA 20-60 part, starch 20-60 part, plasticiser 5-20 part, coupling agent 5-20 part, nucleator 5-10 part, grafting agent 2-5 part, lubricant 2-5 part, antioxidant 2-5 part, antistatic additive 1-2 part, wherein said PLA is injection grade poly (l-lactic acid) and poly-D-ALPHA-Hydroxypropionic acid, and its molecular weight is 1-20 ten thousand dalton；The addition of described poly-D-ALPHA-Hydroxypropionic acid is 0.1%-10%.
Described starch is the mixture of one or more in cornstarch, wheat starch, potato starch, sorghum starch, bean starch, described grafting agent is maleic anhydride, diphenylmethane diisocyanate, formamide and the one with epoxy functional compounds, and described plasticizer is one or more in glycerine, polyethylene glycol, polypropylene glycol, acetic acid tributyl, ATBC, neck dibatyl phithalate, mineral oil, urea.
Described coupling agent is usual auxiliaries, one or more mixtures in silane coupler or titanate coupling agent.
Described nucleator includes talcum powder, montmorillonite, nanometer SO2, CNT, rare earth, N, N '-ethylene bis stearamide, tert-butyl-calix aromatic hydrocarbons.
Described antioxidant is antioxidant 1010 or irgasfos 168.
Described lubricant is one or more in fatty acid, fatty acid ester.
Described antistatic additive is one or more in alkylsulfonate, alkyl sulfate and quaternary ammonium salt.
The preparation method of a kind of high heat-proof polylactic acid/thermoplastic starch powder composite material, comprises the following steps:
(1), by 50-80% starch, 5%-20% glycerine, additive, 5%-20% silane coupler or titanate coupling agent, 2%-5% maleic anhydride, grafting agent, 2%-5% fatty acid or fatty acid ester add stirring in high speed mixing smelting machine, time is 10-50 minute, and normal temperature mixes, stand-by；
(2), poly (l-lactic acid) and poly-D-ALPHA-Hydroxypropionic acid are mixed by same ratio, use its mixed method of solution to prepare polylactic acid stereoscopic composite；
(3) mixture that, by step (1) obtains and after double screw extruder extruding pelletization, mixes granulation again with the stereoscopic composite obtained in 20%-60% PLA, 0.1-2% antistatic additive, 1%-3% antioxidant and 1 part of step (2).
High speed mixing smelting machine in step (1) is banbury, Haake torque rheometer, double screw extruder, and operating temperature is at 20-120 DEG C.
The draw ratio of described double screw extruder is 25: 1-40: 1, and from feeding section to die face, each district temperature controls to be 150 to 230 DEG C.
Detailed description of the invention one:
Cornstarch, PLA are dried；Extracting corn starch 40%, glycerine 15% are in banbury, banburying 20min at 115 DEG C, pulverize after taking out cooling, obtain thermoplastic starch: by thermoplastic starch and 30% PLA (containing 2% dextrorotation PLA), 15% glycerine, 5% maleic anhydride, 5%3-aminopropyl triethoxysilane, 2% stearic acid adds in high-speed mixer and mixes 10 minutes at 100 DEG C；To add 1% antioxidant 1010,1% talcum powder and 1% sodium alkyl sulfonate in mixture and add double screw extruder extruding pelletization, each section of temperature of extruder is set as (from charging aperture to getting to know): 160,180,185,185,190,200 DEG C.Screw speed 110rpm, feeding rotating speed 15rpm, dry the pellet of extrusion at 80 DEG C, blowfilm shaping.Prepared fully biodegradable polylactic acid starch composite material becomes white or slightly yellow solid, after 8 weeks compost, degradation rate is more than 95%, heat distortion temperature 120 DEG C, hot strength 35MPa, elongation at break 40%, melt flow rate (MFR) is 8g/10min (190 DEG C, 2.16kg), can machine-shaping on various process equipments.
