CN112898747B - Preparation method of degradable polylactic acid tableware with strong moisture absorption resistance - Google Patents
Preparation method of degradable polylactic acid tableware with strong moisture absorption resistance Download PDFInfo
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- CN112898747B CN112898747B CN202110095321.4A CN202110095321A CN112898747B CN 112898747 B CN112898747 B CN 112898747B CN 202110095321 A CN202110095321 A CN 202110095321A CN 112898747 B CN112898747 B CN 112898747B
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- polylactic acid
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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
- 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
- C08L2201/06—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
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
Abstract
The invention discloses a preparation method of degradable polylactic acid tableware with strong hygroscopicity resistance, which comprises the following steps: (1) Sequentially adding the coconut shell powder, the nano silicon oxide dispersion liquid and the aspartic acid-lysine copolymer into a mixing and stirring machine, and stirring at a high speed to obtain modified coconut shell powder; (2) Adding a lubricant into the hot melt adhesive binder, and uniformly mixing and stirring to obtain a hot melt adhesive binder-lubricant mixture; (3) Respectively carrying out vacuum drying treatment on polylactic acid and modified coconut shell powder, then adding the polylactic acid, the modified coconut shell powder, a hot melt adhesive-lubricant mixture, a cross-linking agent and an antioxidant into a torque rheometer for blending, and then carrying out compression molding on the mixture in a flat vulcanizing machine to obtain the degradable polylactic acid tableware. The degradable polylactic acid tableware prepared by the invention overcomes the defect of poor moisture resistance and humidity resistance of polylactic acid tableware products in the prior art, and does not wrinkle or crack after being soaked in water for a long time.
Description
Technical Field
The invention belongs to the technical field of polylactic acid material preparation, and particularly relates to a preparation method of degradable polylactic acid tableware with strong moisture absorption resistance.
Background
Plastic tableware is called disposable tableware market by its advantages of light weight, low price and good mechanical property, however, it brings serious plastic white pollution while facilitating people's life, and the disposable foamed plastic tableware can produce 16 toxins when meeting hot soup and hot rice, and when using foamed tableware or plastic bag to contain the hot oil bar, the toxins are melted in the food by accident. Until now, many pollution-free disposable tableware products have been available, and they can be broadly classified into two categories, i.e., photodegradation and biodegradation, wherein the biodegradation includes synthetic polymers and natural polymers, and the latter includes natural products as main raw materials, and starch plastics, paper tableware and cellulose tableware are mainly used at present.
Polylactic acid (PLA) is obtained by polycondensation of lactic acid produced by fermentation of starch or ring-opening polymerization of dimer lactide. Lactic acid (2-hydroxypropionic acid), which is a constituent unit of PLA, has an optically active property because it has an asymmetric carbon atom in the molecule, and thus has two optical isomers, D-or L-lactic acid. The properties of PLA depend on optical rotation, processing temperature, annealing time and molecular weight. For example, pure poly-L-lactic acid has a crystallinity of about 60%, a glass transition temperature of 60 ℃, a melting point of 180 ℃, a tensile strength of more than 70MPa, and a tensile modulus of more than 3GPa, and has good rigidity and strength, but has an elongation at break of only about 3%, and is liable to brittle fracture. PLA is a compostable, biodegradable and renewable thermoplastic 'green' high polymer material, but the large-scale application of PLA in the tableware field is limited by the low heat distortion temperature, high brittleness, insufficient barrier property and the like of PLA. In the prior art, some organic or inorganic powder materials such as bamboo powder are adopted to reinforce the polylactic acid material, and the reinforced polylactic acid material can effectively solve the existing problems, but in practical application, the polylactic acid material still has the defect of poor moisture resistance and humidity resistance, and after the polylactic acid material is soaked in water for too long time, the phenomena of surface wrinkling and poor mechanical property can occur, so that the quality of the polylactic acid material is seriously influenced.
Disclosure of Invention
The invention aims to make up the defect that the current polylactic acid material has poor moisture resistance and humidity resistance, and provides a preparation method of degradable polylactic acid tableware with strong moisture absorption resistance.
The invention is realized by the following technical scheme.
A preparation method of degradable polylactic acid tableware with strong moisture absorption resistance comprises the following steps:
(1) Sequentially adding the coconut shell powder, the nano silicon oxide dispersion liquid and the aspartic acid-lysine copolymer into a mixing stirrer, and stirring at a high speed for 2-3 hours to obtain modified coconut shell powder;
(2) Heating a hot melt adhesive to 65-75 ℃ before use, adding a lubricant, uniformly mixing and stirring, and carrying out heat preservation treatment for 2-3 hours to obtain a hot melt adhesive-lubricant mixture, wherein the hot melt adhesive is prepared from an ethylene-vinyl acetate-vinyl alcohol terpolymer and guar gum according to a mass ratio of 1;
(3) Respectively carrying out vacuum drying treatment on polylactic acid and modified coconut shell powder for 28-32 hours, then adding the polylactic acid, the modified coconut shell powder, a hot melt adhesive-lubricant mixture, a cross-linking agent and an antioxidant into a torque rheometer for blending, and then carrying out compression molding in a flat vulcanization instrument to obtain the degradable polylactic acid tableware, wherein the addition mass ratio of the polylactic acid to the modified coconut shell powder to the hot melt adhesive-lubricant mixture is 55-65.
