CN112080114A - Degradable plastic master batch and preparation method of degradable plastic - Google Patents
Degradable plastic master batch and preparation method of degradable plastic Download PDFInfo
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- 229920006238 degradable plastic Polymers 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 98
- 239000002028 Biomass Substances 0.000 claims abstract description 79
- 239000000463 material Substances 0.000 claims abstract description 44
- 229930182556 Polyacetal Natural products 0.000 claims abstract description 37
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 229920003023 plastic Polymers 0.000 claims abstract description 24
- 239000004033 plastic Substances 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004381 surface treatment Methods 0.000 claims abstract description 19
- 229920002689 polyvinyl acetate Polymers 0.000 claims abstract description 18
- 239000011812 mixed powder Substances 0.000 claims abstract description 16
- WTKXVQOMXURINP-UHFFFAOYSA-N 8-ethenylfluoranthene Chemical compound C1=CC(C2=CC=C(C=C22)C=C)=C3C2=CC=CC3=C1 WTKXVQOMXURINP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000003607 modifier Substances 0.000 claims abstract description 8
- 239000003223 protective agent Substances 0.000 claims abstract description 8
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- 229920002545 silicone oil Polymers 0.000 claims abstract description 5
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- 239000007788 liquid Substances 0.000 claims abstract description 4
- 229920005610 lignin Polymers 0.000 claims abstract description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 44
- 239000000203 mixture Substances 0.000 claims description 14
- 239000010902 straw Substances 0.000 claims description 14
- 229920001187 thermosetting polymer Polymers 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
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- 238000000034 method Methods 0.000 claims description 11
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- 229920005989 resin Polymers 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
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- 239000004626 polylactic acid Substances 0.000 claims description 7
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 229910001923 silver oxide Inorganic materials 0.000 claims description 6
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 6
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- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims 2
- 244000098338 Triticum aestivum Species 0.000 claims 1
- 238000004806 packaging method and process Methods 0.000 abstract description 13
- -1 ethanol Chemical compound 0.000 abstract description 3
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- 239000001993 wax Substances 0.000 description 26
- 235000013305 food Nutrition 0.000 description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 5
- 239000005977 Ethylene Substances 0.000 description 5
- 235000013399 edible fruits Nutrition 0.000 description 5
- 229920001568 phenolic resin Polymers 0.000 description 5
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- 229920000747 poly(lactic acid) Polymers 0.000 description 5
- 230000035882 stress Effects 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
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- 239000004698 Polyethylene Substances 0.000 description 2
- 241000209140 Triticum Species 0.000 description 2
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
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- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
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- 241000335053 Beta vulgaris Species 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- 241000222393 Phanerochaete chrysosporium Species 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
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- 230000002378 acidificating effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229920003232 aliphatic polyester Polymers 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 230000018109 developmental process Effects 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
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- 239000010881 fly ash Substances 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 235000019256 formaldehyde Nutrition 0.000 description 1
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- 239000010903 husk Substances 0.000 description 1
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- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 229910052903 pyrophyllite Inorganic materials 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2286—Oxides; Hydroxides of metals of silver
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- 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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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to a low-temperature wet preparation method of degradable plastic master batch, which comprises the following steps: preparing biomass powder containing plant cellulose and lignin; performing surface treatment on the biomass powder by adopting Fischer-Tropsch wax; pressurizing the biomass powder to eliminate the internal stress of the biomass powder; mixing the biomass powder with PLA, PHA and a plastic modifier to obtain mixed powder; mixing PVB, PVFA and PVAC according to a certain proportion to prepare a polyacetal protectant, and dissolving the polyacetal protectant in liquid alcohol to obtain a polyacetal protectant solution; mixing the mixed powder with the polyacetal protective agent solution, stirring, adding starch, making into smooth dough, coating silicone oil on the inner wall of the extruder and the screw, and extruding and granulating at 20-65 deg.C. The plastic master batch can be prepared into degradable plastic packaging bags and packaging boxes, has good durability, is not easy to age, more importantly, has good recycling property, and almost all the other materials can be naturally degraded after PVB is treated and dissolved by alcohol such as ethanol, and the like, so that the environment-friendly property is excellent.
