CN114716800A - Modified polylactic acid and preparation method thereof - Google Patents
Modified polylactic acid and preparation method thereof Download PDFInfo
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- CN114716800A CN114716800A CN202210340949.0A CN202210340949A CN114716800A CN 114716800 A CN114716800 A CN 114716800A CN 202210340949 A CN202210340949 A CN 202210340949A CN 114716800 A CN114716800 A CN 114716800A
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/325—Calcium, strontium or barium phosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/24—Crystallisation aids
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Biological Depolymerization Polymers (AREA)
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Abstract
The invention discloses a modified polylactic acid and a preparation method thereof, wherein the modified polylactic acid comprises the following raw materials in parts by weight: 60-80 parts of granular polylactic acid, 1-10 parts of plasticizing modifier, 1.5-10 parts of nucleating agent, 0.5-5 parts of thermal decomposition stabilizer, 0.5-5 parts of heat stabilizer and 5-10 parts of toughening agent; the plasticizing modifier is a mixture of citric acid esters, glucose ether, oligomer polyethylene glycol glycerol, sorbitol and fatty acid ether, and comprises the following components in percentage by weight: 10-50% of citrate, 5-15% of glucose ether, 30-40% of oligomer polyethylene glycol glycerol, 2-5% of glycerol, 8-10% of sorbitol and 3-10% of fatty acid ether. The modified polylactic acid and the preparation method thereof synchronously complete toughening modification and heat-resistant modification of the polylactic acid, obviously improve the flexibility and heat resistance of the polylactic acid, have stronger elasticity and flexibility, and can be applied to occasions with high and stable requirements on mechanical properties.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to modified polylactic acid and a preparation method thereof.
Background
Polylactic acid is a polyester, and lactic acid is a biomonomer that occurs in nature. Polylactic acid is thermoplastic and can be processed by common plastic processing techniques to form films, sheets, and fibers. Polylactic acid is soft and hard.
The polylactic acid is transparent, but can be made into opaque material, and can be added with filler. Due to its high strength, it can be made into very thin sheets. The polylactic acid is insoluble in water and has good water resistance and oil resistance.
In terms of performance, polylactic acid in the prior art has poor toughness, is hard and brittle, is easy to break when bent, and has insufficient elasticity and flexibility; in addition, the heat resistance is poor, and the performance of the PLA product is greatly reduced, so that the single polylactic acid cannot be applied to the occasions with high and stable requirements on mechanical properties.
Disclosure of Invention
The present invention is directed to a modified polylactic acid and a method for preparing the same, which solve the problems of the background art mentioned above.
In order to achieve the purpose, the invention provides the following technical scheme: the modified polylactic acid comprises the following raw materials in parts by weight: 60-80 parts of granular polylactic acid, 1-10 parts of plasticizing modifier, 1.5-10 parts of nucleating agent, 0.5-5 parts of thermal decomposition stabilizer, 0.5-5 parts of heat stabilizer and 5-10 parts of toughening agent;
the plasticizing modifier is a mixture of citric acid esters, glucose ether, oligomer polyethylene glycol glycerol, sorbitol and fatty acid ether, and comprises the following components in percentage by weight: 10-50% of citrate, 5-15% of glucose ether, 30-40% of oligomer polyethylene glycol glycerol, 2-5% of glycerol, 8-10% of sorbitol and 3-10% of fatty acid ether.
Preferably, the nucleating agent is a blend of talcum powder, nano-clay, carbon nano-tube, nano-calcium carbonate, starch, lignin, cellulose and cyclodextrin, and the nucleating agent comprises the following components in percentage by weight: 10-40% of talcum powder, 20-30% of nano clay, 5-10% of carbon nano tube, 3-5% of nano calcium carbonate, 10-20% of starch, 5-10% of lignin, 5-8% of cellulose and 5-8% of cyclodextrin.
Preferably, the thermal decomposition stabilizer is phyllosilicate, calcium carbonate and hydroxyapatite, and the thermal decomposition stabilizer comprises the following components in percentage by weight: 15-30% of layered silicate, 20-50% of calcium carbonate and 10-30% of hydroxyapatite.
Preferably, the phyllosilicate is kaolin, montmorillonite or a copolymerized blend of the first two.
Preferably, the heat stabilizer is cellulose, wood powder and coconut shell powder, and the heat stabilizer comprises the following components in percentage by weight: 15-30% of cellulose, 30-50% of wood powder and 20-45% of coconut shell powder.