Specifically, in the step (1), the mass fraction of the nano silicon oxide dispersion liquid is 10-20%, and the solvent of the nano silicon oxide dispersion liquid is absolute ethyl alcohol.
Specifically, in the step (1), the mass ratio of the coconut shell powder, the nano silicon oxide dispersion liquid and the aspartic acid-lysine copolymer is 15-20.
Specifically, in the step (1), the rotation speed during high-speed stirring is 750 to 850r/min, and the temperature in the cylinder of the mixing and stirring machine during high-speed stirring is set to be 45 to 55 ℃.
Specifically, in the step (2), the lubricant is a wood-plastic lubricant TPW604, and the adding amount of the lubricant is 5-10% of the mass of the hot melt adhesive.
Specifically, in the step (3), the crosslinking agent is any one of tri-n-butyl citrate and tert-butyl peroxy-2-ethylhexyl carbonate.
Specifically, the antioxidant is pentaerythritol tetrapropionate.
Specifically, in the step (3), the temperature during blending is 175-185 ℃, and the rotor speed is 120-150r/min.
Specifically, in the step (3), the temperature during compression molding is 180-190 ℃, the pressure during compression molding is 8-12MPa, and the hot pressing time is 2-4min.
According to the technical scheme, the beneficial effects of the invention are as follows:
the degradable polylactic acid tableware with strong moisture absorption resistance prepared by the method disclosed by the invention is wide in application, can be applied to preparation of dinner plates, bowls, dishes, convenient tableware, cups and the like, can realize complete biodegradation, is green and environment-friendly, and the prepared tableware product has excellent mechanical properties, effectively improves the quality of the tableware, particularly overcomes the defect that the polylactic acid tableware product in the prior art is poor in moisture resistance and humidity resistance, and does not wrinkle or crack after being soaked in water for a long time. According to the modified coconut shell powder prepared in the step (1), after the modified coconut shell powder is treated by the nano silicon oxide dispersion liquid, the physical adsorption effect between the modified coconut shell powder and the polylactic acid material can be effectively improved, so that the adhesion of a modified coconut shell powder-polylactic acid interface is effectively improved, various mechanical properties of the polylactic acid tableware are finally improved, and meanwhile, the waterproof and moisture-resistant properties of the polylactic acid tableware are also improved to a certain extent; the aspartic acid-lysine copolymer and the hot melt adhesive have the function of jointly preventing water from entering a modified coconut shell powder-polylactic acid interface, so that the moisture resistance and humidity resistance of the polylactic acid tableware are effectively improved.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.
Example 1
A preparation method of degradable polylactic acid tableware with strong moisture absorption resistance comprises the following steps:
(1) Sequentially adding coconut shell powder, a nano silicon oxide dispersion liquid with the mass fraction of 10% and an aspartic acid-lysine copolymer into a mixing and stirring machine according to the mass ratio of 15 to 1, and performing high-speed stirring treatment for 2 hours to obtain modified coconut shell powder, wherein the solution solvent of the nano silicon oxide dispersion liquid is absolute ethyl alcohol, the rotating speed during high-speed stirring is 750r/min, and the temperature in a cylinder of the mixing and stirring machine during high-speed stirring is set to 45 ℃;
(2) Heating a hot melt adhesive to 65 ℃ before use, adding a lubricant, uniformly mixing and stirring, and carrying out heat preservation treatment for 2 hours to obtain a hot melt adhesive-lubricant mixture, wherein the hot melt adhesive is prepared from an ethylene-vinyl acetate-vinyl alcohol terpolymer and guar gum according to a mass ratio of 1;
(3) Respectively carrying out vacuum drying treatment on polylactic acid and modified coconut shell powder for 28 hours, then adding the polylactic acid, the modified coconut shell powder, a hot melt adhesive-lubricant mixture, a cross-linking agent and an antioxidant into a torque rheometer for blending, wherein the temperature during blending is 175 ℃, the rotating speed of a rotor is 120r/min, then carrying out compression molding on a flat vulcanizing instrument to obtain the degradable polylactic acid tableware, the temperature during compression molding is 180 ℃, the pressure during compression molding is 8MPa, and the hot pressing time is 2min, wherein the adding mass ratio of the polylactic acid, the modified coconut shell powder and the hot melt adhesive-lubricant mixture is 55.8, the adding amount of the cross-linking agent is 0.01 percent of the mass of the polylactic acid, the adding amount of the antioxidant is 0.01 percent of the mass of the polylactic acid, the cross-linking agent is tri-n-butyl citrate, and the antioxidant is pentaerythritol tetrapropionate.
