CN107151427A - A kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin and preparation method thereof - Google Patents
A kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin and preparation method thereof Download PDFInfo
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- CN107151427A CN107151427A CN201610117085.0A CN201610117085A CN107151427A CN 107151427 A CN107151427 A CN 107151427A CN 201610117085 A CN201610117085 A CN 201610117085A CN 107151427 A CN107151427 A CN 107151427A
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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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- 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
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention discloses a kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin and preparation method thereof.The polylactic acid modified resin of the present invention includes following raw material by mass percentage：30-90% PLA, 5-65% thermoplastic starch, 3-40% fully biodegradable string, 1-10% auxiliary agent；Wherein, auxiliary agent is lubricant, coupling agent and antioxidant.Each raw material is first dried, then high-speed mixer is added in the ratio and is blended 5-30 minutes, it is to obtain biodegradable toughness reinforcing heat-proof polylactic acid modified resin that gained compound, which adds plasticizing extruding pelletization in double screw extruder,.The preparation method equipment requirement of the polylactic acid modified resin of the present invention and technological process are simple, and cost is low, easily accomplishes scale production, economical and efficient；By the way that thermoplastic starch and the addition of fully biodegradable string are entered in PLA matrix, it is ensured that product has preferable heat resistance and impact property concurrently.
Description
Technical field
The invention belongs to Biodegradable polymer material blending and Polymer Processing field, and in particular to a kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin and preparation method thereof.
Background technology
PLA is a kind of class aliphatic polyester for coming from renewable resource, with good biocompatibility and biological degradability.Hydrolyzed in natural environment or by microbial degradation, PLA finally can be analyzed to carbon dioxide and water.With the raising of people's environmental consciousness and constantly riseing for conventional petroleum based high-polymer price, PLA is by more and more extensive concern, its application field is also constantly widened, there is biologic medical to be applied to packaging, fiber, to fields such as electronic product, automobiles, it is expected to turn into one of 21 century most important material.As a kind of resource recyclable materials, PLA is a kind of most, the with fastest developing speed biomaterial of Recent study, but also there is the defect in many performances in practical application.With going deep into for basic research and application study, develop the various modified composite materials that many PLAs are main body, it is no longer single especially to emphasize polylactic acid degradable performance as in the past, more prominent PLAs are used as a kind of material, it is that a class has functional plastic material, it can embody that PLA low-carbon, resource are renewable in durable material field, save other performance characteristics such as petroleum resources, poly-lactic acid material is returned in application aspect in reasonable, practical application also expands therewith.
Also it is subject to certain restrictions PLA as versatile material application at this stage, this is mainly the performance deficiency of PLA presence, wherein the two of most critical point are：One is that PLA is crisp frangible, and fracture elongation is low and impact resistance is poor；Two be that PLA heat endurance is not enough, and it also can be that molecular weight significantly declines to be processed below heat decomposition temperature.PLA has a very high intensity and modulus, but existing conventional PLA toughening modifying method, it is generally difficult to accomplish while toughness reinforcing, it is ensured that its transparency, intensity and biocompatibility are not lost.It is carrier, by being modified respectively to PLA, starch, inorganic particle etc. this patent discloses an a kind of PLA, then obtained material that can be degradable is granulated on extruder again, although overcoming black brittleness, be greatly reduced cost, but and unresolved PLA processing in non-refractory, oxidizable decomposition the problem of.This patent prepares polydactyl acid/starch blending system, and with the addition of various auxiliary agents, but heat resisting temperature is improved only to 85 DEG C, still it may not apply in the higher life based article of the heat resisting temperature such as dish, cup, in order to overcome these to limit to, it is necessary to processing is modified to PLA, cost is reduced, temperature limit is improved, while keeping its excellent mechanical property.
Totally biodegradable string is equally a kind of natural material with excellent heat resistance, rigidity and molding processibility.Starch is a kind of natural macromolecular material, has the advantages that source is wide, cheap, biodegradable, is considered as one of most potential research object in degradation material field.But great amount of hydroxy group is carried in starch molecular chain, make its intermolecular and intramolecular there are a large amount of hydrogen bonds to be formed, this make it that starch processing characteristics is undesirable, generally requires to make it have certain plasticity by the way of molecular modification.In patent of the present invention, using PLA as base resin material, will have it is flexible can degradable string be used as activeness and quietness component, and add the heat decomposition temperature that thermoplastic starch improves resin, a variety of auxiliary agents such as antioxidant, coupling agent, profit auxiliary agent are added, heat-resisting and toughening modifying while to poly-lactic acid material is finally realized.Compared with traditional petroleum base high polymer material, the modified polylactic acid material obtained by the above method is suitable for all kinds of environment-friendly biodegradable plastic products of large-scale production.The modification and forming method of the present invention not only reduces production cost, technique is simple and environmentally-friendly, the combination property of product is also improved simultaneously, and such as heat resistance, durability and impact resistance are a class high-performance, low cost, the new modified polylactic acid material of fully biodegradable.
