CN109553941B - Bio-based fully-degradable chopstick material and preparation method thereof - Google Patents

Bio-based fully-degradable chopstick material and preparation method thereof Download PDF

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CN109553941B
CN109553941B CN201811367310.1A CN201811367310A CN109553941B CN 109553941 B CN109553941 B CN 109553941B CN 201811367310 A CN201811367310 A CN 201811367310A CN 109553941 B CN109553941 B CN 109553941B
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CN109553941A (en
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周文强
顾伟军
刘桂刚
何坤鹏
何晓峰
成士安
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Guangdong Zhongsu Degradation Material Co ltd
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    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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    • C08L2205/24Crystallisation aids

Abstract

The invention relates to the technical field of chopstick materials, in particular to a bio-based fully-degradable chopstick material and a preparation method thereof, wherein the chopstick material comprises L-PLA, mineral powder, glass fiber, a biodegradation accelerator, a lubricant and a nucleating agent, the invention takes the L-PLA as a base resin, the mineral powder and the glass powder are added for enhancing and modifying, the tensile property and the impact resistance of the PLA material are effectively improved, the degradation property of the PLA material can be further accelerated after the biodegradation accelerator is added, carbon dioxide and water are finally generated under the condition of natural degradation and participate in the photosynthesis of plants, the environment is not polluted, the full degradation effect can be achieved, and the degradation residual weight rate after 8 months can be reduced to be below 11.4%.

Description

Bio-based fully-degradable chopstick material and preparation method thereof
Technical Field
The invention relates to the technical field of chopstick materials, in particular to a bio-based fully-degradable chopstick material and a preparation method thereof.
Background
The problems of environmental deterioration, resource shortage and the like are increasingly highlighted worldwide, and the problems of environmental pollution and resource waste caused by ecological solid wastes are increasingly serious. With the development of economy and the continuous improvement of the living standard of people, the discharge amount of solid wastes is increased rapidly. It is estimated that about 100 hundred million tons of solid waste are newly added in the world every year, and 2 tons are added in the world. The growing solid waste brings great challenges to the human living environment and becomes one of the main factors of environmental pollution.
Polylactic acid (PLA) is a biodegradable plastic with the best comprehensive property developed in recent years, has no pollution to the environment, has good biodegradability, can be completely degraded by microorganisms in the nature after being used, finally generates carbon dioxide and water, does not pollute the environment, and meets the requirement of the current world on environmental protection; however, polylactic acid has problems of slow crystallization, small ester bond energy in a molecular chain, and easy breakage, which causes low thermal deformation temperature, low impact strength, poor toughness, and the like.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a bio-based fully-degradable chopstick material which is good in mechanical and physical properties and degradation performance, and the invention also aims to provide a preparation method of the bio-based chopstick material, which is simple in preparation process, high in subsequent forming speed and beneficial to industrial production.
The purpose of the invention is realized by the following technical scheme:
a bio-based fully-degradable chopstick material comprises the following raw materials in parts by weight:
Figure BDA0001868918570000011
Figure BDA0001868918570000021
according to the invention, L-PLA is used as a base resin, mineral powder and glass powder are added for enhancement and modification, so that the tensile property and the impact resistance of the PLA material are effectively improved, and the degradation property of the PLA material can be further accelerated after a biodegradation accelerator is added, carbon dioxide and water are finally generated under the condition of natural degradation and participate in the photosynthesis of plants, so that the environment is not polluted, the full degradation effect can be achieved, and the degradation residual weight rate after 8 months can be reduced to be below 11.4%.
Preferably, the feed comprises the following raw materials in parts by weight:
Figure BDA0001868918570000022
wherein the melt index of the L-PLA is 8-10 g/10min, the test condition is 210 ℃/2.16kg, the glass transition temperature is 60-65 ℃, and the crystallization temperature is 155-160 ℃.
Wherein the melt index of the D-PLA is 2-8 g/10min, the test condition is 210 ℃/2.16kg, the glass transition temperature is 55-60 ℃, and the crystallization temperature is 155-160 ℃.
The L-PLA has better rigidity performance than the D-PLA generally, but the L-PLA selected by the invention has better toughness and processing flowability, can realize the improvement of tensile property, bending property and impact strength by being blended with the selected D-PLA, and still has better biodegradability.
The mineral powder is one or more of talcum powder, calcium carbonate and kaolin, and the mesh number of the mineral powder is 3000-10000 meshes.
