CN114085497A - Bio-based fully-degradable film and preparation method thereof - Google Patents
Bio-based fully-degradable film and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 9
- 229920002472 Starch Polymers 0.000 claims abstract description 39
- 239000008107 starch Substances 0.000 claims abstract description 39
- 235000019698 starch Nutrition 0.000 claims abstract description 39
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 26
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 229920001896 polybutyrate Polymers 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 14
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 14
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 13
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 13
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 13
- 235000005822 corn Nutrition 0.000 claims abstract description 13
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 13
- 239000008158 vegetable oil Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 44
- 239000000725 suspension Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 15
- 239000000835 fiber Substances 0.000 claims description 12
- 229920005610 lignin Polymers 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 11
- 239000011246 composite particle Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- 238000000071 blow moulding Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 241000209149 Zea Species 0.000 claims 2
- 238000000034 method Methods 0.000 claims 1
- 240000008042 Zea mays Species 0.000 abstract description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 4
- 244000005700 microbiome Species 0.000 abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 2
- 239000001569 carbon dioxide Substances 0.000 abstract description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 description 12
- 239000004033 plastic Substances 0.000 description 12
- 238000006065 biodegradation reaction Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- 238000009264 composting Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 229920000331 Polyhydroxybutyrate Polymers 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 229920000520 poly(3-hydroxybutyrate-co-3-hydroxyvalerate) Polymers 0.000 description 1
- 229920000903 polyhydroxyalkanoate Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/02—Starch; Degradation products thereof, e.g. dextrin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2497/00—Characterised by the use of lignin-containing materials
- C08J2497/02—Lignocellulosic material, e.g. wood, straw or bagasse
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2499/00—Characterised by the use of natural macromolecular compounds or of derivatives thereof not provided for in groups C08J2401/00 - C08J2407/00 or C08J2489/00 - C08J2497/00
-
- 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
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
Abstract
The invention discloses a bio-based fully-degradable film and a preparation method thereof. The bio-based fully-degradable film comprises the following raw materials in parts by weight: 120 parts of PBAT 100, 20-30 parts of starch dispersion liquid, 10-15 parts of calcium carbonate, 10-15 parts of corn grit, 5-8 parts of vegetable oil, 1-3 parts of tributyl citrate and 10-20 parts of polyvinyl alcohol. The raw materials adopted by the film belong to renewable resources, can be degraded under natural conditions by the action of microorganisms, and finally generate carbon dioxide and water without any burden on the environment.
Description
Technical Field
The invention relates to a bio-based fully-degradable film and a preparation method thereof, belonging to the technical field of plastics.
Background
As a novel material, the plastic product has the advantages of light weight, water resistance, durability, mature production technology and low cost, is widely applied all over the world and is in the trend of increasing year by year. They come from industry, are manufactured by human beings, and are not easily absorbed by nature when finally attributed to nature, thereby influencing the ecological environment of nature. White pollution is the special environmental pollution of cities in China, a large number of waste plastic products can be seen everywhere in various public places, and the plastic products are recycled as far as possible from the perspective of saving resources in the face of increasingly serious white pollution problems, but the recycling cost at the present stage is far higher than the direct production cost, so that the recycling cost is difficult to achieve under the existing market economic conditions. The plastic with the novel function is characterized in that after the plastic is abandoned for a certain service life, the plastic is degraded under specific environmental conditions due to obvious change of chemical structure, certain performance loss and appearance change are caused, and the plastic is harmless or less harmful to the natural environment.
The existing full-biodegradable materials are important research objects, mainly PLA, PBAT, PBS, PHA, PVA, PHB and PHBV, but the materials can be biodegraded only under the controlled composting condition, the requirements on the composting environment and the microbial environment are higher, a large amount of grains are consumed, the cost of raw materials is far higher than that of the original polyolefin plastic materials, the physical and mechanical properties of the materials are poor, and the original plastic products and the application are difficult to be completely replaced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a bio-based fully-degradable film and a preparation method thereof.
The invention is realized by the following technical scheme:
a bio-based fully-degradable film comprises the following raw materials in parts by weight: 120 parts of PBAT 100, 20-30 parts of starch dispersion liquid, 10-15 parts of calcium carbonate, 10-15 parts of corn grit, 5-8 parts of vegetable oil, 1-3 parts of tributyl citrate and 10-20 parts of polyvinyl alcohol.
The bio-based fully degradable film is prepared by the following steps of: adding starch into sulfuric acid solution, heating to 50-60 deg.C, slowly stirring and mixing under ultrasonic condition, adding lignin fiber suspension, and mixing to obtain starch dispersion.
The bio-based fully-degradable film is prepared from the following raw materials in parts by weight, based on 10 parts by weight of starch: 50-60 parts of sulfuric acid solution and 10-15 parts of lignocellulose suspension.