The content of the invention
To solve above-mentioned existing shortcomings and deficiencies, it is an object of the invention to provide a kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin and preparation method thereof.
To achieve these goals, the technical scheme is that：
The invention provides a kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin, it includes following raw material by mass percentage：30-90% PLA, 5-65% thermoplastic starch, 3-40% fully biodegradable string, 1-10% auxiliary agent, total amount meets 100%.Wherein, described auxiliary agent is lubricant, coupling agent and antioxidant.
Described PLA is preferably PDLLA or poly (l-lactic acid), and its viscosity average molecular weigh is 2-30 ten thousand.
Described thermoplastic starch is preferably prepared by the method comprised the following steps：By starch and glycerine in mass ratio 15:1 is put into mixer, in being mediated 10 minutes at 120 DEG C, is crushed after being drawn off cooling, thermoplastic starch is finally made.
Described fully biodegradable string is preferably ramee, wood powder or ramee/wood powder blend.
Described lubricant is preferably stearic acid or atoleine；The consumption of lubricant is preferably the 0.4-5% of PLA, thermoplastic starch and fully biodegradable string gross mass.
Described antioxidant is preferably antioxidant 1010；The consumption of antioxidant is preferably the 0.2-3% of PLA, thermoplastic starch and fully biodegradable string gross mass.
The preparation method of above-mentioned biodegradable toughness reinforcing heat-proof polylactic acid modified resin, comprises the following steps：Above-mentioned each raw material is first dried, is blended 5-30 minutes adding high mixer in the ratio, changing extruding pelletization in gained compound addition double screw extruder obtains biodegradable toughness reinforcing heat-proof polylactic acid modified resin.
Described drying is preferably to be dried 6-24 hours at 50-100 DEG C；
The speed being blended in described high-speed mixer is 800r/min；
The condition of plasticizing extruding pelletization is preferably in double screw extruder：Temperature is 140-200 DEG C, and feed screw speed is 10-30rpm, and driving screw rotating speed is 130-180rpm.
Compared with the existing technology, advantages of the present invention and effect are embodied in：
（1）Thermoplastic starch and string that the present invention is added, all with good processing characteristics and fully biodegradable, maintain the advantage of polylactic acid article energy-conserving and environment-protective；
（2）If only adding thermoplastic starch, the heat resisting temperature of polylactic acid article is difficult to bring up to more than 85 DEG C, and mechanical property has declined.Fully biodegradable string has good ductility, elongation at break and mechanical strength, thermoplastic starch and fully biodegradable string are added in PLA matrix simultaneously, product be ensure that while having preferable heat resistance and impact property concurrently, synergy is ideal；
（3）The addition of thermoplastic starch and fully biodegradable string, effectively reduces the production cost of polylactic acid article.In addition, using preparation method of the present invention, its equipment requirement and technological process are simple, and cost is low, easily accomplishes scale production, economical and efficient, is easy to actual popularization and application.
Polylactic acid article mainly has two defects：Heat resistance is bad, poor toughness.The present invention solves two problems simultaneously, also reduces cost simultaneously, and maintain biodegradability.
Embodiment
With reference to embodiment, the present invention is further detailed explanation.GB is used in following examples（National standard）The properties of material are determined, unless otherwise instructed, the number of component is parts by weight.
Thermoplastic starch in following examples is prepared via a method which to obtain：By starch and glycerine in mass ratio 15:1 is put into mixer, in being mediated 10 minutes at 120 DEG C, is crushed after being drawn off cooling, thermoplastic starch is finally made.
Embodiment 1
（1）A kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin, it includes following raw material by mass percentage：(viscosity average molecular weigh is 100,000 to 70% DL-LACTIC ACID）, 15% thermoplastic starch, 10% ramee, 2% stearic acid, 2% γ-glycidyl ether oxygen propyl trimethoxy silicane and 1% antioxidant 1010；
（2）Each raw material is first dried 12 hours at 80 DEG C, then it is added to high-speed mixer 800r/min by above-mentioned mass percent to be blended 20 minutes, it is that 20rpm, driving screw rotating speed are that plasticizing extruding pelletization obtains biodegradable toughness reinforcing heat-proof polylactic acid modified resin under conditions of 150rpm that gained compound, which adds double screw extruder in 170 DEG C of temperature, feed screw speed,；
（3）The biodegradable toughness reinforcing heat-proof polylactic acid modified resin heat resisting temperature that the present embodiment is obtained is 91 DEG C, and tensile break strength and stretch modulus are up to 81.12MPa, 2871.48MPa respectively.