Preferably, the toughening agent is polycaprolactone, polybutylene succinate, polybutylene adipate terephthalate, polybutylene succinate-adipate, and the toughening agent comprises the following components in percentage by weight: 20-30% of polycaprolactone, 10-30% of polybutylene succinate, 8-20% of polybutylene adipate terephthalate and 20-50% of polybutylene succinate-adipate-butylene glycol.
Preferably, the polylactic acid is poly L-lactic acid, poly DL-lactic acid or a copolymer blend of the two, the number average molecular weight of the polylactic acid is 5-50 ten thousand, and the particle size of the polylactic acid is 0.2-0.6 cm.
A preparation method of modified polylactic acid, which is used for modifying polylactic acid, comprises the following steps:
s1 preprocessing of polylactic acid
Processing granular polylactic acid through a single-screw film casting machine to cast a film with the thickness of 0.1mm-0.2mm for standby;
s2, reprocessing of polylactic acid film
Cutting and crushing the polylactic acid film sheet by a crusher to obtain sheet-shaped polylactic acid for later use;
s2, mixing and processing
Adding a plasticizing modifier, a nucleating agent, a thermal decomposition stabilizer, a heat stabilizer and a toughening agent into a high-speed stirring mixer, starting the high-speed stirring mixer to uniformly mix the plasticizing modifier, the nucleating agent, the thermal decomposition stabilizer, the heat stabilizer and the toughening agent to obtain a mixture A, adding the flaky polylactic acid into the high-speed stirring mixer, starting the high-speed stirring mixer again to uniformly mix the flaky polylactic acid and the modified mixture to obtain a mixture B after the mixture is completely mixed, taking out the mixture B, and drying and cooling the mixture for later use;
s2 melt processing
And adding the mixture B into a double-screw extruder for melt blending, after melt blending, bracing, cooling with water, cutting the particles, and drying the particles at 50-60 ℃ to remove excessive moisture to obtain the modified polylactic acid material.
The invention has the technical effects and advantages that: the modified polylactic acid and the preparation method thereof synchronously complete toughening modification and heat-resistant modification of the polylactic acid, obviously improve the flexibility and heat resistance of the polylactic acid, reduce the occurrence of fracture conditions during bending, have stronger elasticity and flexibility, enable the polylactic acid to be produced in batches and popularized, and can be applied to occasions with high and stable requirements on mechanical properties.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment,
The modified polylactic acid and the preparation method thereof comprise the following raw materials in parts by weight: 65 parts of granular polylactic acid, 5 parts of plasticizing modifier, 8 parts of nucleating agent, 2 parts of thermal decomposition stabilizer, 3 parts of heat stabilizer and 7 parts of toughening agent;
specifically, the polylactic acid is poly-L-lactic acid, poly-DL-lactic acid or a copolymer blend of the two, the number average molecular weight of the polylactic acid is 45 ten thousand, and the particle size of the polylactic acid is 0.3 cm.
Specifically, the plasticizing modifier is a mixture of citric acid esters, glucose ether, oligomer polyethylene glycol glycerol, sorbitol and fatty acid ether, and the plasticizing modifier comprises the following components in percentage by weight: 40% of citric acid esters, 10% of glucose ether, 30% of oligomer polyethylene glycol glycerol, 3% of glycerol, 9% of sorbitol and 8% of fatty acid ether.
Specifically, the nucleating agent is a blend of talcum powder, nano-clay, carbon nano-tube, nano-calcium carbonate, starch, lignin, cellulose and cyclodextrin, and the nucleating agent comprises the following components in percentage by weight: 30% of talcum powder, 25% of nano clay, 8% of carbon nano tube, 4% of nano calcium carbonate, 13% of starch, 8% of lignin, 6% of cellulose and 6% of cyclodextrin.
Specifically, the thermal decomposition stabilizer is phyllosilicate, calcium carbonate and hydroxyapatite, the phyllosilicate is kaolin, montmorillonite or a copolymerization blend of the two, and the thermal decomposition stabilizer comprises the following components in percentage by weight: 25% of layered silicate, 50% of calcium carbonate and 25% of hydroxyapatite.
Specifically, the heat stabilizer is cellulose, wood powder and coconut shell powder, and the heat stabilizer comprises the following components in percentage by weight: 20% of cellulose, 40% of wood powder and 40% of coconut shell powder.
Specifically, the toughening agent is polycaprolactone, polybutylene succinate, polybutylene adipate terephthalate, polybutylene succinate-adipate-butylene glycol, and the toughening agent comprises the following components in percentage by weight: 25% of polycaprolactone, 25% of polybutylene succinate, 10% of polybutylene adipate terephthalate and 40% of polybutylene succinate-adipate-butylene glycol.