The bio-based fully degradable film is characterized in that the mass fraction of sulfuric acid in the sulfuric acid solution is 60-70%.
The bio-based fully degradable film is characterized in that the lignin fiber suspension is obtained by the following steps: and (2) placing the lignocellulose in a ball mill for wet ball milling, wherein the weight ratio of the lignocellulose to the balls to the water is 1:3:1-2, and carrying out ball milling to obtain a lignocellulose suspension.
The preparation method of the bio-based fully degradable film comprises the following steps: mixing PBAT, starch dispersion, calcium carbonate, corn grit, vegetable oil, tributyl citrate and polyvinyl alcohol, adding the mixture into a double-screw extruder, melting, extruding, granulating and drying to obtain composite particles, and processing the composite particles into a film by using a blow molding machine.
The invention achieves the following beneficial effects:
the raw materials adopted by the film belong to renewable resources, can be degraded under natural conditions by the action of microorganisms, and finally generate carbon dioxide and water without any burden on the environment.
The fully degradable film disclosed by the invention takes PBAT as a main raw material, the strength of the PBAT is improved by adding the starch dispersion liquid, the calcium carbonate and the corn grit, and meanwhile, the tensile strength of the PBAT is improved by adding the vegetable oil, the tributyl citrate and the polyvinyl alcohol.
The starch dispersion liquid is added with the lignin fiber, so that the strength of PBAT is improved, the physical and mechanical properties of the film are improved, the normal requirements of the film can be met, and meanwhile, the starch can be fully mixed with the lignin fiber after being treated by the sulfuric acid solution, so that the strength of the starch is enhanced.
Detailed Description
The invention is further described below. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
A bio-based fully-degradable film comprises the following raw materials in parts by weight: 100 parts of PBAT, 30 parts of starch dispersion liquid, 10 parts of calcium carbonate, 10 parts of corn grit, 8 parts of vegetable oil, 1 part of tributyl citrate and 20 parts of polyvinyl alcohol.
The starch dispersion is obtained by the following steps: adding starch into sulfuric acid solution, heating to 50-60 deg.C, slowly stirring and mixing under ultrasonic condition, adding lignin fiber suspension, and mixing to obtain starch dispersion.
The starch is calculated by 10 parts by weight, and the rest raw materials are respectively in parts by weight: 50 parts of sulfuric acid solution and 10 parts of lignocellulose suspension.
The mass fraction of sulfuric acid in the sulfuric acid solution is 70%.
The lignin fiber suspension is obtained by the following steps: and (2) placing the lignocellulose in a ball mill for wet ball milling, wherein the weight ratio of the lignocellulose to the balls to the water is 1:3:1, and carrying out ball milling to obtain a lignocellulose suspension.
A preparation method of a bio-based fully-degradable film comprises the following steps: mixing PBAT, starch dispersion, calcium carbonate, corn grit, vegetable oil, tributyl citrate and polyvinyl alcohol, adding the mixture into a double-screw extruder, melting, extruding, granulating and drying to obtain composite particles, and processing the composite particles into a film by using a blow molding machine.
The lignocellulose subjected to ball milling is mixed with starch under the ultrasonic condition, the mixture can be fully mixed with the starch, the starch is treated by adopting a sulfuric acid solution, the hydrolyzed starch can be biodegraded, and meanwhile, the starch can be fully mixed with the lignocellulose, and the strength of the film can be increased by the integral dispersion liquid.
Example 2
A bio-based fully-degradable film comprises the following raw materials in parts by weight: 120 parts of PBAT, 20 parts of starch dispersion liquid, 15 parts of calcium carbonate, 15 parts of corn grit, 5 parts of vegetable oil, 3 parts of tributyl citrate and 10 parts of polyvinyl alcohol.
The starch dispersion is obtained by the following steps: adding starch into sulfuric acid solution, heating to 50-60 deg.C, slowly stirring and mixing under ultrasonic condition, adding lignin fiber suspension, and mixing to obtain starch dispersion.
The starch is calculated by 10 parts by weight, and the rest raw materials are respectively in parts by weight: 60 parts of sulfuric acid solution and 15 parts of lignocellulose suspension.
The mass fraction of the sulfuric acid in the sulfuric acid solution is 60%.
The lignin fiber suspension is obtained by the following steps: and (2) placing the lignocellulose in a ball mill for wet ball milling, wherein the weight ratio of the lignocellulose to the balls to the water is 1:3:2, and carrying out ball milling to obtain a lignocellulose suspension.
A preparation method of a bio-based fully-degradable film comprises the following steps: mixing PBAT, starch dispersion, calcium carbonate, corn grit, vegetable oil, tributyl citrate and polyvinyl alcohol, adding the mixture into a double-screw extruder, melting, extruding, granulating and drying to obtain composite particles, and processing the composite particles into a film by using a blow molding machine.