Embodiment 2
（1）A kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin, it includes following raw material by mass percentage：(viscosity average molecular weigh is 300,000 to 70% DL-LACTIC ACID）, 15% thermoplastic starch, 10% ramee, 2% stearic acid, 2% γ-glycidyl ether oxygen propyl trimethoxy silicane and 1% antioxidant 1010；
（2）Each raw material is first dried 12 hours at 80 DEG C, then it is added to high-speed mixer 800r/min by above-mentioned mass percent to be blended 20 minutes, it is that 20rpm, driving screw rotating speed are that plasticizing extruding pelletization obtains biodegradable toughness reinforcing heat-proof polylactic acid modified resin under conditions of 180rpm that gained compound, which adds double screw extruder in 170 DEG C of temperature, feed screw speed,；
（3）The biodegradable toughness reinforcing heat-proof polylactic acid modified resin heat resisting temperature that the present embodiment is obtained is 95 DEG C, and tensile break strength and stretch modulus are up to 92.36MPa, 2944.63MPa respectively.
Embodiment 3
（1）A kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin, it includes following raw material by mass percentage：(viscosity average molecular weigh is 20,000 to 70% DL-LACTIC ACID）, 15% thermoplastic starch, 10% ramee, 2% stearic acid, 2% γ-glycidyl ether oxygen propyl trimethoxy silicane and 1% antioxidant 1010；
（2）Each raw material is first dried 12 hours at 80 DEG C, then it is added to high-speed mixer 800r/min by above-mentioned mass percent to be blended 20 minutes, it is that 20rpm, driving screw rotating speed are that plasticizing extruding pelletization obtains biodegradable toughness reinforcing heat-proof polylactic acid modified resin under conditions of 150rpm that gained compound, which adds double screw extruder in 170 DEG C of temperature, feed screw speed,；
（3）The biodegradable toughness reinforcing heat-proof polylactic acid modified resin heat resisting temperature that the present embodiment is obtained is 82 DEG C, and tensile break strength and stretch modulus are up to 77.31MPa, 2830.47MPa respectively.
Embodiment 4
（1）A kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin, it includes following raw material by mass percentage：(viscosity average molecular weigh is 100,000 to 70% DL-LACTIC ACID）, 15% thermoplastic starch, 10% ramee, 2% stearic acid, 2% γ-glycidyl ether oxygen propyl trimethoxy silicane and 1% antioxidant 1010；
（2）Each raw material is first dried 12 hours at 80 DEG C, then it is added to high-speed mixer 800r/min by above-mentioned mass percent to be blended 20 minutes, it is that 20rpm, driving screw rotating speed are that plasticizing extruding pelletization obtains biodegradable toughness reinforcing heat-proof polylactic acid modified resin under conditions of 150rpm that gained compound, which adds double screw extruder in 170 DEG C of temperature, feed screw speed,；
（3）The biodegradable toughness reinforcing heat-proof polylactic acid modified resin heat resisting temperature that the present embodiment is obtained is 105 DEG C, and tensile break strength and stretch modulus are up to 91.61MPa, 2977.86MPa respectively.
Embodiment 5
（1）A kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin, it includes following raw material by mass percentage：(viscosity average molecular weigh is 100,000 to 70% DL-LACTIC ACID）, 15% thermoplastic starch, 10% ramee/wood powder expects altogether（Mass ratio 1:1）, 2% stearic acid, 2% γ-glycidyl ether oxygen propyl trimethoxy silicane and 1% antioxidant 1010；
（2）Each raw material is first dried 12 hours at 80 DEG C, then it is added to high-speed mixer 800r/min by above-mentioned mass percent to be blended 20 minutes, it is that 20rpm, driving screw rotating speed are that plasticizing extruding pelletization obtains biodegradable toughness reinforcing heat-proof polylactic acid modified resin under conditions of 130rpm that gained compound, which adds double screw extruder in 170 DEG C of temperature, feed screw speed,；
（3）The biodegradable toughness reinforcing heat-proof polylactic acid modified resin heat resisting temperature that the present embodiment is obtained is 87 DEG C, and tensile break strength and stretch modulus are up to 78.32MPa, 2750.41MPa respectively.
Embodiment 6
（1）A kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin, it includes following raw material by mass percentage：(viscosity average molecular weigh is 100,000 to 70% DL-LACTIC ACID）, 15% thermoplastic starch, 10% ramee, 2% atoleine, 2% γ-glycidyl ether oxygen propyl trimethoxy silicane and 1% antioxidant 1010；
（2）Each raw material is first dried 12 hours at 80 DEG C, then it is added to high-speed mixer 800r/min by above-mentioned mass percent to be blended 20 minutes, it is that 20rpm, driving screw rotating speed are that plasticizing extruding pelletization obtains biodegradable toughness reinforcing heat-proof polylactic acid modified resin under conditions of 150rpm that gained compound, which adds double screw extruder in 170 DEG C of temperature, feed screw speed,；
（3）The biodegradable toughness reinforcing heat-proof polylactic acid modified resin heat resisting temperature that the present embodiment is obtained is 96 DEG C, and tensile break strength and stretch modulus are up to 83.12MPa, 2819.37MPa respectively.