Generally speaking, the inorganic modified materials at present tend to be nano materials, which can significantly improve the mechanical properties of the materials, while the mineral powder adopted by the invention is in the range of 3000-10000 meshes and is micron-sized, so that the matrix resin with specific physical properties of the invention has better compatibility, is more significant in the improvement degree of the mechanical properties, and has lower cost. Preferably, the mineral powder is 5000 mesh calcium carbonate and/or 3000 mesh talc. The 5000-mesh calcium carbonate is easily dispersed in the matrix resin, and the 3000-mesh talcum powder has partial nucleating effect on PLA and can improve the fluidity of the whole material. Further preferably, the mineral powder consists of 5000-mesh calcium carbonate and 3000-mesh talcum powder according to the weight ratio of 2-3:1, and the improvement on the mechanical property is large.
Wherein the diameter of the glass fiber is 13-17 μm, and the linear density is 1000-2000 g/km. The glass fiber can effectively improve the mechanical property of the PLA material and improve the anti-warping property of the PLA material, and the glass fiber selected by the invention has better dispersibility in the PLA and can not generate the phenomenon of stress concentration.
Wherein the biodegradation accelerator is one or more of calcium dihydrogen phosphate, potassium dihydrogen phosphate and grafted butyl acrylate. The grafted butyl acrylate is specifically n-butyl methacrylate BMA produced by LG company in Korea, the selected biodegradation accelerator can be rapidly decomposed into free radicals in soil, and the free radicals can promote the molecular chains of PLA, PBAT and PCL to be broken, so that the degradation time of the matrix resin is greatly shortened. Further preferably, the biodegradation accelerator consists of calcium dihydrogen phosphate and potassium dihydrogen phosphate in a weight ratio of 1:1, and the degradability of the matrix resin formed by compounding L-PLA and D-PLA is improved to a more remarkable extent.
Wherein the lubricant is one or more of pentaerythritol stearate, zinc stearate and calcium stearate. The lubricant can enhance the processing fluidity of each material, and is beneficial to the uniform mixing and extrusion granulation of each material in the melting process. Preferably, the lubricant is pentaerythritol stearate and/or calcium stearate, the pentaerythritol stearate can play a role in lubrication by being used alone, but slight precipitation exists, the surface is too bright, and the calcium stearate effectively plays a role in extinction, so that the precipitation of the pentaerythritol stearate is reduced. Further preferably, the lubricant consists of pentaerythritol stearate and calcium stearate in a weight ratio of 2:1, and the preferred lubricant can greatly improve the processing fluidity of the composite material and also basically prevent the precipitation phenomenon of pentaerythritol stearate.
Wherein, the nucleating agent is one or more than one of inorganic phyllosilicate, nano silicon dioxide and 1,3, 5-benzene tricarboxyamide. The nucleating agent accelerates the crystallization rate, increases the crystallization density and promotes the grain size to be micronized by changing the crystallization behavior of the resin, thereby achieving the physical and mechanical properties of shortening the molding period, improving the transparency, the surface gloss, the tensile strength, the rigidity, the heat distortion temperature, the impact resistance, the creep resistance and the like of the product. Preferably, the nucleating agent is inorganic layered silicate and/or organic 1,3, 5-benzene tricarboxamide, the inorganic layered silicate refines the crystalline grains of the PLA and increases the strength, and the organic 1,3, 5-benzene tricarboxamide can enable the PLA to be rapidly crystallized and shorten the forming period.
The preparation method of the bio-based fully-degradable chopstick material is characterized by comprising the following steps: the method comprises the following steps:
(1) measuring L-PLA and D-PLA according to a formula amount, and mixing for 2-4 min at a rotating speed of 300-500 r/min to obtain a first mixture;
(2) adding mineral powder, a lubricant and a nucleating agent into the first mixture, and mixing at a rotating speed of 500-800 r/min for 5-10 min to obtain a second mixture;
(3) adding a biodegradation accelerator into the second mixture, heating to 60-90 ℃, and mixing at a rotating speed of 800-1000 r/min for 6-10 min to obtain a third mixture;
(4) and adding the third mixture from a main feeding port of an extruder, adding glass fiber from a side feeding port of the extruder, and performing melt extrusion at the temperature of 170-200 ℃ to obtain the bio-based fully-degradable chopstick material.
