CN112920577A - High-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material and preparation method thereof - Google Patents

High-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material and preparation method thereof Download PDF

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CN112920577A
CN112920577A CN202110141220.6A CN202110141220A CN112920577A CN 112920577 A CN112920577 A CN 112920577A CN 202110141220 A CN202110141220 A CN 202110141220A CN 112920577 A CN112920577 A CN 112920577A
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polylactic acid
percent
magnesium salt
salt whisker
composite material
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孙洲渝
张克伟
樊海彬
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Suzhou Sufa Biomaterials Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/04Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/04Ingredients characterised by their shape and organic or inorganic ingredients
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/324Alkali metal phosphate
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/05Alcohols; Metal alcoholates
    • C08K5/053Polyhydroxylic alcohols
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098Metal salts of carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/36Sulfur-, selenium-, or tellurium-containing compounds
    • C08K5/41Compounds containing sulfur bound to oxygen
    • C08K5/42Sulfonic acids; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/08Oxygen-containing compounds

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Abstract

A high surface quality magnesium salt whisker fiber reinforced polylactic acid composite material and a preparation method thereof belong to the technical field of biodegradable plastics and preparation thereof. The method comprises the following steps: taking 50.9-84.1% of polylactic acid, 10-30% of magnesium salt whisker, 5-15% of toughening agent, 0.1-0.3% of nucleating agent, 0.2-0.8% of lubricant, 0.1-1% of auxiliary agent and 0.5-2% of coloring agent as raw materials, and drying the polylactic acid; putting the dried polylactic acid, the flexibilizer, the nucleating agent, the lubricant, the auxiliary agent and the colorant into a high-speed mixer and stirring; and putting the obtained mixture into a double-screw extruder, and cooling and granulating after the mixture is extruded by the double-screw extruder to obtain the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material. The high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material can be ensured to be obtained; the appearance effect of the final product is good; the rigidity and the strength of the composite material are improved, the process is simple, and the requirement of industrial scale-up production is met.

Description

High-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of biodegradable plastics and preparation thereof, and particularly relates to a high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material and a preparation method thereof.
Background
The high surface quality mentioned above means: since the molded and manufactured product has an excellent smooth surface, the molded product can be directly used without surface coating treatment such as polishing and painting, however, in order to improve the rigidity and strength of the biodegradable material, the prior art is often reinforced by adding mineral materials such as glass fiber, etc., and the diameter ratio of the glass fiber is larger (in 10 μm or more), so that the appearance of the injection molded product is rough, and the injection molded product is difficult to directly use, and can only be used after the treatment such as polishing or painting. Plastics made of petrochemical raw materials are important basic materials and are widely applied in daily life, for example, with the increasing use amount of plastic packages, lunch boxes, expressages, cups, straws and the like, environmental pollution is more and more serious, particularly, marine environment pollution is more and more intensified, so that plastic wastes which are environmentally-friendly and cannot be naturally degraded become public hazards to natural environments including water areas.
In order to protect the environment where human beings rely on to live, biodegradable plastics such as polylactic acid derived from biological raw materials are gaining favor because the biodegradable plastics have properties close to those of common plastics, can be degraded into water and carbon dioxide again in natural environment, water area environment or composting environment after being discarded, can return to natural environment without causing secondary pollution, and can be widely used as degradable plastic bags, disposable plastic tableware, disposable plastic supplies of hotels and restaurants and express plastic packages in logistics industry.
The patent CN106189136B recommends "a modified polylactic acid composite material and its manufacturing method and application", and CN106433053B provides "a method of polylactic acid material and polylactic acid material prepared by the method", but the patents all use glass fiber as reinforcing material, have very high strength and rigidity, the deficiency is obvious, namely the glass fiber is easy to expose, the surface is rough. Chinese patent CN 103131149B adopts talcum powder and glass fiber composite reinforcement, and talcum powder is a flaky substance and has better surface quality, but the reinforcing effect is not good.