Description
Technical Field
The invention relates to the technical field of environment-friendly materials, in particular to a degradable plastic master batch, a degradable plastic and a preparation method thereof.
Background
With the rapid development of the take-out and food delivery industry and the supermarket fresh food industry, the use frequency of the disposable food packaging bags is higher and higher, and the plastic materials can not be degraded generally, so that great pressure is brought to ecological environment protection. In order to solve the degradation problem of materials such as disposable food packaging bags, some solutions are also proposed in the industry at present. Most commonly, natural biomass (straw powder, plant cellulose, wood lignin and the like) is used as a basic material to prepare some environment-friendly and degradable food packaging materials. However, these materials are natural biodegradable materials, and have very poor resistance to moisture, oxidation, acid, and the like, and are oxidized and the polymer bond is broken due to direct contact with surrounding moisture, air, and the like in a short time after being manufactured, so that the packaging material is rapidly aged and the strength is reduced, and thus the packaging material cannot be used. In order to solve the technical problem, it is necessary to improve such environmentally friendly materials.
Disclosure of Invention
The invention aims to solve the technical problem of providing a degradable plastic master batch, a degradable plastic and a preparation method.
The invention comprises the following technical scheme:
on one hand, the low-temperature wet preparation method of the degradable plastic master batch comprises the following steps:
s1 preparation of Biomass powder
Crushing dried crop straws, chaffs, nut shells, weeds, algae or wood, and sieving with a sieve of 80-120 meshes to obtain biomass powder;
s2 surface treatment of Biomass powder
Performing surface treatment on the biomass powder by adopting Fischer-Tropsch wax to make the biomass powder be infected with the Fischer-Tropsch wax to prepare surface-treated biomass powder, and performing the surface treatment to improve the hydrophobicity of the surface of the biomass powder;
s3 pressure treatment
Compacting the biomass powder subjected to surface treatment for 2h-30h under the pressure of 2-10MPa to eliminate the internal stress of the cell wall of the biomass powder, so as to obtain the biomass powder subjected to pressure treatment;
s4, mixing the biomass powder subjected to pressure treatment with polylactic acid (PLA) powder, Polyhydroxyalkanoate (PHA) powder and a plastic modifier to obtain mixed powder;
s5 preparation of polyacetal protectant solution
The polyacetal protectant comprises at least one of polyvinyl butyral (PVB), polyvinyl methylaldehyde (PVFA), and polyvinyl butyral (PVAC);
dissolving the polyacetal protectant in liquid alcohol to obtain a colorless transparent solution, wherein the colorless transparent solution is the solution of the polyacetal protectant;
s6 granulation
And mixing and stirring the mixed powder and the polyacetal protective agent solution, adding a proper amount of starch (serving as an adhesive and a lubricant) to prepare a smooth dough, coating silicone oil on the inner wall and the screw of an extruder, extruding into strips at 20-65 ℃ by using the extruder, granulating, and drying to obtain the degradable plastic master batch.
According to the preferred embodiment of the present invention, in step S1, biomass powder is prepared by sieving with a 100-mesh standard sieve; preferably, the crop stalks comprise rice straw, wheat straw, bean straw, corn stalk, sorghum stalk, cotton stalk, and the like.
Preferably, according to the application and the requirement of the degradable plastic material to be prepared, the biomass powder can be prepared by crushing and proportionally mixing crop straws, herbaceous plant cellulose and wood leather from different sources, the plant cellulose from the crop straws, weeds and the like is usually smaller in molecular weight, and the prepared plastic material has good stretchability and processability; the vegetable cellulose of the wood skin material has larger molecular weight, and can provide better toughness and strength.