Detailed description of the invention two:
Cornstarch, PLA are dried；Extracting corn starch 55%, glycerine 15% are in banbury, banburying 20min at 110 DEG C, pulverize after taking out cooling, obtain thermoplastic starch: by thermoplastic starch and 20% PLA (containing 2% dextrorotation PLA), 15% glycerine, 3% maleic anhydride, 2%3-aminopropyl triethoxysilane, 2% stearic acid adds in high-speed mixer and mixes 10 minutes at 100 DEG C；To add 1% antioxidant 1010,1% talcum powder and 1% sodium alkyl sulfonate in mixture and add double screw extruder extruding pelletization, each section of temperature of extruder is set as (from charging aperture to getting to know): 160,180,185,185,190,200 DEG C.Screw speed 110rpm, feeding rotating speed 15rpm, dry the pellet of extrusion at 80 DEG C, blowfilm shaping.After 8 weeks compost, degradation rate is more than 95%, heat distortion temperature 110 DEG C, hot strength 30MPa, elongation at break 32%, and melt flow rate (MFR) is 6g/10min (190 DEG C, 2.16kg), can machine-shaping on various process equipments.
Claims (10)
1. high heat-proof polylactic acid/thermoplastic starch powder composite material, is mixed by following components and weight portion: PLA 20-60
Part, starch 20-60 part, plasticiser 5-20 part, coupling agent 5-20 part, nucleator 5-10 part, grafting agent 2-5 part, lubricant 2-5
Part, antioxidant 2-5 part, antistatic additive 1-2 part, wherein said PLA is injection grade poly (l-lactic acid) and poly-D-ALPHA-Hydroxypropionic acid, its molecular weight
For 1-20 ten thousand dalton；The addition of described poly-D-ALPHA-Hydroxypropionic acid is 0.1%-10%.
The high heat-proof polylactic acid of one the most according to claim 1/thermoplastic starch powder composite material, it is characterised in that described shallow lake
Powder is the mixture of one or more in cornstarch, wheat starch, potato starch, sorghum starch, bean starch, and described grafting agent is
Maleic anhydride, diphenylmethane diisocyanate, formamide and the one with epoxy functional compounds, described plasticizer is glycerine, poly-second
One or more in glycol, polypropylene glycol, acetic acid tributyl, ATBC, neck dibatyl phithalate, mineral oil, urea.
The high heat-proof polylactic acid of one the most according to claim 1/thermoplastic starch powder composite material, it is characterised in that described idol
Connection agent is usual auxiliaries, one or more mixtures in silane coupler or titanate coupling agent.
The high heat-proof polylactic acid of one the most according to claim 1/thermoplastic starch powder composite material, it is characterised in that described one-tenth
Core agent includes talcum powder, covers de-upper, nanometer S02, CNT, dilute upper, N, N '-ethylene bis stearamide, tert-butyl-calix aromatic hydrocarbons.
The high heat-proof polylactic acid of one the most according to claim 1/thermoplastic starch powder composite material, it is characterised in that described is anti-
Oxygen agent is antioxidant 1010 or irgasfos 168.
The high heat-proof polylactic acid of one the most according to claim 1/thermoplastic starch powder composite material, it is characterised in that described lubrication
Agent is one or more in fatty acid, fatty acid ester.
The high heat-proof polylactic acid of one the most according to claim 1/thermoplastic starch powder composite material, it is characterised in that described is anti-
Electrostatic agent is one or more in alkylsulfonate, alkyl sulfate and quaternary ammonium salt.
8. the preparation method of one kind high heat-proof polylactic acid/thermoplastic starch powder composite material, it is characterised in that comprise the following steps:
(1), by 50-80% starch, 5%-20% glycerine, additive, 5%-20% silane coupler or titanate coupling agent, 2%-5% Malaysia
Acid anhydrides, by branch agent, 2%-5% fatty acid or fatty acid ester add in high speed mixing smelting machine and stir, and the time is 10-50 minute, and normal temperature mixes,
Stand-by；
(2), poly (l-lactic acid) and poly-D-ALPHA-Hydroxypropionic acid are mixed by same ratio, use its mixed method of solution to prepare polylactic acid stereoscopic composite；
(3) mixture that, by step (1) obtains and after double screw extruder extruding pelletization, resists with 20%-60% PLA, 0.1-2%
The stereoscopic composite obtained in electrostatic agent, 1%-3% antioxidant and 1 part of step (2) mixes granulation again.
The preparation method of a kind of high heat-proof polylactic acid/thermoplastic starch powder composite material the most according to claim 8, it is characterised in that
High speed mixing smelting machine in step (1) is banbury, Haake torque rheometer, double screw extruder, and operating temperature is at 20-120 DEG C.