Chinese patent application nos. 201510183525.8 and 201910179923.0 mention magnesium salt whiskers, but primarily serve as flame retardants and heat stabilizers, and do not address the use of magnesium salt whiskers for reinforcement.
In view of the above situation, the present patent uses magnesium salt whiskers with high aspect ratio to reinforce the polylactic acid composite material, so as to obtain a polylactic acid composite material with high surface quality, high strength, high rigidity and full degradation.
Disclosure of Invention
The invention aims to provide a high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material with high surface quality, high strength, high rigidity and full degradation.
The invention also aims to provide a preparation method of the magnesium salt whisker fiber reinforced polylactic acid composite material with high surface quality, which can ensure the obtained high surface quality and can ensure the technical effects of high strength and high rigidity.
The invention is primarily aimed at completing the following tasks, and the magnesium salt whisker fiber reinforced polylactic acid composite material with high surface quality comprises the following raw materials in percentage by mass: 50.9-84.1% of polylactic acid, 10-30% of magnesium salt whisker, 5-15% of toughening agent, 0.1-0.3% of nucleating agent, 0.2-0.8% of lubricant, 0.1-1% of auxiliary agent and 0.5-2% of coloring agent.
A high surface quality magnesium salt whisker fiber reinforced polylactic acid composite material comprises the following raw materials in percentage by mass; 50.9 percent of polylactic acid, 30 percent of magnesium salt whisker, 15 percent of flexibilizer, 0.3 percent of nucleating agent, 0.8 percent of lubricant, 1 percent of auxiliary agent and 2 percent of colorant.
A high surface quality magnesium salt whisker fiber reinforced polylactic acid composite material comprises the following raw materials in percentage by mass; 84.1 percent of polylactic acid, 10 percent of magnesium salt whisker, 5 percent of flexibilizer, 0.1 percent of nucleating agent, 0.2 percent of lubricant, 0.1 percent of auxiliary agent and 0.5 percent of colorant.
A high surface quality magnesium salt whisker fiber reinforced polylactic acid composite material comprises the following raw materials in percentage by mass; 67.7 percent of polylactic acid, 20 percent of magnesium salt whisker, 10 percent of flexibilizer, 0.2 percent of nucleating agent, 0.6 percent of lubricant, 0.5 percent of auxiliary agent and 1 percent of colorant.
In a specific embodiment of the invention, the polylactic acid is injection molding grade L-lactide polylactic acid with a melt index of 10-30g/10min, a purity of more than 98% and a melting point of more than 160 ℃.
In another specific embodiment of the invention, the magnesium salt whisker has a molecular formula of MgSO4 & 5Mg (OH)2 & 3H2O, the average diameter of the whisker is less than 0.5 μm, the average length of the whisker is 10-20 μm, and the density of the whisker is 2.3 g/cm3The pH value is 9; the toughening agent is poly terephthalic acid-adipic acid-butanediol ester (PBAT) and/or poly adipic acid-butanediol ester (PBS); the melting index of the polybutylene terephthalate-adipate is 2-5g/10min and the melting point is 110-120 ℃, and the melting index of the polybutylene terephthalate-adipate is 4-20g/10min and the melting point is 110-120 ℃.
In another specific embodiment of the invention, the nucleating agent is one or a combination of more of superfine talcum powder with the diameter of less than 20 μm, sodium benzoate, sorbitol nucleating agent, organic sodium phosphate and potassium benzene sulfonate; the lubricant is pentaerythritol ester, fatty acid amide or alkane substance; the fatty acid amide is oleamide or ethylene bis stearamide, and the alkane substance is polyethylene wax; the auxiliary agent is a main antioxidant, an auxiliary antioxidant, hydroxybenzophenone, hydroxybenzotriazole or a metal ion passivator; the main antioxidant is an antioxidant 1010 or an antioxidant 1076; the secondary antioxidant is antioxidant 168 or phosphorous acid amide; the colorant is titanium dioxide, carbon black or carbon black master batch.