The invention has the beneficial effects that: according to the invention, L-PLA is used as a base resin, mineral powder and glass powder are added for enhancement and modification, so that the tensile property and the impact resistance of the PLA material are effectively improved, and the degradation property of the PLA material can be further accelerated after a biodegradation accelerator is added, carbon dioxide and water are finally generated under the condition of natural degradation and participate in the photosynthesis of plants, so that the environment is not polluted, the full degradation effect can be achieved, and the degradation residual weight rate after 8 months can be reduced to be below 11.4%.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
A bio-based fully-degradable chopstick material comprises the following raw materials in parts by weight:
Figure BDA0001868918570000051
wherein the melt index of the L-PLA is 9g/10min, the test conditions are 210 ℃/2.16kg, the glass transition temperature is 62 ℃, and the crystallization temperature is 157 ℃.
Wherein the melt index of the D-PLA is 5g/10min, the test conditions are 210 ℃/2.16kg, the glass transition temperature is 57 ℃, and the crystallization temperature is 157 ℃.
Wherein the mineral powder is talcum powder, and the mesh number of the mineral powder is 3000 meshes.
Wherein the diameter of the glass fiber is 13 μm, and the linear density is 1000 g/km.
Wherein the biodegradation accelerator is calcium dihydrogen phosphate.
Wherein the lubricant is pentaerythritol stearate.
Wherein the nucleating agent is inorganic layered silicate.
The preparation method of the bio-based fully-degradable chopstick material is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing L-PLA and D-PLA according to a formula amount, and mixing for 3min at a rotating speed of 400r/min to obtain a first mixture;
(2) adding mineral powder, a lubricant and a nucleating agent into the first mixture, and mixing at a rotating speed of 650r/min for 7.5min to obtain a second mixture;
(3) adding a biodegradation accelerator into the second mixture, heating to 75 ℃, and mixing at a rotating speed of 900r/min for 8min to obtain a third mixture;
(4) and adding the third mixture from a main feeding port of an extruder, adding the glass fiber from a side feeding port of the extruder, and performing melt extrusion at 185 ℃ to obtain the bio-based fully-degradable chopstick material.
Example 2
A bio-based fully-degradable chopstick material comprises the following raw materials in parts by weight:
Figure BDA0001868918570000061
wherein the melt index of the L-PLA is 9g/10min, the test conditions are 210 ℃/2.16kg, the glass transition temperature is 62 ℃, and the crystallization temperature is 157 ℃.
Wherein the mineral powder is calcium carbonate, and the mesh number of the mineral powder is 5000 meshes.
Wherein the diameter of the glass fiber is 14 μm, and the linear density is 1200 g/km.
Wherein the biodegradation accelerator is potassium dihydrogen phosphate.
Wherein the lubricant is zinc stearate.
Wherein the nucleating agent is nano silicon dioxide.
The preparation method of the bio-based fully-degradable chopstick material is characterized by comprising the following steps: the method comprises the following steps:
(1) measuring L-PLA according to a formula amount, and mixing for 3min at a rotating speed of 400r/min to obtain a first mixture;
(2) adding mineral powder, a lubricant and a nucleating agent into the first mixture, and mixing at a rotating speed of 650r/min for 7.5min to obtain a second mixture;
(3) adding a biodegradation accelerator into the second mixture, heating to 75 ℃, and mixing at a rotating speed of 900r/min for 8min to obtain a third mixture;
(4) and adding the third mixture from a main feeding port of an extruder, adding the glass fiber from a side feeding port of the extruder, and performing melt extrusion at 185 ℃ to obtain the bio-based fully-degradable chopstick material.
Example 3
A bio-based fully-degradable chopstick material comprises the following raw materials in parts by weight:
Figure BDA0001868918570000071
wherein the melt index of the L-PLA is 9g/10min, the test conditions are 210 ℃/2.16kg, the glass transition temperature is 62 ℃, and the crystallization temperature is 157 ℃.
Wherein the melt index of the D-PLA is 5g/10min, the test conditions are 210 ℃/2.16kg, the glass transition temperature is 57 ℃, and the crystallization temperature is 157 ℃.
Wherein the mineral powder is kaolin, and the mesh number of the mineral powder is 8000 meshes.
Wherein the diameter of the glass fiber is 17 μm, and the linear density is 2000 g/km.
Wherein the biodegradation accelerator is grafted butyl acrylate.
Wherein the lubricant is calcium stearate.
Wherein the nucleating agent is 1,3, 5-benzene tricarboxyamide.