Example 3
A bio-based fully-degradable film comprises the following raw materials in parts by weight: 110 parts of PBAT, 26 parts of starch dispersion liquid, 12 parts of calcium carbonate, 12 parts of corn grit, 7 parts of vegetable oil, 2 parts of tributyl citrate and 16 parts of polyvinyl alcohol.
The starch dispersion is obtained by the following steps: adding starch into sulfuric acid solution, heating to 50-60 deg.C, slowly stirring and mixing under ultrasonic condition, adding lignin fiber suspension, and mixing to obtain starch dispersion.
The starch is calculated by 10 parts by weight, and the rest raw materials are respectively in parts by weight: 50-60 parts of sulfuric acid solution and 10-15 parts of lignocellulose suspension.
The mass fraction of the sulfuric acid in the sulfuric acid solution is 60-70%.
The lignin fiber suspension is obtained by the following steps: and (2) placing the lignocellulose in a ball mill for wet ball milling, wherein the weight ratio of the lignocellulose to the balls to the water is 1:3:1, and carrying out ball milling to obtain a lignocellulose suspension.
A preparation method of a bio-based fully-degradable film comprises the following steps: mixing PBAT, starch dispersion, calcium carbonate, corn grit, vegetable oil, tributyl citrate and polyvinyl alcohol, adding the mixture into a double-screw extruder, melting, extruding, granulating and drying to obtain composite particles, and processing the composite particles into a film by using a blow molding machine.
Comparative example 1
A bio-based fully-degradable film comprises the following raw materials in parts by weight: 110 parts of PBAT, 12 parts of calcium carbonate, 12 parts of corn grit, 7 parts of vegetable oil, 2 parts of tributyl citrate and 16 parts of polyvinyl alcohol.
The plastic particles in the examples and the comparative examples are subjected to performance tests and biodegradation tests at the same time, wherein the biodegradation tests refer to GB/T19275-2003 evaluation on potential biodegradation and disintegration capability of materials under the action of specific microorganisms, the soil landfill test method is used, the landfill time is 90 days, the biodegradation capability of the materials is evaluated by using the average percentage (%) of mass change as an evaluation standard, and the higher the value, the better the biodegradation capability is, and specific results are shown in Table 1.
TABLE 1 Plastic particle Performance test and biodegradation test results
| Example 1 | Example 1 | Example 3 | Comparative example 1 | |
| Tensile strength MPa | 52.5 | 51.2 | 50.3 | 43.5 |
| Bending strength MPa | 57.3 | 56.6 | 50.8 | 40.3 |
| Biodegradation Rate (%) | 28.9 | 28.5 | 28.6 | 10.2 |
| Impact strength kJ/m2 | 15.3 | 14.5 | 16.1 | 6.9 |
From table 1, examples 1, 2 and 3, to which modified starch was added, had good strength and good biodegradability as compared to comparative example 1.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A bio-based fully degradable film is characterized by comprising the following raw materials in parts by weight: 120 parts of PBAT 100, 20-30 parts of starch dispersion liquid, 10-15 parts of calcium carbonate, 10-15 parts of corn grit, 5-8 parts of vegetable oil, 1-3 parts of tributyl citrate and 10-20 parts of polyvinyl alcohol.
2. The bio-based fully degradable film as claimed in claim 1, wherein said starch dispersion is obtained by the steps of: adding starch into sulfuric acid solution, heating to 50-60 deg.C, slowly stirring and mixing under ultrasonic condition, adding lignin fiber suspension, and mixing to obtain starch dispersion.
3. The bio-based fully degradable film as claimed in claim 2, wherein the weight parts of the starch are 10 parts, and the weight parts of the other raw materials are respectively as follows: 50-60 parts of sulfuric acid solution and 10-15 parts of lignocellulose suspension.
4. The bio-based fully degradable film as claimed in claim 3, wherein the mass fraction of sulfuric acid in said sulfuric acid solution is 60-70%.
5. The bio-based fully degradable film as claimed in claim 3, wherein said lignin fiber suspension is obtained by the following steps: and (2) placing the lignocellulose in a ball mill for wet ball milling, wherein the weight ratio of the lignocellulose to the balls to the water is 1:3:1-2, and carrying out ball milling to obtain a lignocellulose suspension.
6. The method for preparing the bio-based fully degradable film according to any one of claims 1 to 5, which comprises the following steps: mixing PBAT, starch dispersion, calcium carbonate, corn grit, vegetable oil, tributyl citrate and polyvinyl alcohol, adding the mixture into a double-screw extruder, melting, extruding, granulating and drying to obtain composite particles, and processing the composite particles into a film by using a blow molding machine.
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