The invention also aims to complete the preparation method of the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material, which comprises the following steps:
A) preparing materials, namely taking the following raw materials in percentage by mass: 50.9-84.1% of polylactic acid, 10-30% of magnesium salt whisker, 5-15% of toughening agent, 0.1-0.3% of nucleating agent, 0.2-0.8% of lubricant, 0.1-1% of auxiliary agent and 0.5-2% of coloring agent, and drying the polylactic acid to obtain a raw material;
B) mixing, namely putting the dried polylactic acid, the toughening agent, the nucleating agent, the lubricant, the auxiliary agent and the coloring agent in the step A) into a high-speed mixer and stirring to obtain a mixture;
C) and (3) melt extrusion, namely putting the mixture obtained in the step B) into a double-screw extruder with the length-diameter ratio of 40-44: 1 and the screw diameter of 65-75 mm, melt extrusion under the conditions of controlling the rotation speed and the extrusion temperature of the screw, feeding the magnesium salt whiskers in the step A) laterally in the fifth section of the double screw in the melt extrusion process, and cooling and pelletizing the mixture after extrusion by the double-screw extruder to obtain the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material.
In another specific embodiment of the invention, the temperature of the drying in the step A) is 75-85 ℃, and the drying is carried out until the water content is less than 500 ppm; the stirring time in the step B) is 1-5 min.
In still another specific embodiment of the present invention, the screw rotation speed in step C) is controlled to 180-.
The technical scheme provided by the invention has the technical effects that: the raw materials and mass percentage of polylactic acid, magnesium salt whisker, flexibilizer, nucleating agent, lubricant, auxiliary agent and coloring agent are selected reasonably, so that the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material can be ensured to be obtained, and the composite material also has ideal heat resistance, dimensional stability, strength, rigidity and degradability, and can meet the requirements of manufacturing products such as degradable chopsticks and degradable handles by an injection molding method; because the magnesium salt whisker is an inorganic substance, the strength, the rigidity and the heat resistance of the polylactic acid can be obviously improved; because the magnesium salt whisker with smaller size is adopted, the problem of rough introduction appearance similar to glass fiber is solved, and the appearance effect of the final product is fully reflected; meanwhile, the magnesium salt whisker has a better length-diameter ratio, and the length-diameter ratio of the whisker is more than 20:1, so that compared with talc powder reinforcing agents, the rigidity and the strength of the composite material can be improved, the provided preparation method has simple process and no harsh process elements, and the obtained polylactic acid composite material can comprehensively embody the technical effects and meet the requirements of industrial amplification production.
Detailed Description
Example 1:
A) preparing materials, namely preparing the following raw materials in percentage by mass (namely in percentage by mass): 50.9 percent of polylactic acid, 30 percent of magnesium salt whisker, 15 percent of flexibilizer, 0.3 percent of nucleating agent, 0.8 percent of lubricant, 1 percent of auxiliary agent and 2 percent of coloring agent to obtain raw materials, wherein the polylactic acid is injection-grade L-lactide polylactic acid (PLLA) with the melt index of 10g/10min, the purity of more than 98 percent, the melting point of more than 160 ℃ and the water content of less than 500ppm after being dried at 85 ℃, the molecular formula of the magnesium salt whisker in the step is MgSO4 & 5Mg (OH)2 & 3H2O, the average diameter of the whisker is less than 0.5 mu m, the average length is 15 mu m, and the density is 2.3 g/cm3The pH value is 9, the toughening agent in the step is a mixture of polybutylene terephthalate-adipate-butylene glycol (PBAT) with a melt index of 2-5g/10min and a melting point of 110-120 ℃ and polybutylene adipate-butylene glycol (PBS) with a melt index of 4-20g/10min and a melting point of 110-120 ℃ which are mixed according to the same weight ratio, the nucleating agent in the step is a mixture of ultrafine talcum powder with the diameter of less than 20 mu m, sodium benzoate and sodium organophosphate which are mixed according to the same weight ratio, the lubricant in the step is pentaerythritol ester, the auxiliary agent in the step is antioxidant 1010 which is a main antioxidant (antioxidant 1076 can also be used), and the coloring agent in the step is titanium dioxide;
B) mixing, namely putting the dried L-lactide polylactic acid (PLLA) obtained in the step A), a toughening agent, a nucleating agent, a lubricant, an auxiliary agent and a coloring agent into a high-speed mixer to be mixed for 5min to obtain a mixture;
C) melt extrusion (namely screw melt extrusion), putting the mixture obtained in the step B) into a double-screw extruder with the length-diameter ratio of 40: 1 and the diameter of 65mm, melt extrusion at the screw rotation speed of 600rpm and the extrusion temperature of 200 ℃, feeding the magnesium salt whisker fiber obtained in the step A) into the double-screw extruder in the lateral direction in a fifth section (namely a fifth area) of the double screw, cooling and dicing the mixture after melt extrusion by the double-screw extruder to obtain the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material (also referred to as plastic for short), wherein the magnesium salt whisker fiber is fed into the fifth section of the double screw in the lateral direction in the step to avoid the breakage of the magnesium salt whisker fiber, thereby ensuring the length-diameter ratio of the magnesium salt whisker and providing the high strength and high modulus of the final composite material.
Example 2:
A) preparing materials, namely preparing the following raw materials in percentage by mass (namely in percentage by mass): 84.1 percent of polylactic acid, 10 percent of magnesium salt whisker, 5 percent of flexibilizer, 0.1 percent of nucleating agent, 0.2 percent of lubricant, 0.1 percent of auxiliary agent and 0.5 percent of coloring agent to obtain raw materials, wherein the polylactic acid in the step is injection molding grade L-lactide polylactic acid (PLLA) with the melt index of 30g/10min, the purity of more than 98 percent, the melting point of more than 160 ℃ and the moisture content of less than 500ppm after being dried at 80 ℃, the molecular formula of the magnesium salt whisker in the step is MgSO4 & 5Mg (OH)2 & 3H2O, the average diameter of the whisker is less than 0.5 mu m, the average length is 20 mu m, and the density is 2.3 g/cm3The pH value is 9, the toughening agent in the step is poly terephthalic acid-adipic acid-butylene glycol ester (PBAT) with the melting index of 2-5g/10min and the melting point of 110-120 ℃, the nucleating agent in the step is sorbitol nucleating agent with the diameter of below 20 μm, the lubricant in the step is oleamide, the auxiliary agent in the step is antioxidant 168 (phosphite amide can also be used), and the coloring agent in the step is carbon black;
B) mixing, namely putting the dried L-lactide polylactic acid (PLLA) obtained in the step A), a toughening agent, a nucleating agent, a lubricant, an auxiliary agent and a coloring agent into a high-speed mixer to be mixed for 1min to obtain a mixture;
C) melt extrusion (namely screw melt extrusion), putting the mixture obtained in the step B) into a double-screw extruder with the length-diameter ratio of 44: 1 and the diameter of 70mm, melt extrusion at the rotating speed of the screw of 180rpm and the extrusion temperature of 220 ℃, feeding the magnesium salt whisker fiber obtained in the step A) into the double-screw extruder in the lateral direction in a fifth section (namely a fifth area) of the double screw, cooling and granulating the mixture after melt extrusion by the double-screw extruder, and obtaining the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material (also referred to as plastic for short).
