CN108948703B - Weather-resistant degradable plastic bottle and preparation method thereof - Google Patents
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- 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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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08L2203/00—Applications
- C08L2203/10—Applications used for bottles
Abstract
The invention discloses a weather-resistant degradable plastic bottle and a preparation method thereof, wherein the weather-resistant degradable plastic bottle comprises the following components in parts by weight: 50-70 parts of polylactic acid, 15-25 parts of attapulgite/polymethyl methacrylate hybrid particles, 1-5 parts of nano titanium dioxide, 1-5 parts of nano zinc oxide, 5-10 parts of glass fiber, 0.01-1 part of plasticizer and 0.05-1.2 parts of compatilizer. The plastic bottle prepared by the invention is environment-friendly and degradable, can be applied outdoors and is subjected to climate tests, the mechanical property and weather resistance of polylactic acid are improved by introducing the modified attapulgite grafted polymethyl methacrylate, and meanwhile, the plastic bottle added with the nano particles has the excellent characteristics of ultraviolet resistance, sterilization, antifouling property and the like.
Description
Technical Field
The invention relates to the technical field of plastic product production, in particular to a weather-resistant degradable plastic bottle.
Background
The polylactic acid is pollution-free in the production process, and the product can be biodegraded to realize circulation in nature, so that the polylactic acid is an ideal green high polymer material. However, the pure polylactic acid resin has slow crystallization speed, large shrinkage rate of a molded product, poor dimensional stability, brittle material, poor processing thermal stability and the like, and the application of the pure polylactic acid resin as engineering plastic is limited. Meanwhile, plastic products are easily affected by external conditions such as sunlight irradiation, temperature change, wind, rain and the like, a series of aging phenomena such as color fading, color change, cracking, pulverization, strength reduction and the like occur, and in addition, the breeding of bacteria also affects the storage of food.
In recent decades, a great deal of research has been carried out on modified polylactic acid materials filled with attapulgite, and the nano effect of the attapulgite causes the attapulgite to exist in larger rod crystal aggregates, which is not beneficial to improving the system performance when the attapulgite is directly added, so that the modification of the surface performance by chemical means is a commonly used modification means.
Polymethyl methacrylate (PMMA) is an important thermoplastic which is developed earlier, has better transparency, chemical stability and weather resistance, is heterodyeing, is easy to process, has beautiful appearance and is widely applied to the building industry. A PMMA molecular chain is grafted to the surface of the attapulgite single rod crystal, so that a rudiment particle of a hybrid material can be obtained, the agglomeration phenomenon of the attapulgite rod crystal in a polymer is effectively improved, and the nanoscale dispersion is realized.
The nano particles are novel multifunctional inorganic materials, the nano titanium dioxide and the nano zinc oxide can sterilize for a long time under the action of ultraviolet rays in light, and the killing rate of the nano titanium dioxide and the nano zinc oxide on black variant spores of bacillus subtilis, pseudomonas aeruginosa, escherichia coli, staphylococcus aureus, salmonella, mycobacterium dentis and aspergillus all reaches more than 98 percent; the physical shielding type ultraviolet protective agent can absorb ultraviolet rays, reflect and scatter the ultraviolet rays and transmit visible light, has excellent performance and has great development prospect.
The invention of Chinese patent 201610931603.2 relates to an attapulgite/polylactic acid nanocomposite and a preparation method thereof, and the prepared attapulgite/polylactic acid nanocomposite has greatly improved performance and wide application prospect in the fields of biodegradable films, sheets, injection molding and packaging materials. However, the attapulgite has poor dispersibility in polylactic acid, hardly achieves the maximum reinforcing effect, has no ultraviolet resistance and has poor weather resistance.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a weather-resistant degradable plastic bottle and a preparation method thereof.
The weather-resistant degradable plastic bottle comprises the following raw materials in parts by weight:
50-70 parts of polylactic acid, 15-25 parts of attapulgite/polymethyl methacrylate hybrid particles, 1-5 parts of nano titanium dioxide, 1-5 parts of nano zinc oxide, 5-10 parts of glass fiber, 0.01-1 part of plasticizer and 0.05-1.2 parts of compatilizer.
The purity and the particle size of the attapulgite and the polymerization degree of the polymethyl methacrylate influence the composition of the plastic bottle raw material, so that the mechanical property, the light transmittance and the weather resistance of the polylactic acid composite material are influenced.
The particle size of the attapulgite is 30-100 mu m, and the attapulgite is purified attapulgite.