Claims (9)
1. a kind of biodegradable toughness reinforcing heat-proof polylactic acid modified resin, it is characterised in that：Include raw material as follows by mass percentage：30-90% PLA, 5-65% thermoplastic starch, 3-40% fully biodegradable string, 1-10% auxiliary agents；Wherein, described auxiliary agent is lubricant, coupling agent and antioxidant.
2. the biodegradable toughness reinforcing heat-proof polylactic acid modified resin according to claims 1, it is characterised in that：Described PLA is PDLLA or Pfansteihl, and its viscosity average molecular weigh is 2-30 ten thousand.
3. the biodegradable toughness reinforcing heat-proof polylactic acid modified resin according to claims 1, it is characterised in that：Described thermoplastic starch is prepared by the method comprised the following steps：By starch and glycerine in mass ratio 15:1 is put into mixer, in being mediated 10 minutes at 120 DEG C, is crushed after being drawn off cooling, thermoplastic starch is finally made.
4. the biodegradable toughness reinforcing heat-proof polylactic acid modified resin according to claims 1, it is characterised in that：Described fully biodegradable string ramee, wood powder or ramee/wood powder blend.
5. the biodegradable toughness reinforcing heat-proof polylactic acid modified resin according to claims 1, it is characterised in that：Described lubricant is stearic acid or atoleine；The consumption of lubricant is the 0.4-5% of PLA, thermoplastic starch and fully biodegradable string gross mass.
6. the biodegradable toughness reinforcing heat-proof polylactic acid modified resin according to claims 1, it is characterised in that：Described coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane；The consumption of coupling agent is the 0.4-5% of PLA, thermoplastic starch and fully biodegradable string gross mass.
7. the biodegradable toughness reinforcing heat-proof polylactic acid modified resin according to claims 1, it is characterised in that：Described antioxidant is antioxidant 1010；The consumption of antioxidant is the 0.2-3% of PLA, thermoplastic starch and fully biodegradable string gross mass.
8. the preparation method of the biodegradable toughness reinforcing heat-proof polylactic acid modified resin described in claim any one of 1-7, it is characterised in that comprise the following steps：Each raw material is first dried, is blended 5-30 minutes adding high mixer in the ratio, changing extruding pelletization in gained compound addition double screw extruder obtains biodegradable toughness reinforcing heat-proof polylactic acid modified resin.
9. the biodegradable toughness reinforcing heat-proof polylactic acid modified resin preparation method according to claims 8, it is characterised in that：
Described drying is to be dried 6-24 hours at 50-100 DEG C；
The speed being blended in described high-speed mixer is 800r/min；
The condition of plasticizing extruding pelletization is in double screw extruder：Temperature is 140-200 DEG C, and feed screw speed is 10-30rpm, and driving screw rotating speed is 130-180rpm.
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| CN112266583A (en) * | 2020-10-26 | 2021-01-26 | 苏州和塑美科技有限公司 | Preparation method of high-strength low-cost full-biodegradable material and product thereof |
| CN112500688A (en) * | 2020-11-30 | 2021-03-16 | 捷成实业（深圳）有限公司 | Biodegradable antibacterial toy material and preparation method thereof |
| CN113278272A (en) * | 2021-06-04 | 2021-08-20 | 四川宽窄纸品有限责任公司 | Plant cellulose-based full-biodegradable material and preparation method thereof |
| CN113683874A (en) * | 2021-09-24 | 2021-11-23 | 南京五瑞生物降解新材料研究院有限公司 | Full-biomass full-degradable material and preparation method and application thereof |
| CN113831606A (en) * | 2021-09-24 | 2021-12-24 | 南京五瑞生物降解新材料研究院有限公司 | Complete bio-based material and preparation method and application thereof |
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- 2016-03-02 CN CN201610117085.0A patent/CN107151427A/en active Pending
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| CN112266583A (en) * | 2020-10-26 | 2021-01-26 | 苏州和塑美科技有限公司 | Preparation method of high-strength low-cost full-biodegradable material and product thereof |
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| CN113683874A (en) * | 2021-09-24 | 2021-11-23 | 南京五瑞生物降解新材料研究院有限公司 | Full-biomass full-degradable material and preparation method and application thereof |
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| CN114292501B (en) * | 2021-12-03 | 2023-10-20 | 东莞职业技术学院 | Biodegradable material and preparation method and application thereof |
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