Example 3:
A) preparing materials, namely preparing the following raw materials in percentage by mass (namely in percentage by mass): 67.7% of polylactic acid, 20% of magnesium salt whisker, 10% of toughening agent, 0.2% of nucleating agent, 0.6% of lubricant, 0.5% of auxiliary agent and 1% of coloring agent to obtain a raw material, wherein the polylactic acid is injection-grade L-lactide polylactic acid (PLLA) with the melt index of 20g/10min, the purity of more than 98%, the melting point of more than 160 ℃ and the moisture content of less than 500ppm after being dried at 75 ℃, the molecular formula of the magnesium salt whisker in the step is MgSO4 & 5Mg (OH)2 & 3H2O, the average diameter of the whisker is less than 0.5 μm, the average length is 10 μm, and the density is 2.3 g/cm3The pH value is 9, the toughening agent in the step is poly (butylene adipate-co-glycol) (PBS) with the melt index of 4-20g/10min and the melting point of 110-120 ℃, the nucleating agent in the step is a mixture of potassium benzene sulfonate with the diameter of less than 20 mu m and superfine talcum powder which are mixed according to the same weight ratio, the lubricant in the step is polyethylene wax, the auxiliary agent in the step is hydroxybenzotriazole (or phosphorous acid amide can be used), and the coloring agent in the step is carbon black master batch;
B) mixing, namely putting the dried L-lactide polylactic acid (PLLA) obtained in the step A), a toughening agent, a nucleating agent, a lubricant, an auxiliary agent and a coloring agent into a high-speed mixer to be mixed for 3min to obtain a mixture;
C) melt extrusion (namely screw melt extrusion), putting the mixture obtained in the step B) into a double-screw extruder with the length-diameter ratio of 42: 1 and the diameter of 75mm, melt extrusion at the rotating speed of 400rpm and the extrusion temperature of 160 ℃, feeding the magnesium salt whisker fiber obtained in the step A) into the double-screw extruder in the lateral direction in a fifth section (namely a fifth area) of the double screw, cooling and pelletizing the mixture after melt extrusion by the double-screw extruder to obtain the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material (also referred to as plastic for short), wherein the magnesium salt whisker fiber is fed into the fifth section of the double screw in the lateral direction in the step to avoid the breakage of the magnesium salt whisker fiber, thereby ensuring the length-diameter ratio of the magnesium salt whisker and providing the high strength and high modulus of the final composite material.
Comparative example 1:
polylactic acid L130: 58 percent of
Glass fiber 534A: 30 percent of
Toughening agent PBAT TH 801T: 10.3 percent of
Nucleating agent NA-110.2%
Lubricant EBS: 0.5 percent
Primary antioxidant Irganox 1010: 0.2 percent of
Secondary antioxidant Irganox 168: 0.3 percent of
Black master CABOT-UN 20140.5%
The model of the glass fiber manufacturing company, China boulder glass fiber Co., Ltd, is 534A.
Comparative example 2:
polylactic acid L130: 63 percent of
Talc powder HYT-04C: 25 percent of
Toughening agent PBAT TH 801T: 10.3 percent of
Nucleating agent NA-110.2%
Lubricant EBS: 0.5 percent
Primary antioxidant Irganox 1010: 0.2 percent of
Secondary antioxidant Irganox 168: 0.3 percent of
Black master CABOT-UN 20140.5%
The talcum powder is HYT-04C, has silicon content of above 60%, and average particle diameter of 0.75 μm.
The data obtained by comparing examples 1 to 3 with comparative examples 1 and 2 according to the invention are shown in the following table:
Figure BDA0002928686380000061
the evaluation method comprises the following steps:
drying the particles granulated by the double screw, drying for 4-8 hours under the drying condition of 80 ℃, then putting the particles into an injection molding machine, performing injection molding by adopting an ISO 294 standard mold, and simultaneously performing surface roughness evaluation by utilizing a flat plate, wherein the evaluation is divided into three grades of good, general and rough. Other mechanical and thermal test criteria are as follows:
test items Test method
Mechanical properties
Tensile breaking strength ISO 527-1/-2
Elongation at tensile break ISO 527-1/-2
Bending strength ISO 178
Flexural modulus ISO 178
Notched izod impact strength 23 deg.c ISO 180/1eA
Thermal performance
Heat distortion temperature (0.45MPa) ISO 75
Others
Density of ISO 1183
Compared with the surface roughness, the product added with the magnesium salt whisker has higher bending modulus, lower density and good surface quality, while the glass fiber product has the highest rigidity but has rough surface. The talcum powder product has the best surface quality and is lack of rigidity. Meanwhile, the processing is relatively easy and is better implemented, so the invention solves the problems of surface quality, rigidity, toughness, heat resistance and size stabilizer of the polylactic acid product, ensures that the polylactic acid degradable plastic product can be fully applied to injection molding such as degradable chopsticks, degradable handles and the like, and greatly expands the application range of the degradable polylactic acid plastic. The manufacturing method of the invention has simple process.