The preparation method of the weather-resistant degradable plastic bottle comprises the following preparation steps: the purification method of the attapulgite comprises the following steps: dissolving 1 part of sodium pyrophosphate in 100 parts of deionized water, adding 20 parts of attapulgite, stirring for 1h at 30-60 ℃, standing for a period of time, taking the upper suspension, adding HCl solution, and stirring for 1h at 30-60 ℃. And (4) performing centrifugal separation, washing with water to be neutral, and drying to obtain purified attapulgite.
The preparation method of the weather-resistant degradable plastic bottle comprises the following preparation steps: the preparation method of the attapulgite/polymethyl methacrylate hybrid particle comprises the following steps: (1) adding an aminosilane coupling agent solution into a certain amount of purified attapulgite, stirring for 2h at 50 ℃, washing with alcohol and water respectively, and drying to obtain the aminated and modified attapulgite. (2) Adding a certain amount of xylene, methyl methacrylate and an initiator into the modified attapulgite, performing ultrasonic dispersion for 10-20min, magnetically stirring for 3-5h at 80 ℃ in a nitrogen environment, washing and drying after the reaction is finished, thereby obtaining the attapulgite/polymethyl methacrylate hybrid particles.
Through carrying out amination modification on the attapulgite, the modifier is adsorbed on the surface of the attapulgite to form a coating layer on the surface, so that the surface tension is reduced, and the agglomeration among particles is reduced. For the modified attapulgite, an initiator is used for initiating active sites, and a surface graft polymerization method is adopted for grafting polymethyl methacrylate, so that the tensile resistance and the aging resistance of the material are improved.
The weather-resistant degradable plastic bottle disclosed by the invention is further preferably composed of the following raw materials in parts by weight: 60 parts of polylactic acid, 20 parts of attapulgite/polymethyl methacrylate hybrid particles, 3 parts of nano titanium dioxide, 2 parts of nano zinc oxide, 5 parts of glass fiber, 0.02 part of plasticizer and 0.1 part of compatilizer.
The particle size of the nano titanium dioxide is 30-100nm, the crystal form of the nano titanium dioxide is anatase, and the particle size of the nano zinc oxide is 30-100 nm.
The nano particles selected by the invention have small size and high activity, can reflect and scatter ultraviolet rays and absorb ultraviolet rays, thereby having stronger barrier capability to the ultraviolet rays, and simultaneously effectively killing harmful bacteria to play antibacterial and bacteriostatic effects.
The plasticizer is one or two of glycerol triacetate, citrate ether, fatty acid ester ether and ethylene glycol monobutyl ether acetate.
Although the plasticizer is added in a small amount in the invention, the dispersion condition of each component in the compounding process can be improved, the connectivity among the components can be increased, and the mechanical property of the composite material can be improved.
The compatilizer is one of octadecyl ammonium bromide, p-hydroxybenzoate, diisocyanate and o-hydroxybenzoic acid methyl ester.
The compatilizer selected by the invention can improve the dispersibility of attapulgite/polymethyl methacrylate hybrid particles and nano particles in polylactic acid and prevent the particles from agglomerating.
The concentration of the hydrochloric acid solution is 1-3 mol/L.
The aminosilane coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, N-beta (aminoethyl) -gamma-aminopropylmethyldimethoxysilane and gamma-aminopropylmethyldiethoxysilane.
The silane coupling agent can adjust the interaction between the attapulgite and the methyl methacrylate, and improve the dispersibility and the polymerization degree of particles in the polymerization process, thereby improving the comprehensive performance of the polylactic acid composite material.
The mass ratio of the purified attapulgite, the xylene, the methyl methacrylate to the initiator is 3-8: 50: 10-15: 0.5-2, wherein the initiator is an azo initiator.
The preparation method of the weather-resistant degradable plastic bottle comprises the following steps:
adding polylactic acid, attapulgite/polymethyl methacrylate hybrid particles, nano titanium dioxide, nano zinc oxide, glass fiber, a plasticizer and a compatilizer into a high-speed mixer according to the parts by weight, uniformly mixing, extruding at the temperature of 190 plus materials and 240 ℃ by using a double-screw extruder, and finally performing blow molding to obtain the weather-resistant degradable plastic bottle.
The weather-resistant degradable plastic bottle prepared by adopting the technical scheme has the following advantages:
1. the modified attapulgite grafted polymethyl methacrylate used in the invention is compounded with polylactic acid, so that the weather resistance and the mechanical property of the polylactic acid are greatly improved.
2. According to the invention, the nano titanium dioxide and the zinc oxide as well as the anatase type nano titanium dioxide and the nano zinc oxide are added into the raw materials, so that the plastic bottle has the functions of peculiar smell elimination, antibiosis and bacteriostasis, and has absorption and barrier properties on ultraviolet rays, and the ultraviolet ray resistance, aging resistance and other properties of the polylactic acid plastic bottle are improved.