According to a preferred embodiment of the present invention, in step S2, the method for performing surface treatment on the biomass powder by using the fischer-tropsch wax comprises: firstly adding a surfactant into water to prepare a solution, then adding Fischer-Tropsch wax, heating until the Fischer-Tropsch wax is completely melted, emulsifying by using ultrasonic waves to obtain Fischer-Tropsch wax emulsion, uniformly spraying the Fischer-Tropsch wax emulsion on the surface of the biomass powder, uniformly stirring, drying, rubbing and scattering, and drying until the water content is below 1%, thereby preparing the biomass powder subjected to surface treatment. Wherein the drying temperature is preferably 100-110 ℃.
According to a preferred embodiment of the present invention, in step S2, a surfactant is added to water to prepare a solution with a mass concentration of 0.03 wt% to 0.4 wt%; the mass ratio of the added Fischer-Tropsch wax to the solution is 4-8: 100-150.
According to a preferred embodiment of the present invention, in step S2, the mass ratio of the fischer-tropsch wax to the biomass powder is 1: 9-25.
The molecular weight of the Fischer-Tropsch wax is far lower than that of the common paraffin wax, the branched chain is less, and the crystallinity is high; the melted Fischer-Tropsch wax can be effectively infiltrated and infiltrated into the surface of the biomass powder, so that the hydrophobicity of the surface of the biomass powder can be improved, the fusion degree with a resin material can be enhanced, and the extrusion viscosity can be reduced in the later period.
According to the preferred embodiment of the present invention, the purpose of the pressurization treatment in S3 is to eliminate the internal stress generated by the organic cell wall due to the free water or the bound water contained in the cells of the biomass powder, thereby improving the processing properties of the biomass powder, such as granulation compatibility, homogenization, etc.
According to the preferred embodiment of the present invention, in S4, the mass ratio of each component in the mixed powder is: 10-40 wt% of biomass powder, 40-60 wt% of PLA and PHA powder and 3-15 wt% of plastic modifier; the plastic modifier is natural rubber powder. Natural rubber functions as a crosslinking agent in the present invention. In the process of preparing the degradable plastic material, a cross-linked network structure is formed in a screw extruder by heating. The crosslinked network structure can enhance the strength and durability of the degradable plastic material.
According to the preferred embodiment of the present invention, in S4, 13-35 wt% of a reinforcing material is further added to the mixed powder, and the reinforcing material is a thermosetting resin. When the thermosetting resin is extruded and granulated, the temperature of the extrusion and granulation does not reach the thermosetting temperature, but the thermosetting resin is uniformly dispersed in a polyacetal solution in a molecular form to prepare degradable plastic master batches; when the degradable plastic master batch is melted and extruded to be further made into materials such as a degradable plastic film material or a sheet material, the thermosetting resin can generate crosslinking (lose water molecules) to be cured due to higher temperature (reaching the thermosetting generation temperature of the thermosetting resin), and all components of the degradable plastic material can be tightly bonded together, so that the strength of the degradable plastic film material or the sheet material is enhanced.
Preferably, the thermosetting resin is a thermosetting phenolic resin (which can be degraded by Phanerochaete chrysosporium, a white rot fungus, and can be cured after being kept at 150 ℃ for a period of time). The high cross-linking properties give the phenolic resin hardness, good thermal stability and chemical barrier properties. According to the preferred embodiment of the invention, 0.5-3.0 wt% of antioxidant and/or 0.05-0.2 wt% of nano silver oxide is added into the mixed powder in S4.
The nano silver oxide has the effects of sterilization and antibiosis, and can catalyze and decompose ethylene, so that the deterioration of fresh fruits and vegetables can be delayed. Therefore, the plastic master batch added with the nano silver oxide is very suitable for packaging foods such as fresh fruits and vegetables after being prepared into a plastic package.
