CN111647183A - Preparation method of inorganic micropowder/PBAT full-degradable composite film - Google Patents
Preparation method of inorganic micropowder/PBAT full-degradable composite film Download PDFInfo
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- CN111647183A CN111647183A CN202010572177.4A CN202010572177A CN111647183A CN 111647183 A CN111647183 A CN 111647183A CN 202010572177 A CN202010572177 A CN 202010572177A CN 111647183 A CN111647183 A CN 111647183A
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- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229920001896 polybutyrate Polymers 0.000 title claims abstract 13
- 239000000843 powder Substances 0.000 claims abstract description 49
- 238000010096 film blowing Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 20
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 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 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- 239000010445 mica Substances 0.000 claims description 4
- 229910052618 mica group Inorganic materials 0.000 claims description 4
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 3
- 239000010440 gypsum Substances 0.000 claims description 3
- 229910052602 gypsum Inorganic materials 0.000 claims description 3
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000004575 stone Substances 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000004033 plastic Substances 0.000 description 6
- 229920003023 plastic Polymers 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- -1 Polybutylene terephthalate adipate Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920008262 Thermoplastic starch Polymers 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004595 color masterbatch Substances 0.000 description 1
- 229920006238 degradable plastic Polymers 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000004628 starch-based polymer Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- 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
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
-
- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- 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
- C08K3/34—Silicon-containing compounds
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention provides a preparation method of an inorganic micro powder/PBAT full-degradable composite film, which is characterized in that a certain proportion of inorganic micro powder is added before the process of producing the PBAT film by hot melting and film blowing to produce the full-degradable composite film with excellent performance, wherein the inorganic micro powder is derived from various stone powder in the nature, and has rich reserve and low price; the addition of a certain amount of inorganic micro powder not only reduces the easy adhesion property of the PBAT film, but also improves the stiffness of the film, which is beneficial to the PBAT film blowing bag making process, and meanwhile, the addition of the inorganic micro powder reduces the production cost and provides a shortcut for the rapid popularization and application of fully degradable materials.
Description
Technical Field
The invention relates to a degradable composite film, in particular to a preparation method of an inorganic micropowder/PBAT fully-degradable composite film, belonging to the technical field of packaging materials.
Technical Field
Polybutylene terephthalate adipate (PBAT) is a novel degradable plastic, has excellent mechanical properties (tensile strength and elongation at break) and very good film forming property, and is an ideal green and environment-friendly film packaging material. But the high price currently inhibits its large-scale use. The PBAT film has excellent mechanical property, but the PBAT molecular chain contains benzene rings, has larger molecular chain polarity and shows good adhesiveness, so that the film produced by film blowing is adhered without opening.
In the publication CN105086395A patent, felipine et al propose biodegradable composites blended with PLA and PBAT, with the addition of a compatibilizer and a plasticizer. Yuanliang in publication No. CN103627153A, a fully biodegradable composite material using a twin screw extruder with PLA and PBAT as the matrix and thermoplastic starch and filler as additives was proposed. Liu Eillin et al in open No. CN101724242A propose PPC and PBAT, PCL and PLA blends and preparation method. In publication No. CN108102318A, Wushengyan et al propose a biodegradable film prepared by mixing PLA, PBAT and PBS as matrix, food-grade agricultural waste, quality modifier and organic decomposing bacteria. In the past, the research of patents focuses on blending other bio-based plastics to improve the film forming property of the bio-based plastics, and the application of the bio-based plastics to inorganic micro powder is relatively simple.
The inorganic micro powder is from stones in nature, and has low price, rich yield and various varieties. The inorganic micro powder is used as a plastic cheap agent, so that the production cost can be effectively reduced, and the good mechanical property of a plastic matrix is kept. The invention adopts PBAT as the only matrix and environment-friendly inorganic micro powder as an additive for improving the film blowing production. The inorganic micro powder can be well dispersed in the PBAT composite film, and simultaneously, the softness and easy adhesion characteristics of the composite film are reduced, so that the later processing and bag making are facilitated. The invention takes the performance and the production cost of the fully degradable film into consideration, meets the concept of 'green packaging', is beneficial to popularization and application in China and even all over the world, and has huge market prospect.
Disclosure of Invention
In order to overcome the problems of high cost, easy adhesion and the like of the existing degradable composite film, the invention aims to provide a preparation method of an inorganic micropowder/PBAT fully-degradable composite film, which has optimized performance and reduced production cost so as to meet the market demand of the public.
The inorganic micro powder is obtained by crushing various stones in the nature, is safe and environment-friendly, and is low in cost and easy to obtain.
In order to achieve the purpose, the technical scheme of the invention comprises the following steps:
1) carrying out cold material blending on a certain proportion of inorganic micro powder and PBAT master batches to obtain a blending raw material;
2) preparing the blending raw material obtained in the step 1) into an inorganic micropowder/PBAT fully-degradable composite film by a screw extruder and a film blowing process.