Detailed Description
The following examples are further illustrative of the present invention.
Example 1
A weather-resistant degradable plastic bottle is prepared by the following steps:
(1) dissolving 1 part of sodium pyrophosphate in 100 parts of deionized water, adding 20 parts of attapulgite, stirring for 1h at 30-60 ℃, standing for a period of time, taking the upper suspension, adding HCl solution, and stirring for 1h at 30-60 ℃. Performing centrifugal separation, washing with water to be neutral, and drying to obtain purified attapulgite;
(2) adding a gamma-aminopropyltriethoxysilane solution into the purified attapulgite obtained in the step (1), stirring for 2h at 50 ℃, washing with alcohol and water for three times respectively, and drying to obtain aminated and modified attapulgite;
(3) adding a certain amount of xylene, methyl methacrylate and an initiator into the modified attapulgite obtained in the step (2), performing ultrasonic dispersion for 10-20min, performing magnetic stirring for 3-5h at 80 ℃ in a nitrogen environment, washing and drying after the reaction is finished to obtain attapulgite/polymethyl methacrylate hybrid particles, wherein the mass ratio of the purified attapulgite, xylene, methyl methacrylate to the initiator is 3: 50: 10: 0.5;
(4) weighing 15 parts by weight of the attapulgite/polymethyl methacrylate hybrid particles obtained in the step (3), 50 parts by weight of polylactic acid, 1 part by weight of nano titanium dioxide, 1 part by weight of nano zinc oxide, 5 parts by weight of glass fiber, 0.01 part by weight of glycerol triacetate and 0.05 part by weight of octadecyl ammonium bromide, adding into a high-speed mixer, uniformly mixing, extruding by adopting a double-screw extruder at the temperature of 190 plus materials and 240 ℃, and finally performing blow molding to obtain the weather-resistant degradable plastic bottle.
Example 2
A weather-resistant degradable plastic bottle is prepared by the following steps:
(1) dissolving 1 part of sodium pyrophosphate in 100 parts of deionized water, adding 20 parts of attapulgite, stirring for 1h at 30-60 ℃, standing for a period of time, taking the upper suspension, adding HCl solution, and stirring for 1h at 30-60 ℃. Performing centrifugal separation, washing with water to be neutral, and drying to obtain purified attapulgite;
(2) adding an aminosilane coupling agent solution into the purified attapulgite obtained in the step (1), stirring for 2h at 50 ℃, washing with alcohol and water for three times respectively, and drying to obtain aminated and modified attapulgite;
(3) adding a certain amount of xylene, methyl methacrylate and an initiator into the modified attapulgite obtained in the step (2), performing ultrasonic dispersion for 10-20min, performing magnetic stirring for 3-5h at 80 ℃ in a nitrogen environment, washing and drying after the reaction is finished to obtain attapulgite/polymethyl methacrylate hybrid particles, wherein the mass ratio of the purified attapulgite, xylene, methyl methacrylate to the initiator is 4: 50: 12: 0.7;
(4) weighing 20 parts by weight of the attapulgite/polymethyl methacrylate hybrid particles obtained in the step (3), 55 parts by weight of polylactic acid, 2 parts by weight of nano titanium dioxide, 1 part by weight of nano zinc oxide, 6 parts by weight of glass fiber, 0.03 part by weight of plasticizer and 0.07 part by weight of compatilizer, adding the obtained mixture into a high-speed mixer, uniformly mixing, extruding the mixture by adopting a double-screw extruder at the temperature of 190 plus material and 240 ℃, and finally performing blow molding to obtain the weather-resistant degradable plastic bottle.
Example 3
A weather-resistant degradable plastic bottle is prepared by the following steps:
(1) dissolving 1 part of sodium pyrophosphate in 100 parts of deionized water, adding 20 parts of attapulgite, stirring for 1h at 30-60 ℃, standing for a period of time, taking the upper suspension, adding HCl solution, and stirring for 1h at 30-60 ℃. Performing centrifugal separation, washing with water to be neutral, and drying to obtain purified attapulgite;
(2) adding an N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane solution into the purified attapulgite obtained in the step (1), stirring for 2h at 50 ℃, washing with alcohol and water for three times respectively, and drying to obtain the aminated and modified attapulgite;
(3) adding a certain amount of xylene, methyl methacrylate and an initiator into the modified attapulgite obtained in the step (2), performing ultrasonic dispersion for 10-20min, performing magnetic stirring for 3-5h at 80 ℃ in a nitrogen environment, washing and drying after the reaction is finished to obtain attapulgite/polymethyl methacrylate hybrid particles, wherein the mass ratio of the purified attapulgite, xylene, methyl methacrylate to the initiator is 5: 50: 14: 0.8;
(4) weighing 15 parts by weight of the attapulgite/polymethyl methacrylate hybrid particles obtained in the step (3), 60 parts by weight of polylactic acid, 3 parts by weight of nano titanium dioxide, 2 parts by weight of nano zinc oxide, 7 parts by weight of glass fiber, 0.03 part by weight of plasticizer and 0.08 part by weight of compatilizer, adding the obtained mixture into a high-speed mixer, uniformly mixing, extruding the mixture by adopting a double-screw extruder at the temperature of 190 plus material and 240 ℃, and finally performing blow molding to obtain the weather-resistant degradable plastic bottle.