Claims (10)

1. A high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material is characterized by comprising the following raw materials in percentage by mass: 50.9-84.1% of polylactic acid, 10-30% of magnesium salt whisker, 5-15% of toughening agent, 0.1-0.3% of nucleating agent, 0.2-0.8% of lubricant, 0.1-1% of auxiliary agent and 0.5-2% of coloring agent.
2. The high-surface-quality magnesium salt whisker fiber-reinforced polylactic acid composite material as claimed in claim 1, wherein the raw material composition comprises, by mass percentage; 50.9 percent of polylactic acid, 30 percent of magnesium salt whisker, 15 percent of flexibilizer, 0.3 percent of nucleating agent, 0.8 percent of lubricant, 1 percent of auxiliary agent and 2 percent of colorant.
3. The high-surface-quality magnesium salt whisker fiber-reinforced polylactic acid composite material as claimed in claim 1, wherein the raw material composition comprises, by mass percentage; 84.1 percent of polylactic acid, 10 percent of magnesium salt whisker, 5 percent of flexibilizer, 0.1 percent of nucleating agent, 0.2 percent of lubricant, 0.1 percent of auxiliary agent and 0.5 percent of colorant.
4. The high-surface-quality magnesium salt whisker fiber-reinforced polylactic acid composite material as claimed in claim 1, wherein the raw material composition comprises, by mass percentage; 67.7 percent of polylactic acid, 20 percent of magnesium salt whisker, 10 percent of flexibilizer, 0.2 percent of nucleating agent, 0.6 percent of lubricant, 0.5 percent of auxiliary agent and 1 percent of colorant.
5. The high surface quality magnesium salt whisker fiber reinforced polylactic acid composite material as claimed in any one of claims 1 to 4, wherein the polylactic acid is injection molding grade L-lactide polylactic acid having a melt index of 10-30g/10min, a purity of 98% or more and a melting point of 160 ℃ or more.
6. A high surface according to any one of claims 1 to 4The mass magnesium salt whisker fiber reinforced polylactic acid composite material is characterized in that the molecular formula of the magnesium salt whisker is MgSO4 seed, 5Mg seed, (OH)2 seed, 3H2O, the average diameter of the whisker is less than 0.5 mu m, the average length is 10-20 mu m, and the density is 2.3 g/cm3The pH value is 9; the toughening agent is poly terephthalic acid-adipic acid-butanediol ester and/or poly adipic acid-butanediol ester; the melting index of the polybutylene terephthalate-adipate is 2-5g/10min and the melting point is 110-120 ℃, and the melting index of the polybutylene terephthalate-adipate is 4-20g/10min and the melting point is 110-120 ℃.
7. The high surface quality magnesium salt whisker fiber reinforced polylactic acid composite material as claimed in any one of claims 1 to 4, wherein the nucleating agent is one or a combination of more of superfine talcum powder with the diameter of less than 20 μm, sodium benzoate, sorbitol nucleating agent, organic sodium phosphate and potassium benzene sulfonate; the lubricant is pentaerythritol ester, fatty acid amide or alkane substance; the fatty acid amide is oleamide or ethylene bis stearamide, and the alkane substance is polyethylene wax; the auxiliary agent is a main antioxidant, an auxiliary antioxidant, hydroxybenzophenone, hydroxybenzotriazole or a metal ion passivator; the main antioxidant is an antioxidant 1010 or an antioxidant 1076; the secondary antioxidant is antioxidant 168 or phosphorous acid amide; the colorant is titanium dioxide, carbon black or carbon black master batch.