The preparation method of the bio-based fully-degradable chopstick material is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing L-PLA and D-PLA according to a formula amount, and mixing for 3min at a rotating speed of 400r/min to obtain a first mixture;
(2) adding mineral powder, a lubricant and a nucleating agent into the first mixture, and mixing at a rotating speed of 650r/min for 7.5min to obtain a second mixture;
(3) adding a biodegradation accelerator into the second mixture, heating to 75 ℃, and mixing at a rotating speed of 900r/min for 8min to obtain a third mixture;
(4) and adding the third mixture from a main feeding port of an extruder, adding the glass fiber from a side feeding port of the extruder, and performing melt extrusion at 185 ℃ to obtain the bio-based fully-degradable chopstick material.
Example 4
This example differs from example 1 in that:
the mineral powder consists of 5000-mesh calcium carbonate and 3000-mesh talcum powder according to the weight ratio of 2.5: 1.
Example 5
This example differs from example 1 in that:
the mineral powder is 100nm talcum powder.
Example 6
This example differs from example 1 in that:
the biodegradation accelerator consists of calcium dihydrogen phosphate and potassium dihydrogen phosphate according to the weight ratio of 1: 1.
Example 7
A bio-based fully-degradable chopstick material comprises the following raw materials in parts by weight:
Figure BDA0001868918570000081
Figure BDA0001868918570000091
wherein the melt index of the L-PLA is 8g/10min, the test conditions are 210 ℃/2.16kg, the glass transition temperature is 60 ℃, and the crystallization temperature is 155 ℃.
Wherein the melt index of the D-PLA is 2g/10min, the test conditions are 210 ℃/2.16kg, the glass transition temperature is 55 ℃, and the crystallization temperature is 155 ℃.
Wherein the mineral powder is talcum powder, and the mesh number of the mineral powder is 3000 meshes.
Wherein the diameter of the glass fiber is 13 μm, and the linear density is 1000 g/km.
Wherein the biodegradation accelerator is calcium dihydrogen phosphate.
Wherein the lubricant is pentaerythritol stearate.
Wherein the nucleating agent is inorganic layered silicate.
The preparation method of the bio-based fully-degradable chopstick material is characterized by comprising the following steps: the method comprises the following steps:
(1) measuring L-PLA and D-PLA according to a formula amount, and mixing for 4min at a rotating speed of 300r/min to obtain a first mixture;
(2) adding mineral powder, a lubricant and a nucleating agent into the first mixture, and mixing at a rotating speed of 500r/min for 10min to obtain a second mixture;
(3) adding a biodegradation accelerator into the second mixture, heating to 60 ℃, and mixing at a rotating speed of 800-1000 r/min for 10min to obtain a third mixture;
(4) and adding the third mixture from a main feeding port of an extruder, adding the glass fiber from a side feeding port of the extruder, and performing melt extrusion at the temperature of 170 ℃ to obtain the bio-based fully-degradable chopstick material.
Example 8
A bio-based fully-degradable chopstick material comprises the following raw materials in parts by weight:
Figure BDA0001868918570000101
wherein the melt index of the L-PLA is 10g/10min, the test conditions are 210 ℃/2.16kg, the glass transition temperature is 65 ℃, and the crystallization temperature is 160 ℃.
Wherein the melt index of the D-PLA is 8g/10min, the test conditions are 210 ℃/2.16kg, the glass transition temperature is 60 ℃, and the crystallization temperature is 60 ℃.
Wherein the mineral powder is calcium carbonate, and the mesh number of the mineral powder is 10000 meshes.
Wherein the diameter of the glass fiber is 17 μm, and the linear density is 2000 g/km.
Wherein the biodegradation accelerator is potassium dihydrogen phosphate.
Wherein the lubricant is zinc stearate.
Wherein the nucleating agent is nano silicon dioxide.
The preparation method of the bio-based fully-degradable chopstick material is characterized by comprising the following steps: the method comprises the following steps:
(1) measuring L-PLA and D-PLA according to a formula, and mixing for 2min at a rotating speed of 500r/min to obtain a first mixture;
(2) adding mineral powder, a lubricant and a nucleating agent into the first mixture, and mixing at the rotating speed of 800r/min for 5min to obtain a second mixture;
(3) adding a biodegradation accelerator into the second mixture, heating to 90 ℃, and mixing at a rotating speed of 1000r/min for 6min to obtain a third mixture;
(4) and adding the third mixture from a main feeding port of an extruder, adding the glass fiber from a side feeding port of the extruder, and performing melt extrusion at the temperature of 200 ℃ to obtain the bio-based fully-degradable chopstick material.
Comparative example 1
This comparative example differs from example 1 in that:
no biodegradation accelerator was added.