Example 4
A weather-resistant degradable plastic bottle is prepared by the following steps:
(1) dissolving 1 part of sodium pyrophosphate in 100 parts of deionized water, adding 20 parts of attapulgite, stirring for 1h at 30-60 ℃, standing for a period of time, taking the upper suspension, adding HCl solution, and stirring for 1h at 30-60 ℃. Performing centrifugal separation, washing with water to be neutral, and drying to obtain purified attapulgite;
(2) adding a gamma-aminopropyl methyl diethoxy silane solution into the purified attapulgite obtained in the step (1), stirring for 2 hours at 50 ℃, washing with alcohol and water for three times respectively, and drying to obtain aminated and modified attapulgite;
(3) adding a certain amount of xylene, methyl methacrylate and an initiator into the modified attapulgite obtained in the step (2), performing ultrasonic dispersion for 10-20min, performing magnetic stirring for 3-5h at 80 ℃ in a nitrogen environment, washing and drying after the reaction is finished to obtain attapulgite/polymethyl methacrylate hybrid particles, wherein the mass ratio of the purified attapulgite, xylene, methyl methacrylate to the initiator is 6: 50: 15: 1.2;
(4) weighing 15 parts by weight of the attapulgite/polymethyl methacrylate hybrid particles obtained in the step (3), 65 parts by weight of polylactic acid, 3 parts by weight of nano titanium dioxide, 3 parts by weight of nano zinc oxide, 8 parts by weight of glass fiber, 0.05 part by weight of plasticizer and 0.09 part by weight of compatilizer, adding the obtained mixture into a high-speed mixer, uniformly mixing, extruding the mixture by adopting a double-screw extruder at the temperature of 190 plus material and 240 ℃, and finally performing blow molding to obtain the weather-resistant degradable plastic bottle.
Comparative example 1
A weather-resistant degradable plastic bottle is prepared by the following steps:
weighing 60 parts of polylactic acid, 3 parts of nano titanium dioxide, 2 parts of nano zinc oxide, 7 parts of glass fiber, 0.03 part of plasticizer and 0.08 part of compatilizer according to the parts by weight, adding the materials into a high-speed mixer, uniformly mixing, extruding into an embryo at the temperature of 190 plus materials and 240 ℃ by adopting a double-screw extruder, and finally performing blow molding to obtain the weather-resistant degradable plastic bottle.
Comparative example 2
A weather-resistant degradable plastic bottle is prepared by the following steps:
(1) dissolving 1 part of sodium pyrophosphate in 100 parts of deionized water, adding 20 parts of attapulgite, stirring for 1h at 30-60 ℃, standing for a period of time, taking the upper suspension, adding HCl solution, and stirring for 1h at 30-60 ℃. Performing centrifugal separation, washing with water to be neutral, and drying to obtain purified attapulgite;
(2) adding an N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane solution into the purified attapulgite obtained in the step (1), stirring for 2h at 50 ℃, washing with alcohol and water for three times respectively, and drying to obtain the aminated and modified attapulgite;
(3) adding a certain amount of xylene, methyl methacrylate and an initiator into the modified attapulgite obtained in the step (2), performing ultrasonic dispersion for 10-20min, performing magnetic stirring for 3-5h at 80 ℃ in a nitrogen environment, washing and drying after the reaction is finished to obtain attapulgite/polymethyl methacrylate hybrid particles, wherein the mass ratio of the purified attapulgite, xylene, methyl methacrylate to the initiator is 5: 50: 14: 0.8;
(4) weighing 15 parts by weight of the attapulgite/polymethyl methacrylate hybrid particles obtained in the step (3), 60 parts by weight of polylactic acid, 7 parts by weight of glass fiber, 0.03 part by weight of plasticizer and 0.08 part by weight of compatilizer, adding the obtained mixture into a high-speed mixer, uniformly mixing, extruding the mixture by adopting a double-screw extruder at the temperature of 190 ℃ and 240 ℃, and finally performing blow molding to obtain the weather-resistant degradable plastic bottle.