Example II,
The modified polylactic acid and the preparation method thereof comprise the following raw materials in parts by weight: 75 parts of granular polylactic acid, 5 parts of plasticizing modifier, 6 parts of nucleating agent, 4 parts of thermal decomposition stabilizer, 3 parts of heat stabilizer and 7 parts of toughening agent;
specifically, the polylactic acid is poly-L-lactic acid, poly-DL-lactic acid or a copolymer blend of the two, the number average molecular weight of the polylactic acid is 43 ten thousand, and the particle size of the polylactic acid is 0.5 cm.
Specifically, the plasticizing modifier is a mixture of citric acid esters, glucose ether, oligomer polyethylene glycol glycerol, sorbitol and fatty acid ether, and the plasticizing modifier comprises the following components in percentage by weight: 45% of citric acid esters, 10% of glucose ether, 30% of oligomer polyethylene glycol glycerol, 3% of glycerol, 9% of sorbitol and 3% of fatty acid ether.
Specifically, the nucleating agent is a blend of talcum powder, nano-clay, carbon nano-tube, nano-calcium carbonate, starch, lignin, cellulose and cyclodextrin, and the nucleating agent comprises the following components in percentage by weight: 25% of talcum powder, 25% of nano clay, 6.5% of carbon nano tube, 3.5% of nano calcium carbonate, 17% of starch, 8% of lignin, 7.5% of cellulose and 7.5% of cyclodextrin.
Specifically, the thermal decomposition stabilizer is phyllosilicate, calcium carbonate and hydroxyapatite, the phyllosilicate is kaolin, montmorillonite or a copolymer blend of the two, and the thermal decomposition stabilizer comprises the following components in percentage by weight: 25% of layered silicate, 50% of calcium carbonate and 25% of hydroxyapatite.
Specifically, the heat stabilizer is cellulose, wood powder and coconut shell powder, and the heat stabilizer comprises the following components in percentage by weight: 25% of cellulose, 45% of wood powder and 30% of coconut shell powder.
Specifically, the toughening agent is polycaprolactone, polybutylene succinate, polybutylene adipate terephthalate, polybutylene succinate-adipate-butylene glycol, and the toughening agent comprises the following components in percentage by weight: 25% of polycaprolactone, 25% of polybutylene succinate, 15% of polybutylene adipate-terephthalate and 35% of polybutylene succinate-adipate-butanediol.
Example III,
The modified polylactic acid and the preparation method thereof comprise the following raw materials in parts by weight: 65 parts of granular polylactic acid, 9 parts of plasticizing modifier, 6 parts of nucleating agent, 5 parts of thermal decomposition stabilizer, 5 parts of heat stabilizer and 10 parts of toughening agent.
Example four,
The modified polylactic acid and the preparation method thereof comprise the following raw materials in parts by weight: 74 parts of granular polylactic acid, 6 parts of plasticizing modifier, 8 parts of nucleating agent, 2 parts of thermal decomposition stabilizer, 3 parts of heat stabilizer and 7 parts of toughening agent.
A preparation method of modified polylactic acid, which is used for modifying polylactic acid, comprises the following steps:
s1 preprocessing of polylactic acid
Processing granular polylactic acid by a single-screw casting film machine to cast a film with the thickness of 0.1mm-0.2mm for standby;
s2, reprocessing of polylactic acid film
Cutting and crushing the polylactic acid film sheet by a crusher to obtain sheet-shaped polylactic acid for later use;
s2, mixing and processing
Adding a plasticizing modifier, a nucleating agent, a thermal decomposition stabilizer, a heat stabilizer and a toughening agent into a high-speed stirring mixer, starting the high-speed stirring mixer to uniformly mix the plasticizing modifier, the nucleating agent, the thermal decomposition stabilizer, the heat stabilizer and the toughening agent to obtain a mixture A, adding the flaky polylactic acid into the high-speed stirring mixer, starting the high-speed stirring mixer again to uniformly mix the flaky polylactic acid and the modified mixture to obtain a mixture B after the mixture is completely mixed, taking out the mixture B, and drying and cooling the mixture for later use;
s2 melt processing
And adding the mixture B into a double-screw extruder for melt blending, after melt blending, bracing, cooling with water, cutting the particles, and drying the particles at 50-60 ℃ to remove excessive moisture to obtain the modified polylactic acid material.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still make modifications to the technical solutions described in the foregoing embodiments, or make equivalent substitutions and improvements to part of the technical features of the foregoing embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The modified polylactic acid is characterized by comprising the following raw materials in parts by weight: 60-80 parts of granular polylactic acid, 1-10 parts of plasticizing modifier, 1.5-10 parts of nucleating agent, 0.5-5 parts of thermal decomposition stabilizer, 0.5-5 parts of heat stabilizer and 5-10 parts of toughening agent;
the plasticizing modifier is a mixture of citric acid esters, glucose ether, oligomer polyethylene glycol glycerol, sorbitol and fatty acid ether, and comprises the following components in percentage by weight: 10-50% of citrate, 5-15% of glucose ether, 30-40% of oligomer polyethylene glycol glycerol, 2-5% of glycerol, 8-10% of sorbitol and 3-10% of fatty acid ether.