The inorganic micro powder is one or more of various stone powders, and further is one or more of calcium carbonate micro powder, silica micro powder (quartz powder), talcum powder, mica powder, gypsum powder, montmorillonite powder and hydromica powder.
The mesh number of the inorganic micro powder is 500-10000 meshes.
The addition amount of the inorganic micro powder accounts for 0.5 to 120 percent of the PBAT master batch.
The thickness of the composite film is 5-200 mu m, and the width of the composite film is 0.01-1 m.
The inorganic micropowder/PBAT fully-degradable composite film prepared by the invention can be directly used and can be applied to the aspects of mulching films, packaging films and the like; the film can be wound to produce fully degradable bags with different specifications through a bag making process, can be applied to production and living aspects such as packaging bags, garbage bags, shopping bags and the like, accords with sustainable development and the concept of 'green packaging', meets the performance requirements of different application fields, and has great market potential.
The mechanical properties of the composite films, including elongation at break and tensile stress, were characterized using a universal tester. The micrometer screw is used for measuring the thickness of the composite film. And observing the surface of the composite film by using a scanning electron microscope, and observing the dispersion of the inorganic micro powder added with high proportion in the composite film.
Compared with the background art, the invention has the beneficial effects that:
(1) according to the invention, various stone micro powders with rich sources and low price are selected as additives, so that the cost is reduced, the film blowing production process of PBAT is improved, the bag making and printing of PBAT are improved, different inorganic micro powders endow the composite film with different smoothness and stiffness, and the composite film is suitable for the consumption of the public;
(2) the method has simple process, and can realize good dispersion of inorganic micropowder in the PBAT film by only simple cold material blending, without additional compatilizer and plasticizer, or without melt blending with other bio-based plastics to improve the film blowing process.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a fully degradable composite film by inorganic micropowder/PBAT blending blown film.
FIG. 2 is a graph showing the mechanical properties of a calcium carbonate/PBAT composite film prepared in example 1 and having a relative content of 25%.
FIG. 3 is a microscopic morphology of the 50% relative talc powder and quartz powder (1: 1)/PBAT composite film prepared in example 3.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The invention is further illustrated below with reference to specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. In addition, after reading the teaching of the present invention, those skilled in the art can make various changes or modifications to the invention, and these equivalents also fall within the scope of the claims appended to the present application.
Example 1
As shown in FIG. 1, 5000 mesh calcium carbonate micropowder (CaCO)3Limestone) is added into a hopper, the mixture is mixed with PBAT master batch, the amount of calcium carbonate micro powder is 25 percent of that of the PBAT master batch, the calcium carbonate micro powder and the PBAT master batch are fully and uniformly mixed, the mixed raw materials are processed by a screw extruder and a film blowing process to produce a composite film, the composite film is wound, the temperature of each area of the screw extruder is between 120 and 150 ℃, the thickness of the composite film is 50 mu m, and the width of the composite film is 0.01 m.
The composite film with narrow width can be applied to the external package of disposable straws, chopsticks and the like, and the composite film with wider width can be applied to shopping bags, packaging bags, takeaway bags and the like with various specifications. FIG. 2 shows the mechanical property test of calcium carbonate/PBAT composite film with a relative content of 25%, which shows a strength of 32MPa and an elongation at break of 110%, and the performance is very excellent.
Example 2
Adding 500-mesh mica powder (from mica stone) into a hopper, blending with PBAT master batch, wherein the amount of the silicon powder is 0.5%, 5% and 10% of that of the PBAT master batch, and fully and uniformly mixing; the blended raw materials are subjected to film blowing process to produce a composite film, the composite film is wound, the thickness of the obtained composite film is 10-50 mu m, the width of the obtained composite film is 0.2-1 m, the wound composite film can be used as an agricultural mulching film, and the wound composite film is subjected to bag making process to produce fully degradable bags of different specifications.
Example 3
Mixing 2000-mesh talcum powder and quartz powder in a ratio of 1: 1, adding the powder material into a hopper, mixing the powder material and the PBAT master batch, wherein the powder material is 50% of the PBAT master batch, fully and uniformly mixing, producing a composite film by the mixed raw materials through a film blowing process, winding, controlling the temperature of each area of a screw extruder to be between 120 and 150 ℃, controlling the thickness of the composite film to be 5-30 mu m and the width to be 0.15-0.35 m, and producing the fully degradable bags with different specifications by the wound composite film through a bag making process.
FIG. 3 shows the micro-topography of the talc powder and quartz powder (1: 1)/PBAT composite film with a relative content of 50%, which shows good dispersibility and performance meeting the application requirements.
Example 4
Adding 10000-mesh red montmorillonite powder into a hopper, blending with PBAT master batch, wherein the powder is 10-20% of the PBAT master batch, and fully and uniformly mixing; the blended raw materials are subjected to film blowing process to produce a composite film, the composite film is wound, the thickness of the composite film is 20-35 mu m, the width of the composite film is 0.15-0.5 m, the wound composite film is subjected to bag making process to produce fully-degradable bags of different specifications, color master batches are not required to be added into the obtained fully-degradable bags, and uniform red distribution is shown.