According to a preferred embodiment of the present invention, in S5, the polyacetal protectant has a composition of one of the following three compositions:
the composition is as follows: 1-35 parts by mass of polyvinyl butyral (PVB), 1-45 parts by mass of polyvinyl methyl acetaldehyde (PVFA), 0-15 parts by mass of polyvinyl butyral (PVAC)1 type and 0-15 parts by mass of polyvinyl butyral (PVAC)2 type;
the composition is two: 1-35 parts by mass of polyvinyl butyral (PVB), 1-45 parts by mass of polyvinyl methyl acetaldehyde (PVFA), 15-60 parts by mass of polyvinyl butyral (PVAC)1 type and 15-60 parts by mass of polyvinyl butyral (PVAC)2 type;
the composition is three: 1-35 parts of polyvinyl butyral (PVB), 1-45 parts of polyvinyl methyl acetaldehyde (PVFA), 60-120 parts of polyvinyl butyral (PVAC)1 type and 60-120 parts of polyvinyl butyral (PVAC)2 type.
Wherein, the first composition is suitable for preparing plastic materials or tableware materials used at normal temperature or low temperature (the applicable temperature range is 0-50 ℃), the second composition is suitable for preparing plastic packaging materials or tableware materials used at medium temperature (the applicable temperature range is 0-80 ℃), and the third composition is suitable for preparing plastic packaging materials or tableware materials used at high temperature (the applicable temperature range is 0-120 ℃).
According to a preferred embodiment of the present invention, in S5, the polyacetal protectant is dissolved in ethanol to prepare a colorless transparent solution with a concentration of 3% to 15% by weight, thereby obtaining a polyacetal protectant solution.
In another aspect, the present invention relates to a degradable plastic masterbatch, which is prepared by any one of the above methods.
In another aspect, the invention relates to a method for preparing a degradable plastic material, which comprises the following steps:
uniformly mixing the degradable plastic master batch with the filler and the auxiliary agent, and extruding by using a screw machine to prepare a degradable plastic material;
wherein, the components are mixed according to the following proportion:
50-65 wt% of degradable plastic master batch, 5-10 wt% of plasticizer, 5-10 wt% of toughening agent, 5-25 wt% of filler, 5-20 wt% of PVB protective agent and 5-10 wt% of silane coupling agent, and mixing to 100%; then, uniformly stirring, and finally extruding and molding the degradable plastic material by adopting a screw machine; the screw temperature of the screw extruder is 120-240 ℃.
Wherein, the filler is selected from one or more of light calcium carbonate, wollastonite powder, talcum powder, barium sulfate, pyrophyllite powder, kaolin, fly ash, silicon carbide, boron nitride and alumina.
Wherein the silane coupling agent is KH-550 or KH 560.
Wherein the screw temperature of the screw extruder is 170-180 ℃.
The technical effects of the invention comprise:
(1) according to the invention, polyacetal such as PVB is used as a protective agent to coat the surface of the biomass powder to form an isolation protective film, so that the prepared biomass powder is prevented from directly contacting components such as water vapor, oxygen, acidic gas and the like in the air, the oxidative decomposition speed of the biomass powder is delayed, the service life of the biodegradable material is prolonged, and the problems of quick aging, short service life and the like of the degradable plastic prepared from the biomass material are solved.
(2) The invention adopts PVB (and PVFA or PVAC) bonding granulation to solve the compatibility problem among various materials, solves the problem that the granulation cannot use thermosetting plastics for modification (due to the low extrusion granulation temperature, thermosetting phenolic resin and the like can be added as reinforcing materials), increases the application range and modification space of the materials, and can use more materials to further improve the product. The extrusion granulation of the invention adopts PVB (and PVFA or PVAC) which can be dissolved in ethanol (methanol) as a binder, and the problem of uneven homogenization between powder and particles and between powder and liquid can be solved by granulation in a bonding mode. The PVB, PVFA or PVAC are mixed according to different proportions, so that the final product capable of being used in different temperature environments can be obtained.
(3) The Fischer-Tropsch wax is adopted to carry out surface treatment on the biomass powder, so that the hydrophobicity of the surface of the biomass powder is improved, the fat solubility of the biomass powder is enhanced, the compatibility between the biomass powder and other polymeric organic substances is improved, and the problems that the granulation compatibility between the biomass powder and other organic synthetic polymer materials (such as polylactic acid (PLA) powder, Polyhydroxyalkanoate (PHA) powder, a plastic modifier and the like) is poor, the biomass powder is easy to corrode and age by moisture in the air and the like are solved.