2. The modified polylactic acid according to claim 1, wherein: the nucleating agent is a blend of talcum powder, nano clay, carbon nano tubes, nano calcium carbonate, starch, lignin, cellulose and cyclodextrin, and the nucleating agent comprises the following components in percentage by weight: 10-40% of talcum powder, 20-30% of nano clay, 5-10% of carbon nano tube, 3-5% of nano calcium carbonate, 10-20% of starch, 5-10% of lignin, 5-8% of cellulose and 5-8% of cyclodextrin.
3. The modified polylactic acid according to claim 1, wherein: the thermal decomposition stabilizer is layered silicate, calcium carbonate and hydroxyapatite, and comprises the following components in percentage by weight: 15-30% of layered silicate, 20-50% of calcium carbonate and 10-30% of hydroxyapatite.
4. A modified polylactic acid according to claim 3, wherein: the phyllosilicate is kaolin, montmorillonite or a copolymer blend of the first two.
5. The modified polylactic acid according to claim 1, wherein: the heat stabilizer comprises cellulose, wood powder and coconut shell powder, and comprises the following components in percentage by weight: 15-30% of cellulose, 30-50% of wood flour and 20-45% of coconut shell powder.
6. The modified polylactic acid according to claim 1, wherein: the toughening agent is polycaprolactone, polybutylene succinate, polybutylene adipate terephthalate and polybutylene succinate-adipate, and comprises the following components in percentage by weight: 20-30% of polycaprolactone, 10-30% of polybutylene succinate, 8-20% of polybutylene adipate terephthalate and 20-50% of polybutylene succinate-adipate-butylene glycol.
7. The modified polylactic acid according to claim 1, wherein: the polylactic acid is poly L-lactic acid, poly DL-lactic acid or the copolymer blend of the two, the number average molecular weight is 5-50 ten thousand, and the particle size of the polylactic acid is 0.2-0.6 cm.
8. A method for producing a modified polylactic acid, which is used for the modified polylactic acid according to any one of claims 1 to 7, characterized by comprising the steps of:
s1 preprocessing of polylactic acid
Processing granular polylactic acid by a single-screw casting film machine to cast a film with the thickness of 0.1mm-0.2mm for standby;
s2, reprocessing of polylactic acid film
Cutting and crushing the polylactic acid film sheet by a crusher to obtain sheet polylactic acid for later use;
s2, mixing and processing
Adding a plasticizing modifier, a nucleating agent, a thermal decomposition stabilizer, a heat stabilizer and a toughening agent into a high-speed stirring mixer, starting the high-speed stirring mixer to uniformly mix the plasticizing modifier, the nucleating agent, the thermal decomposition stabilizer, the heat stabilizer and the toughening agent to obtain a mixture A, adding the flaky polylactic acid into the high-speed stirring mixer, starting the high-speed stirring mixer again to uniformly mix the flaky polylactic acid and the modified mixture to obtain a mixture B, taking out the mixture B, and drying and cooling the mixture for later use;
s2 melt processing
And adding the mixture B into a double-screw extruder for melt blending, after melt blending, bracing, cooling with water, cutting the particles, and drying the particles at 50-60 ℃ to remove excessive moisture to obtain the modified polylactic acid material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210340949.0A CN114716800A (en) | 2022-04-02 | 2022-04-02 | Modified polylactic acid and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210340949.0A CN114716800A (en) | 2022-04-02 | 2022-04-02 | Modified polylactic acid and preparation method thereof |
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| CN202210340949.0A Withdrawn CN114716800A (en) | 2022-04-02 | 2022-04-02 | Modified polylactic acid and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115109398A (en) * | 2022-07-15 | 2022-09-27 | 江苏中科睿赛污染控制工程有限公司 | Reinforced and toughened degradable material and preparation method thereof |
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2022
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115109398A (en) * | 2022-07-15 | 2022-09-27 | 江苏中科睿赛污染控制工程有限公司 | Reinforced and toughened degradable material and preparation method thereof |
| CN115109398B (en) * | 2022-07-15 | 2023-11-21 | 江苏中科睿赛污染控制工程有限公司 | Reinforced and toughened degradable material and preparation method thereof |
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Application publication date: 20220708 |