The preparation method of a kind of high heat-proof polylactic acid/thermoplastic starch powder composite material the most according to claim 8 or claim 9, its feature
Being, the draw ratio of described double screw extruder is 25: 1-40: 1, and from feeding section to die face, each district temperature controls to be 150 to 230 DEG C.
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Cited By (11)
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| CN106366587A (en) * | 2016-08-26 | 2017-02-01 | 江苏允友成生物环保材料有限公司 | Preparation method of biodegradable polylactic acid/starch composite |
| CN108219208A (en) * | 2017-12-05 | 2018-06-29 | 湖北光合生物科技有限公司 | A kind of thermoplastic starch powder composite material and preparation method thereof |
| CN108752888A (en) * | 2018-07-02 | 2018-11-06 | 江南大学 | A kind of heat-proof polylactic acid composition and preparation method thereof |
| CN108841153A (en) * | 2018-07-02 | 2018-11-20 | 江南大学 | A kind of high-ductility, high heat distortion temperature poly (lactic acid) composition and preparation method thereof |
| CN109486083A (en) * | 2018-12-20 | 2019-03-19 | 吉林中粮生化有限公司 | A kind of biodegradable blend film and preparation method thereof |
| CN109651784A (en) * | 2018-12-17 | 2019-04-19 | 吉林中粮生化有限公司 | Fully biodegradable equipment for prepn. of yoghurt and preparation method thereof |
| CN109912945A (en) * | 2018-11-19 | 2019-06-21 | 江苏科技大学 | A kind of poly-lactic acid in high molecular weight material and preparation method thereof |
| CN109988400A (en) * | 2019-04-18 | 2019-07-09 | 谷水英 | A kind of environment-friendly type degradable packaging composite film and preparation method thereof |
| CN110452512A (en) * | 2019-09-18 | 2019-11-15 | 南京博方生物科技有限公司 | A kind of amyloid biomass imitative rattan material and preparation method thereof |
| CN112626637A (en) * | 2020-12-08 | 2021-04-09 | 浩珂科技有限公司 | Fully-degradable polylactic acid fiber with high crystallinity and low water absorption and preparation method thereof |
| CN114381043A (en) * | 2022-03-22 | 2022-04-22 | 中科南京绿色制造产业创新研究院 | Starch-based biodegradable plastic and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108752888B (en) * | 2018-07-02 | 2020-10-30 | 江南大学 | Heat-resistant polylactic acid composition and preparation method thereof |
| CN108841153A (en) * | 2018-07-02 | 2018-11-20 | 江南大学 | A kind of high-ductility, high heat distortion temperature poly (lactic acid) composition and preparation method thereof |
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| CN109651784A (en) * | 2018-12-17 | 2019-04-19 | 吉林中粮生化有限公司 | Fully biodegradable equipment for prepn. of yoghurt and preparation method thereof |
| CN109486083A (en) * | 2018-12-20 | 2019-03-19 | 吉林中粮生化有限公司 | A kind of biodegradable blend film and preparation method thereof |
| CN109988400A (en) * | 2019-04-18 | 2019-07-09 | 谷水英 | A kind of environment-friendly type degradable packaging composite film and preparation method thereof |
| CN109988400B (en) * | 2019-04-18 | 2021-05-14 | 瑞力恒生态科技(深圳)有限公司 | Environment-friendly degradable packaging composite film and preparation method thereof |
| CN110452512A (en) * | 2019-09-18 | 2019-11-15 | 南京博方生物科技有限公司 | A kind of amyloid biomass imitative rattan material and preparation method thereof |
| CN112626637A (en) * | 2020-12-08 | 2021-04-09 | 浩珂科技有限公司 | Fully-degradable polylactic acid fiber with high crystallinity and low water absorption and preparation method thereof |
| CN112626637B (en) * | 2020-12-08 | 2022-12-30 | 浩珂科技有限公司 | Fully-degradable polylactic acid fiber with high crystallinity and low water absorption and preparation method thereof |
| CN114381043A (en) * | 2022-03-22 | 2022-04-22 | 中科南京绿色制造产业创新研究院 | Starch-based biodegradable plastic and preparation method thereof |
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