The invention performs a performance test on examples 1-6 and comparative example 1, with the following results:
Figure BDA0001868918570000111
Figure BDA0001868918570000112
Figure BDA0001868918570000121
as can be seen from the comparison among examples 1, 4 and 5, the preferred compound mineral powder can improve the degradation performance of the mechanical properties of the chopstick material, and on the contrary, the nano-sized talc powder can cause the degradation of the mechanical properties.
As can be seen from the comparison of the examples 1 and 6 with the comparative example 1, the addition of the biodegradation accelerator has little influence on the mechanical properties of the chopstick material, but the degradation performance is significantly improved, the degradation performance can be further improved by selecting the proper compound biodegradation accelerator, and the residual weight ratio of 9.4 percent can be realized under the natural degradation for 8 months.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.

Claims (3)

1. A bio-based fully-degradable chopstick material is characterized in that: the feed comprises the following raw materials in parts by weight:
40-65 parts of L-PLA
0-30 parts of D-PLA
15-25 parts of mineral powder
10-15 parts of glass fiber
0.1-0.5 part of biodegradation accelerator
0.1 to 0.5 portion of lubricant
0.5-1.5 parts of nucleating agent;
the melt index of the D-PLA is 2-8 g/10min, the testing condition is 210 ℃/2.16kg, the glass transition temperature is 55-60 ℃, and the crystallization temperature is 155-160 ℃;
the biodegradation accelerator consists of calcium dihydrogen phosphate and potassium dihydrogen phosphate according to the weight ratio of 1: 1;
the lubricant consists of pentaerythritol stearate and calcium stearate in a weight ratio of 2: 1;
the nucleating agent is one or more than one of inorganic phyllosilicate, nano silicon dioxide and 1,3, 5-benzene tricarboxyamide;
the melt index of the L-PLA is 8-10 g/10min, the test condition is 210 ℃/2.16kg, the glass transition temperature is 60-65 ℃, and the crystallization temperature is 155-160 ℃;
the mineral powder consists of 5000-mesh calcium carbonate and 3000-mesh talcum powder according to the weight ratio of 2-3: 1;
the diameter of the glass fiber is 13-17 mu m, and the linear density is 1000-2000 g/km.
2. The bio-based fully degradable chopstick material as claimed in claim 1, wherein: the feed comprises the following raw materials in parts by weight:
40-65 parts of L-PLA
5-30 parts of D-PLA
15-25 parts of mineral powder
10-15 parts of glass fiber
0.1-0.5 part of biodegradation accelerator
0.1 to 0.5 portion of lubricant
0.5-1.5 parts of nucleating agent;
the melt index of the D-PLA is 2-8 g/10min, the testing condition is 210 ℃/2.16kg, the glass transition temperature is 55-60 ℃, and the crystallization temperature is 155-160 ℃;
the biodegradation accelerator consists of calcium dihydrogen phosphate and potassium dihydrogen phosphate according to the weight ratio of 1: 1;
the lubricant consists of pentaerythritol stearate and calcium stearate in a weight ratio of 2: 1;
the nucleating agent is one or more than one of inorganic phyllosilicate, nano silicon dioxide and 1,3, 5-benzene tricarboxyamide;
the melt index of the L-PLA is 8-10 g/10min, the test condition is 210 ℃/2.16kg, the glass transition temperature is 60-65 ℃, and the crystallization temperature is 155-160 ℃;
the mineral powder consists of 5000-mesh calcium carbonate and 3000-mesh talcum powder according to the weight ratio of 2-3: 1;
the diameter of the glass fiber is 13-17 mu m, and the linear density is 1000-2000 g/km.
3. The preparation method of the bio-based fully degradable chopstick material as recited in any one of claims 1-2, wherein the method comprises the following steps: the method comprises the following steps:
(1) measuring L-PLA and D-PLA according to a formula amount, and mixing for 2-4 min at a rotating speed of 300-500 r/min to obtain a first mixture;
(2) adding mineral powder, a lubricant and a nucleating agent into the first mixture, and mixing at a rotating speed of 500-800 r/min for 5-10 min to obtain a second mixture;
(3) adding a biodegradation accelerator into the second mixture, heating to 60-90 ℃, and mixing at a rotating speed of 800-1000 r/min for 6-10 min to obtain a third mixture;
(4) and adding the third mixture from a main feeding port of an extruder, adding glass fiber from a side feeding port of the extruder, and performing melt extrusion at the temperature of 170-200 ℃ to obtain the bio-based fully-degradable chopstick material.
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