8. The preparation method of the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material as claimed in claim 1, characterized by comprising the following steps:
A) preparing materials, namely taking the following raw materials in percentage by mass: 50.9-84.1% of polylactic acid, 10-30% of magnesium salt whisker, 5-15% of toughening agent, 0.1-0.3% of nucleating agent, 0.2-0.8% of lubricant, 0.1-1% of auxiliary agent and 0.5-2% of coloring agent, and drying the polylactic acid to obtain a raw material;
B) mixing, namely putting the dried polylactic acid, the toughening agent, the nucleating agent, the lubricant, the auxiliary agent and the coloring agent in the step A) into a high-speed mixer and stirring to obtain a mixture;
C) and (3) melt extrusion, namely putting the mixture obtained in the step B) into a double-screw extruder with the length-diameter ratio of 40-44: 1 and the screw diameter of 65-75 mm, melt extrusion under the conditions of controlling the rotation speed and the extrusion temperature of the screw, feeding the magnesium salt whiskers in the step A) laterally in the fifth section of the double screw in the melt extrusion process, and cooling and pelletizing the mixture after extrusion by the double-screw extruder to obtain the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material.
9. The method for preparing the high-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material according to claim 8, wherein the drying temperature in the step A) is 75-85 ℃, and the drying is carried out until the water content is less than 500 ppm; the stirring time in the step B) is 1-5 min.
10. The method for preparing the high surface quality magnesium salt whisker fiber reinforced polylactic acid composite material as claimed in claim 8, wherein the screw rotation speed is controlled to be 180-600rpm in step C), and the screw extrusion temperature is controlled to be 160-220 ℃.
CN202110141220.6A 2021-02-02 2021-02-02 High-surface-quality magnesium salt whisker fiber reinforced polylactic acid composite material and preparation method thereof Pending CN112920577A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115433450A (en) * 2022-09-30 2022-12-06 金发科技股份有限公司 Good-appearance glass mineral composite reinforced PC alloy composition and preparation method and application thereof
WO2023145665A1 (en) * 2022-01-25 2023-08-03 宇部マテリアルズ株式会社 Biodegradable resin composition, molded article, and production method for biodegradable resin composition

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102585462A (en) * 2011-12-08 2012-07-18 汕头卜高通美实业有限公司 Heat-resistant polylactic acid composite material and preparation method thereof
CN105462193A (en) * 2014-09-03 2016-04-06 东北林业大学 Whisker reinforced biodegradable polyester composite material and preparation method
CN105820522A (en) * 2016-04-01 2016-08-03 安徽理工大学 Calcium sulfate whisker reinforced and toughened polylactic acid composite and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102585462A (en) * 2011-12-08 2012-07-18 汕头卜高通美实业有限公司 Heat-resistant polylactic acid composite material and preparation method thereof
CN105462193A (en) * 2014-09-03 2016-04-06 东北林业大学 Whisker reinforced biodegradable polyester composite material and preparation method
CN105820522A (en) * 2016-04-01 2016-08-03 安徽理工大学 Calcium sulfate whisker reinforced and toughened polylactic acid composite and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
袁瑞登: "无机填料改性聚乳酸的研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023145665A1 (en) * 2022-01-25 2023-08-03 宇部マテリアルズ株式会社 Biodegradable resin composition, molded article, and production method for biodegradable resin composition
CN115433450A (en) * 2022-09-30 2022-12-06 金发科技股份有限公司 Good-appearance glass mineral composite reinforced PC alloy composition and preparation method and application thereof
CN115433450B (en) * 2022-09-30 2024-03-22 金发科技股份有限公司 Glass-ore composite reinforced PC alloy composition with good appearance, and preparation method and application thereof

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