Example 5
The calcium carbonate micro powder in the embodiment 1 is replaced by hydromica powder, other preparation conditions and steps are kept unchanged, and the inorganic micro powder/PBAT fully-degradable composite film is prepared.
Example 6
Adding gypsum powder of 5000 meshes into a hopper, blending with the PBAT master batch, wherein the amount of calcium carbonate micro powder is 0.5%, 25%, 50%, 75%, 100% and 120% of the PBAT master batch respectively, and fully and uniformly mixing; the blended raw materials are processed by a screw extruder and a film blowing process to produce a composite film, the composite film is wound, the temperature of each area of the screw extruder is between 120 and 150 ℃, the thickness of the composite film is 5 mu m, 100 mu m and 200 mu m, the width of the composite film is 0.01, 0.1 and 1m, and the wound composite film can be processed by a bag making process to produce fully-degradable bags with different specifications.
Claims (5)
1. A preparation method of an inorganic micropowder/PBAT full-degradable composite film is characterized by comprising the following specific steps:
1) carrying out cold material blending on a certain proportion of inorganic micro powder and PBAT master batches to obtain a blending raw material;
2) preparing the blending raw material obtained in the step 1) into an inorganic micropowder/PBAT fully-degradable composite film by a screw extruder and a film blowing process.
2. The preparation method of the inorganic micropowder/PBAT fully-degradable composite film according to claim 1, wherein the inorganic micropowder in the step (1) is one or more of calcium carbonate micropowder, silica micropowder (quartz powder), talcum powder, mica powder, gypsum powder, montmorillonite powder and hydromica powder.
3. The preparation method of the inorganic micropowder/PBAT fully-degradable composite film according to claim 1, wherein the mesh number of the inorganic micropowder in the step (1) is 500-10000 meshes.
4. The method for preparing the inorganic micropowder/PBAT fully-degradable composite film according to claim 1, wherein the addition amount of the inorganic micropowder in the step (1) accounts for 0.5-120% of that of the PBAT master batch.
5. The preparation method of the inorganic micropowder/PBAT fully-degradable composite film according to claim 1, wherein the thickness of the composite film in the step (2) is 5-200 μm, and the width is 0.01-1 m.
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| CN202010572177.4A CN111647183A (en) | 2020-06-22 | 2020-06-22 | Preparation method of inorganic micropowder/PBAT full-degradable composite film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112812516A (en) * | 2020-12-31 | 2021-05-18 | 佛山安亿纳米材料有限公司 | Composite material of inorganic filler doped degradable film and preparation method thereof |
| CN112810109A (en) * | 2020-12-31 | 2021-05-18 | 佛山安亿纳米材料有限公司 | Preparation method of multi-morphology multi-size inorganic filler doped degradable film |
| CN113580700A (en) * | 2021-08-02 | 2021-11-02 | 浙江大成新材料科技有限公司 | High-strength double-layer composite fully-degradable packaging material and preparation method and application thereof |
| CN114478123A (en) * | 2022-02-24 | 2022-05-13 | 内蒙古科学技术研究院 | Degradable bioactive liquid mulching film and preparation method thereof |
| CN115678214A (en) * | 2022-10-10 | 2023-02-03 | 万华化学（宁波）有限公司 | High-stiffness degradable transparent functional master batch and preparation method and application thereof |
| CN116789970A (en) * | 2023-07-17 | 2023-09-22 | 南京大学 | PBAT-PLA-based biodegradable hot melt adhesive and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112812516A (en) * | 2020-12-31 | 2021-05-18 | 佛山安亿纳米材料有限公司 | Composite material of inorganic filler doped degradable film and preparation method thereof |
| CN112810109A (en) * | 2020-12-31 | 2021-05-18 | 佛山安亿纳米材料有限公司 | Preparation method of multi-morphology multi-size inorganic filler doped degradable film |
| CN113580700A (en) * | 2021-08-02 | 2021-11-02 | 浙江大成新材料科技有限公司 | High-strength double-layer composite fully-degradable packaging material and preparation method and application thereof |
| CN114478123A (en) * | 2022-02-24 | 2022-05-13 | 内蒙古科学技术研究院 | Degradable bioactive liquid mulching film and preparation method thereof |
| CN115678214A (en) * | 2022-10-10 | 2023-02-03 | 万华化学（宁波）有限公司 | High-stiffness degradable transparent functional master batch and preparation method and application thereof |
| CN115678214B (en) * | 2022-10-10 | 2023-12-19 | 万华化学（宁波）有限公司 | High-stiffness degradable transparent functional master batch as well as preparation method and application thereof |
| CN116789970A (en) * | 2023-07-17 | 2023-09-22 | 南京大学 | PBAT-PLA-based biodegradable hot melt adhesive and preparation method and application thereof |
| CN116789970B (en) * | 2023-07-17 | 2024-03-26 | 南京大学 | PBAT-PLA-based biodegradable hot melt adhesive and preparation method and application thereof |
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