Example 2
A preparation method of degradable polylactic acid tableware with strong moisture absorption resistance comprises the following steps:
(1) Sequentially adding the coconut shell powder, the nano silicon oxide dispersion liquid with the mass fraction of 15% and the aspartic acid-lysine copolymer into a mixing and stirring machine according to the mass ratio of 18 to 1, and performing high-speed stirring treatment for 2.5 hours to obtain modified coconut shell powder, wherein the solution solvent of the nano silicon oxide dispersion liquid is absolute ethyl alcohol, the rotating speed during high-speed stirring is 800r/min, and the temperature in a cylinder of the mixing and stirring machine during high-speed stirring is set to be 50 ℃;
(2) Heating a hot melt adhesive to 70 ℃ before use, adding a lubricant, uniformly mixing and stirring, and carrying out heat preservation treatment for 2.5 hours to obtain a hot melt adhesive-lubricant mixture, wherein the hot melt adhesive is prepared from an ethylene-vinyl acetate-vinyl alcohol terpolymer and guar gum according to a mass ratio of 1;
(3) Respectively carrying out vacuum drying treatment on polylactic acid and modified coconut shell powder for 30 hours, then adding the polylactic acid, the modified coconut shell powder, a hot melt adhesive-lubricant mixture, a cross-linking agent and an antioxidant into a torque rheometer for blending, wherein the temperature during blending is 180 ℃, the rotating speed of a rotor is 130r/min, then carrying out compression molding in a flat vulcanizing instrument to obtain the degradable polylactic acid tableware, the temperature during compression molding is 185 ℃, the pressure during compression molding is 10MPa, and the hot pressing time is 3min, wherein the addition mass ratio of the polylactic acid, the modified coconut shell powder, the hot melt adhesive-lubricant mixture is 60.2.
Example 3
A preparation method of degradable polylactic acid tableware with strong moisture absorption resistance comprises the following steps:
(1) Sequentially adding coconut shell powder, nano silicon oxide dispersion liquid with the mass fraction of 20% and aspartic acid-lysine copolymer into a mixing and stirring machine according to the mass ratio of 20;
(2) Heating a hot melt adhesive to 75 ℃ before use, adding a lubricant, uniformly mixing and stirring, and carrying out heat preservation treatment for 3 hours to obtain a hot melt adhesive-lubricant mixture, wherein the hot melt adhesive is prepared from an ethylene-vinyl acetate-vinyl alcohol terpolymer and guar gum according to a mass ratio of 1;
(3) Respectively carrying out vacuum drying treatment on polylactic acid and modified coconut shell powder for 32 hours, then adding the polylactic acid, the modified coconut shell powder, a hot melt adhesive-lubricant mixture, a cross-linking agent and an antioxidant into a torque rheometer for blending, wherein the temperature during blending is 185 ℃, the rotating speed of a rotor is 150r/min, then carrying out compression molding on a flat vulcanizing instrument to obtain the degradable polylactic acid tableware, the temperature during compression molding is 190 ℃, the pressure during compression molding is 12MPa, and the hot pressing time is 4min, wherein the adding mass ratio of the polylactic acid, the modified coconut shell powder and the hot melt adhesive-lubricant mixture is 65.3, the adding amount of the cross-linking agent is 0.03 percent of the mass of the polylactic acid, the adding amount of the antioxidant is 0.03 percent of the mass of the polylactic acid, the cross-linking agent is tri-n-butyl citrate, and the antioxidant is pentaerythritol tetrapropionate.
Comparative example 1
The operation steps in step (1) were completely the same as in example 1 except that the nano-silica dispersion was not added.
Comparative example 2
The aspartic acid-lysine copolymer was not added in step (1), and the remaining procedure was exactly the same as in example 2.
Comparative example 3
In the step (2), the ethylene-vinyl acetate-vinyl alcohol terpolymer in the hot melt adhesive was replaced with an equal amount of guar gum, and the remaining operation steps were exactly the same as in example 3.
Degradable polylactic acid tableware was prepared by the methods of examples and comparative examples, respectively, and then tested for various mechanical properties and water resistance, the test results are shown in table 1,
TABLE 1 degradable polylactic acid tableware Performance test
In addition, in the experiment, it is found that after 5 days of the soaking treatment, the surfaces of the degradable polylactic acid tableware prepared in each proportion have more wrinkling phenomena, and the surfaces of the degradable polylactic acid tableware prepared in the examples have no obvious change.