(4) The biomass powder is compacted for 2h to 30h under the pressure of 2 MPa to 10MPa to eliminate the internal stress of the biomass powder, so that the biomass powder subjected to pressurization treatment is obtained, the morphology, the dimensional stability and the processing performance of the biomass powder are improved, and the size and the morphology stability of the finally prepared degradable plastic material are further improved.
(5) The polylactic acid PLA used therein, also known as polylactide, is a thermoplastic aliphatic polyester derived from renewable materials, usually from fermented plant starches, such as corn, tapioca, sugarcane or beet pulp, and has good biocompatibility and biodegradability. Polyhydroxyalkanoate PHA is an intracellular polyester synthesized by a plurality of bacteria, mainly exists as a storage substance of a carbon source and an energy source in organisms, has physicochemical characteristics similar to those of synthetic plastics and biodegradability and biocompatibility which are not possessed by the synthetic plastics, and has the defect of higher production cost. However, the amount of PHA used in the present invention is small and the cost of the final product is not very high.
(6) The degradable plastic of the invention is very easy to recycle. After the plastic material is discarded, the plastic material can be heated and soaked by ethanol water solution, and PVB (and PVFA or PVAC) serving as an isolation protective film and an adhesive phase can be dissolved in ethanol, so that after the PVB is damaged, the material which is not protected by the PVB can be buried in soil and can be decomposed by microorganisms, and the plastic disclosed by the invention has very good overall degradability and environmental friendliness. At the same time, the solution of the polyacetal protectant used in the step S5 can be recovered again from the PVB or the like dissolved in ethanol.
The present invention will be further described with reference to the following specific examples.
Detailed Description
Example 1
A preparation method of a degradable plastic food bag comprises the following steps:
(1) preparation of Biomass powder
Crushing the dried crop straws, rice husks and tree skins, and sieving the crushed materials with a 100-mesh sieve to obtain the biomass powder.
(2) Surface treatment of biomass powder
Firstly, adding a surfactant sodium dodecyl benzene sulfonate into water to prepare a solution with the concentration of 0.2 wt%, adding Fischer-Tropsch wax, wherein the mass ratio of the Fischer-Tropsch wax to the solution is 6:120, heating the solution until the Fischer-Tropsch wax is completely melted, stirring and emulsifying by using ultrasonic waves to obtain Fischer-Tropsch wax emulsion, uniformly spraying the Fischer-Tropsch wax emulsion on the surface of biomass powder, uniformly stirring, drying at 110 ℃, rubbing and scattering, and drying until the water content is below 1%, thus preparing the biomass powder subjected to surface treatment. In the Fischer-Tropsch wax emulsion, the mass ratio of the net Fischer-Tropsch wax to the biomass powder is 1: 20.
After the surface treatment, the hydrophobicity of the surface of the biomass powder can be improved, and the fat solubility of the biomass powder can be increased.
(3) Pressure treatment
And (3) loading the biomass powder subjected to surface treatment in a pressure die, and compacting for 18h under the pressure of 6MPa to eliminate the internal stress of the biomass powder, thereby obtaining the biomass powder subjected to pressure treatment.
(4) Mixing material
Mixing the biomass powder subjected to pressure treatment by 40%, PLA powder and PHA powder by 50%, natural rubber powder by 8.3%, antioxidant (citric acid) by 1.5% and nano-silver oxide by 0.2% to obtain mixed powder.
(5) Preparation of polyacetal protectant solution
Firstly preparing a polyacetal protectant, which comprises the following components: 30 parts by mass of PVB, 30 parts by mass of PVFA, 2 parts by mass of PVAC-1 type and 2 parts by mass of PVAC-2 type.
A solution of polyacetal protectant was then prepared: the polyacetal protectant was dissolved in ethanol to prepare a colorless transparent solution having a concentration of 12 wt%, thereby obtaining a polyacetal protectant solution.
