CN113214615B - Ternary complete biodegradable film and preparation method thereof - Google Patents
Ternary complete biodegradable film and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- 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
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- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
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- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention provides a ternary complete biodegradable film, which comprises the following raw materials: 40-65 parts of polybutylene terephthalate-adipate resin, 15-30 parts of modified starch, 9-40 parts of polypropylene carbonate, 0.1-1 part of an opening agent, 0.5-2 parts of a lubricant, 3-13 parts of a plasticizer and 1-5 parts of talcum powder; the modified starch is modified starch by a modifier, and the modifier is citric acid or maleic anhydride, and is mixed with one of a titanate coupling agent, an aluminate coupling agent and a silane coupling agent; the opening agent is erucamide; the lubricant is one or more of ethylene bis stearamide and calcium stearate; the plasticizer is one or more of glycerol and sorbitol. The prepared completely degradable film has the advantages of good mechanical property and complete biodegradation by adding the modified starch and selecting and limiting the content of the auxiliary agent, and has wide application value.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a ternary complete biodegradable film and a preparation method thereof.
Background
The environmental pollution caused by petroleum-based plastics is increasing, and the replacement of fully degradable plastics is urgently needed. Polybutylene terephthalate-adipate (PBAT) is a fully degradable plastic widely studied at home and abroad. But the thin film prepared by pure PBAT is softer, has smaller strength and higher cost, and is limited in a plurality of application fields. Thus, during application processing, PBAT is often blend modified with other materials to improve its application properties.
In the prior art, the cost of materials can be greatly reduced by blending and modifying with starch, and the starch is a degradable natural polymer, so that the cost of the polybutylene terephthalate-adipic acid/starch film after blending and modifying is greatly reduced, but the film is poor in water resistance and does not resist the humid environment.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a ternary full biodegradable film and a preparation method thereof, which have better mechanical properties, water resistance and moisture resistance.
In order to achieve the above purpose, the invention provides a ternary full biodegradable film, which comprises the following raw materials:
40-65 parts of polybutylene terephthalate-adipate resin, 15-30 parts of modified starch, 9-40 parts of polypropylene carbonate, 0.1-1 part of an opening agent, 0.5-2 parts of a lubricant, 3-13 parts of a plasticizer and 1-5 parts of talcum powder;
the modified starch is modified starch by a modifier, and the modifier is citric acid or maleic anhydride, and is mixed with one of a titanate coupling agent, an aluminate coupling agent and a silane coupling agent;
the opening agent is erucamide;
the lubricant is one or more of ethylene bis stearamide and calcium stearate;
the plasticizer is one or more of glycerol and sorbitol.
The prepared completely degradable film has good mechanical property and full biodegradation advantage by adding the modified starch, selecting the auxiliary agent and limiting the content, can be completely degraded into water and carbon dioxide in soil, is beneficial to protecting the environment, and has wide application value.
Preferably, the raw materials of the invention comprise:
45-60 parts of polybutylene terephthalate-adipate resin, 20-25 parts of modified starch, 15-35 parts of polypropylene carbonate, 0.2-0.5 part of a pore opener, 1-2 parts of a lubricant, 5-10 parts of a plasticizer and 2-4 parts of talcum powder.
Preferably, the modified starch is modified starch by a modifier, and preferably, the modified starch is obtained by mixing the modifier and the starch for modification treatment.
Preferably, the modified starch is modified corn starch or tapioca starch.
Preferably, the weight ratio of the starch and the modifier in the modified starch is (97-99): (1-3).
The modifier is preferably citric acid or maleic anhydride, and is mixed with one of a titanate coupling agent, an aluminate coupling agent and a silane coupling agent.
In the preferred modifier, the weight ratio of the citric acid or the maleic anhydride to one of the titanate coupling agent, the aluminate coupling agent and the silane coupling agent is 1: (0.2-1).