Comparative example 3
A weather-resistant degradable plastic bottle is prepared by the following steps:
weighing 60 parts of polylactic acid, 7 parts of glass fiber, 0.03 part of plasticizer and 0.08 part of compatilizer according to the parts by weight, adding the materials into a high-speed mixer, uniformly mixing, extruding at 240 ℃ by adopting a double-screw extruder, and finally performing blow molding to obtain the weather-resistant degradable plastic bottle.
The test specimens were exposed to UV light using the plastic UV light exposure test method ASTM D4329-05 and observed for aging at various time periods (Table 1).
TABLE 1 Effect of UV irradiation on aging of plastics (UV intensity 3000 uW/cm)2)
The tensile strength, elongation at break and impact strength are tested according to GB/T1040-1992, GB/T1040.1-2006 and GB/T1043-1993, and the antibacterial performance of the test sample is tested by using JC/T897-2014 improved method, and the results are shown in Table 2:
TABLE 2
As can be seen from tables 1 and 2, the degradable polylactic acid composite materials prepared in examples 1 to 4 have better mechanical properties and aging resistance, and the ultraviolet resistance, tensile strength, impact strength and antibacterial property of the composite materials are correspondingly increased with the increase of the contents of the hybrid particles and the nanoparticles. From comparative examples 1 to 3, it is understood that the composite material was degraded in all properties when no hybrid particles or nanoparticles were added, and had no antibacterial property when no nanoparticles were added.
Claims (5)
1. A weather-resistant degradable plastic bottle is characterized in that: the material composition comprises, by weight, 50-70 parts of polylactic acid, 15-25 parts of attapulgite/polymethyl methacrylate hybrid particles, 1-5 parts of nano titanium dioxide, 1-5 parts of nano zinc oxide, 5-10 parts of glass fiber, 0.01-1 part of plasticizer and 0.05-1.2 parts of compatilizer;
the particle size of the attapulgite is 10-50 μm, the attapulgite is purified attapulgite, and the purification method of the attapulgite comprises the following steps: dissolving sodium pyrophosphate in deionized water, adding attapulgite, stirring at 30-60 ℃ for 1-2h, standing for a period of time, taking an upper suspension, adding HCl solution, stirring at 30-60 ℃ for 1h, performing centrifugal separation, washing with water to neutrality, and drying to obtain purified attapulgite;
(1) adding an aminosilane coupling agent solution into a certain amount of purified attapulgite, stirring for 2h at 50 ℃, washing with alcohol and water respectively, and drying to obtain aminated and modified attapulgite; (2) adding a certain amount of xylene, methyl methacrylate and an initiator into the modified attapulgite, performing ultrasonic dispersion for 10-20min, performing magnetic stirring for 3-5h at 80 ℃ in a nitrogen environment, washing and drying after the reaction is finished to obtain attapulgite/polymethyl methacrylate hybrid particles;
the particle size of the nano titanium dioxide is 30-100nm, and the crystal form of the nano titanium dioxide is anatase;
the plasticizer is one or more of glycerol triacetate, citrate ether, fatty acid ester ether and ethylene glycol monobutyl ether acetate;
the concentration of the hydrochloric acid solution is 1-3 mol/L.
2. A weather-resistant, degradable plastic bottle according to claim 1, wherein: the compatilizer is one or more of octadecyl ammonium bromide, p-hydroxybenzoate, diisocyanate and o-hydroxybenzoate.
3. A weather-resistant, degradable plastic bottle according to claim 1, wherein: the amino silane coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, N-beta (aminoethyl) -gamma-aminopropylmethyldimethoxysilane or gamma-aminopropylmethyldiethoxysilane.
4. The weather-resistant degradable plastic bottle of claim 1, wherein: the mass ratio of the purified attapulgite, xylene, methyl methacrylate to the initiator is 3-8: 50: 10-15: 0.5-2, wherein the initiator is an azo initiator.
5. A method of producing the weather-resistant degradable plastic bottle as claimed in any one of claims 1 to 4, wherein: the preparation method comprises the following steps: adding polylactic acid, attapulgite/polymethyl methacrylate hybrid particles, nano titanium dioxide, nano zinc oxide, glass fiber, a plasticizer and a compatilizer into a high-speed mixer according to the parts by weight, uniformly mixing, extruding at the temperature of 190 plus materials and 240 ℃ by using a double-screw extruder, and finally performing blow molding to obtain the weather-resistant degradable plastic bottle.
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