(6) Granulating
And (3) mixing the mixed powder prepared in the step (5) with the polyacetal protectant solution prepared in the step (6), fully stirring, adding a proper amount of starch of 4 percent to prepare a smooth dough, coating silicone oil (release agent) on the inner wall and the screw of an extruder, extruding into strips and granules by the extruder at 25 ℃, and drying in a fume hood to obtain the degradable plastic master batch.
(7) Preparation of degradable plastic food packaging bag
Mixing the following ingredients in proportion:
60 wt% of degradable plastic master batch, 5 wt% of plasticizer phthalic diester, 5 wt% of toughening agent (302 polyester), 20 wt% of filler, 5 wt% of PVB protective agent and 5 wt% of silane coupling agent (KH550) which are mixed to 100%. Then, uniformly mixing the components, finally extruding and molding a degradable plastic film (with the thickness of 1mm) by adopting a screw machine, and preparing the plastic film into a food plastic bag through hot-pressing compounding. Wherein the screw temperature of the screw extruder is 170 ℃. Wherein, the filler is prepared by mixing light calcium carbonate and kaolin in a ratio of 1: 1. All fillers come from nature and return to nature after degradation.
The degradable plastic food bag of the embodiment can be suitable for the environment with the temperature of 0-50 ℃. Of course, lower environments, such as those placed in a refrigerator at-20 deg.C, are also useful. The durability in use of this example is similar to that of a common polyethylene plastic bag. The food plastic bag of the embodiment can not release ethylene by itself, and can also catalyze and decompose the ethylene released by mature fruits, so that the excessive ripening, deterioration, rot and the like of the fruits can be delayed.
Example 2
The embodiment prepares a food packaging box, and the preparation method comprises the following steps:
(1) preparation of Biomass powder
And crushing the dried wheat straws, the bean straws, the corn stalks and the sorghum stalks, and sieving the crushed materials by a 100-mesh sieve to obtain the biomass powder.
(2) Surface treatment of biomass powder
Firstly, adding a surfactant sodium dodecyl benzene sulfonate into water to prepare a solution with the concentration of 0.15 wt%, adding Fischer-Tropsch wax, wherein the mass ratio of the Fischer-Tropsch wax to the solution is 8:140, heating the solution until the Fischer-Tropsch wax is completely melted, stirring and emulsifying by using ultrasonic waves to obtain Fischer-Tropsch wax emulsion, uniformly spraying the Fischer-Tropsch wax emulsion on the surface of biomass powder, uniformly stirring, drying at 110 ℃, rubbing and scattering, and drying until the water content is below 1%, thus preparing the biomass powder subjected to surface treatment. In the Fischer-Tropsch wax emulsion, the mass ratio of the net Fischer-Tropsch wax to the biomass powder is 1: 15.
(3) Pressure treatment
And (3) loading the biomass powder subjected to surface treatment in a pressure die, and compacting for 15h under the pressure of 10MPa to eliminate the internal stress of the biomass powder, thereby obtaining the biomass powder subjected to pressure treatment.
(4) Mixing material
Mixing the biomass powder subjected to pressure treatment by 40%, PLA powder and PHA powder by 40%, natural rubber powder by 5.3%, antioxidant (citric acid) by 1.5%, nano silver oxide by 0.2%, and thermosetting phenolic resin by 13% to obtain mixed powder.
(5) Preparation of polyacetal protectant solution
Firstly preparing a polyacetal protectant, which comprises the following components: 30 parts by mass of PVB, 20 parts by mass of PVFA, 30 parts by mass of PVAC-1 type and 30 parts by mass of PVAC-2 type.
A solution of polyacetal protectant was then prepared: the polyacetal protectant was dissolved in ethanol to prepare a colorless transparent solution having a concentration of 10 wt%, thereby obtaining a polyacetal protectant solution.