As can be seen from the data in Table 1, in example 1 and comparative example 1, the modified coconut husk powder prepared in step (1) of the present invention can effectively improve various mechanical properties of the polylactic acid tableware, and simultaneously improve the water resistance and moisture resistance of the polylactic acid tableware to a certain extent; as can be seen from the data of example 2 and comparative example 2 and the data of example 3 and comparative example 3, the aspartic acid-lysine copolymer and the hot melt adhesive have the function of preventing water from entering the modified coconut husk powder-polylactic acid interface, so that the moisture resistance and humidity resistance of the polylactic acid tableware are effectively improved.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. 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.
Claims (9)
1. A preparation method of degradable polylactic acid tableware with strong moisture absorption resistance is characterized by comprising the following steps:
(1) Sequentially adding the coconut shell powder, the nano silicon oxide dispersion liquid and the aspartic acid-lysine copolymer into a mixing and stirring machine, and stirring at a high speed for 2-3 hours to obtain modified coconut shell powder;
(2) Heating a hot melt adhesive to 65-75 ℃ before use, adding a lubricant, uniformly mixing and stirring, and carrying out heat preservation treatment for 2-3 hours to obtain a hot melt adhesive-lubricant mixture, wherein the hot melt adhesive is prepared from an ethylene-vinyl acetate-vinyl alcohol terpolymer and guar gum according to a mass ratio of 1;
(3) Respectively carrying out vacuum drying treatment on polylactic acid and modified coconut shell powder for 28-32 hours, then adding the polylactic acid, the modified coconut shell powder, a hot melt adhesive-lubricant mixture, a cross-linking agent and an antioxidant into a torque rheometer for blending, and then carrying out compression molding in a flat vulcanization instrument to obtain the degradable polylactic acid tableware, wherein the addition mass ratio of the polylactic acid to the modified coconut shell powder to the hot melt adhesive-lubricant mixture is 55-65.
2. The method for preparing degradable polylactic acid tableware having high moisture absorption resistance according to claim 1, wherein in the step (1), the mass fraction of the nano-silica dispersion is 10 to 20%, and the solvent of the nano-silica dispersion is absolute ethyl alcohol.
3. The method for preparing degradable polylactic acid tableware with strong moisture absorption resistance according to claim 1, wherein in the step (1), the mass ratio of the coconut shell powder, the nano silicon oxide dispersion and the aspartic acid-lysine copolymer is 15-20.
4. The method for preparing degradable polylactic acid tableware having high moisture absorption resistance according to claim 1, wherein in the step (1), the rotation speed during high-speed stirring is 750 to 850 rpm, and the temperature in the cylinder of the mixer/blender during high-speed stirring is set to 45 to 55 ℃.
5. The method for preparing degradable polylactic acid tableware having high moisture absorption resistance according to claim 1, wherein in the step (2), the lubricant is wood plastic lubricant TPW604, and the amount of the lubricant added is 5 to 10% of the mass of the hot melt adhesive.
6. The method for preparing degradable polylactic acid tableware having high moisture absorption resistance according to claim 1, wherein the crosslinking agent in the step (3) is any one of tri-n-butyl citrate and t-butyl peroxy-2-ethylhexyl carbonate.
7. The method for preparing degradable polylactic acid tableware having high moisture absorption resistance according to claim 1, wherein the antioxidant is pentaerythritol tetrapropionate.
8. The method for preparing degradable polylactic acid tableware having high moisture absorption resistance according to claim 1, wherein the blending temperature in the step (3) is 175-185 ℃ and the rotor speed is 120-150r/min.
9. The method for preparing degradable polylactic acid tableware with strong moisture absorption resistance according to claim 1, wherein in the step (3), the temperature for compression molding is 180-190 ℃, the pressure for compression molding is 8-12MPa, and the hot pressing time is 2-4min.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002069303A (en) * | 2000-08-31 | 2002-03-08 | O Masaru | Molding of vegetable fiber resin |
| CN101602884A (en) * | 2009-06-25 | 2009-12-16 | 浙江海正生物材料股份有限公司 | A kind of heat-resistance polylactic acid composite material and preparation method thereof |
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| CN113292759B (en) * | 2021-06-22 | 2022-02-25 | 运鸿集团股份有限公司 | Preparation method of low-cost biological full-degradable plant fiber starch tableware |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002069303A (en) * | 2000-08-31 | 2002-03-08 | O Masaru | Molding of vegetable fiber resin |
| CN101602884A (en) * | 2009-06-25 | 2009-12-16 | 浙江海正生物材料股份有限公司 | A kind of heat-resistance polylactic acid composite material and preparation method thereof |
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