(6) Granulating
And (3) mixing the mixed powder prepared in the step (5) with the polyacetal protectant solution prepared in the step (6), fully stirring, adding a proper amount of starch of 4 percent to prepare a smooth dough, coating silicone oil (release agent) on the inner wall and the screw of an extruder, extruding into strips and granules by the extruder at 60 ℃, and drying in a fume hood to obtain the degradable plastic master batch.
(7) Preparation of degradable plastic food box
Mixing the following ingredients in proportion:
60 wt% of degradable plastic master batch, 5 wt% of plasticizer phthalic diester, 5 wt% of toughening agent (302 polyester), 20 wt% of filler, 5 wt% of PVB protective agent and 5 wt% of silane coupling agent (KH550) which are mixed to 100%. Then, stirring and mixing evenly, finally adopting a screw machine to extrude and form a degradable plastic plate (the thickness is 2mm), and cutting, softening, blowing and hot-pressing the degradable plastic plate to prepare the food packaging box. Wherein the screw temperature of the screw extruder is 170 ℃. Wherein the filler is pumice powder, kaolin 1: mixing to obtain the final product. The fillers are all from nature.
The degradable food packaging box can be suitable for the environment of 0-80 ℃ and lower environment, can be used in a refrigerator of-20 ℃ and has better use durability than a disposable polyethylene fruit preservation box in a common supermarket. The food box of the embodiment can not release ethylene by itself, and can catalyze and decompose the ethylene released by mature fruits, so that the excessive ripening, deterioration, rotting and the like of the fruits can be delayed. In addition, the packaging box is superior to a food packaging box in that thermosetting phenolic resin is added as a reinforcing phase, so that the bearing strength of the food packaging box is improved, and the durability is further increased.
Example 3
The embodiment prepares a food lunch box, and the preparation method comprises the following steps:
example 3 in addition to example 2, the polyacetal protectant composition in the polyacetal protectant solution prepared in step (5) was changed as follows: 35 parts by mass of PVB, 15 parts by mass of PVFA, 80 parts by mass of PVAC-1 type and 60 parts by mass of PVAC-2 type. And (3) increasing the thickness of the degradable plastic plate extruded and formed by the screw extruder in the step (7) from 2mm to 5mm, wherein the other conditions are the same as those of the example 2.
The degradable food packaging box of the embodiment can be suitable for 0-120 ℃ environment (lower environment can be used), the use durability is equivalent to that of a PP lunch box in the market, but the PP lunch box needs 15 years for degradation and is difficult to degrade by adopting dissolving methods such as ethanol, and therefore the environment-friendly property of the lunch box of the embodiment is superior to that of the PP lunch box.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (11)
1. A low-temperature wet preparation method of degradable plastic master batches is characterized by comprising the following steps:
s1 preparation of biomass powder containing plant cellulose and lignin
Crushing dried crop straws, chaffs, nut shells, weeds, algae or wood, and sieving with a sieve of 80-120 meshes to obtain biomass powder;
s2 surface treatment of Biomass powder
Performing surface treatment on the biomass powder by adopting Fischer-Tropsch wax to improve the hydrophobicity of the surface of the biomass powder;
s3 pressure treatment
Compacting the biomass powder subjected to surface treatment for 2h-30h under the pressure of 2-10MPa to eliminate the internal stress of the biomass powder, so as to obtain the biomass powder subjected to pressure treatment;
s4, mixing the biomass powder subjected to pressure treatment with polylactic acid (PLA) powder, Polyhydroxyalkanoate (PHA) powder and a plastic modifier to obtain mixed powder;
s5 preparation of polyacetal protectant solution
The polyacetal protectant comprises at least one of polyvinyl butyral, polyvinyl formal acetaldehyde and polyvinyl butyral;
dissolving the polyacetal protectant in liquid alcohol to obtain a colorless transparent solution, wherein the colorless transparent solution is the solution of the polyacetal protectant;
s6 granulation
And mixing and stirring the mixed powder and the polyacetal protective agent solution, adding a proper amount of starch to prepare a smooth dough, coating silicone oil on the inner wall of an extruder and a screw, extruding into strips at 20-65 ℃ by using the extruder, granulating, and drying to obtain the degradable plastic master batch.
2. The method according to claim 1, wherein in step S1, the biomass powder is prepared by sieving with a 100-mesh standard sieve; preferably, the crop stalks are rice straws, wheat straws, bean straws, corn stalks, sorghum stalks or cotton stalks.
3. The method according to claim 1, wherein in step S2, the method for surface-treating the biomass powder with the fischer-tropsch wax comprises: firstly adding a surfactant into water to prepare a solution, then adding Fischer-Tropsch wax, heating until the Fischer-Tropsch wax is completely melted, emulsifying by using ultrasonic waves to obtain Fischer-Tropsch wax emulsion, uniformly spraying the Fischer-Tropsch wax emulsion on the surface of the biomass powder, uniformly stirring, drying, rubbing and scattering, and drying until the water content is below 1%, thereby preparing the biomass powder subjected to surface treatment.
4. The method according to claim 3, wherein in step S2, the surfactant is added to water to prepare a solution having a mass concentration of 0.03 wt% to 0.4 wt%; the mass ratio of the added Fischer-Tropsch wax to the solution is 4-8: 100-150.
5. The preparation method according to claim 3 or 4, wherein in step S2, the Fischer-Tropsch wax emulsion is used in an amount of: wherein the mass ratio of the Fischer-Tropsch wax to the biomass powder is 1: 9-25.
6. The preparation method according to claim 1, wherein in step S4, the mass ratio of each component in the mixed powder is: 10-40 wt% of biomass powder, 40-60 wt% of PLA and PHA powder and 3-15 wt% of plastic modifier; the plastic modifier is natural rubber.
7. The preparation method according to claim 6, wherein in step S4, 13-35 wt% of a reinforcing material is further added to the mixed powder, wherein the reinforcing material is a thermosetting resin.
8. The preparation method according to claim 6 or 7, wherein in step S4, 0.5-3.0 wt% of antioxidant and/or 0.05-0.2 wt% of nano silver oxide is further added to the mixed powder.
9. The method according to claim 1, wherein in step S5, the polyacetal protectant composition is one of the following three compositions:
the composition is as follows: 1-35 parts by mass of polyvinyl butyral (PVB), 1-45 parts by mass of polyvinyl methyl acetaldehyde (PVFA), 0-15 parts by mass of polyvinyl butyral (PVAC)1 type and 0-15 parts by mass of polyvinyl butyral (PVAC)2 type;
the composition is two: 1-35 parts by mass of polyvinyl butyral (PVB), 1-45 parts by mass of polyvinyl methyl acetaldehyde (PVFA), 15-60 parts by mass of polyvinyl butyral (PVAC)1 type and 15-60 parts by mass of polyvinyl butyral (PVAC)2 type;
the composition is three: 1-35 parts of polyvinyl butyral (PVB), 1-45 parts of polyvinyl methyl acetaldehyde (PVFA), 60-120 parts of polyvinyl butyral (PVAC)1 type and 60-120 parts of polyvinyl butyral (PVAC)2 type.
10. The method according to claim 1 or 9, wherein the polyacetal protectant is dissolved in ethanol in step S5 to prepare a colorless transparent solution having a concentration of 3% to 15% by weight, thereby obtaining a polyacetal protectant solution.
11. A preparation method of a degradable plastic material comprises the following steps:
uniformly mixing the degradable plastic master batch prepared by the preparation method of any one of claims 1-10 with a filler and an auxiliary agent, and extruding by using a screw machine to prepare a degradable plastic material;
wherein, the components are mixed according to the following proportion:
50-65 wt% of degradable plastic master batch, 5-10 wt% of plasticizer, 5-10 wt% of toughening agent, 5-25 wt% of filler, 5-20 wt% of PVB protective agent and 5-10 wt% of silane coupling agent, and mixing to 100%; then, uniformly stirring, and finally extruding and molding the degradable plastic material by adopting a screw machine; the screw temperature of the screw extruder is 120-240 ℃.
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