Preferably, the polypropylene carbonate has a weight average molecular weight of 6X 10 4 ～5×10 5 g/mol。
The invention provides a preparation method of the ternary full biodegradable film, which comprises the following steps:
s1) mixing starch with a modifier for modification treatment to obtain modified starch;
s2) mixing and extruding polybutylene terephthalate-adipate resin, modified starch, polypropylene carbonate, talcum powder, a pore-forming agent, a lubricant and a plasticizer to obtain resin for film blowing;
s3) film blowing is carried out on the resin for film blowing, and the ternary full biodegradable film is obtained.
In the invention, the extrusion temperature is preferably 80-160 ℃, the screw rotation speed is 200-350 rpm, and the processing temperature of the blown film is 145-175 ℃.
Compared with the prior art, the invention provides a ternary complete biodegradable film, which comprises the following raw materials: 40-65 parts of polybutylene terephthalate-adipate resin, 15-30 parts of modified starch, 9-40 parts of polypropylene carbonate, 0.1-1 part of an opening agent, 0.5-2 parts of a lubricant, 3-13 parts of a plasticizer and 1-5 parts of talcum powder; the modified starch is modified starch by a modifier, and the modifier is citric acid or maleic anhydride, and is mixed with one of a titanate coupling agent, an aluminate coupling agent and a silane coupling agent; the opening agent is erucamide; the lubricant is one or more of ethylene bis stearamide and calcium stearate; the plasticizer is one or more of glycerol and sorbitol.
According to the invention, the polybutylene terephthalate-adipate resin is mixed with the modified starch, the polypropylene carbonate and the rest of auxiliary agents, and the specific proportion is combined, so that the film prepared from the composition finally prepared has the advantages of high tensile strength and tearing strength, good elastic modulus, good breaking elongation, good barrier property, good degradation performance, strong water resistance and moisture resistance and the like due to the compatibilization effect between the polybutylene terephthalate-adipate resin, the starch and the polypropylene carbonate of the mixture of the citric acid or the maleic anhydride and the titanate coupling agent, the aluminate coupling agent or the silane coupling agent. And because of the addition of low-cost starch, plasticizer and talcum powder, the cost of the film is greatly reduced, the prices of the biodegradable film and film bag products thereof can be better reduced, and the market demands of shopping bags, express bags, garbage bags and mulching films are met.
Detailed Description
In order to further illustrate the present invention, the ternary full biodegradable film and the preparation method thereof provided by the present invention are described in detail below with reference to examples.
The PBAT in the following examples was purchased from polyester Co., ltd. In mountain Tuber, xinjiang, model TH801T; starch was purchased by Shandong Shouguang golden corn development Co., ltd; the polypropylene carbonate is prepared by copolymerizing carbon dioxide and propylene oxide under the action of a catalyst according to a method disclosed in a patent CN101402726B of the issued Chinese invention, wherein the weight average molecular weight is 3.0x10 5 Gram/mole; talcum powder, model SK-98 purchased by Liaoning essence New Material Co., ltd; the opening agent is erucamide, purchased from Jiangxi Weike oil chemistry Co., ltd; the lubricant is ethylene bis stearamide, purchased from Sichuan Tianyu oil chemistry Co., ltd; other adjuvants are not limited to purchase sources. The film tensile properties in the following examples were tested in accordance with GB/T1010.3-2006; tear strength was tested according to QB/T1130-91; the surface contact angle is a film sample tested by DSA100 type contact angle measuring instrument of Kruss company, germany.
Example 1
(1) Weighing 98.1 parts of starch, 1.5 parts of maleic anhydride and 0.4 part of titanate coupling agent; the adding sequence is starch, maleic anhydride and titanate coupling agent in turn; the mixing speed is increased to high speed, the mixture is stirred to 90 ℃ at high speed, and the mixture is continuously stirred for about 3 minutes to obtain the modified starch;
(2) 56 parts of PBAT, 21 parts of modified starch, 9 parts of polypropylene carbonate, 9 parts of sorbitol liquid, 3 parts of talcum powder, 0.5 part of erucamide, 0.5 part of calcium stearate and 1 part of ethylene bisstearamide are weighed;
(3) Adding the raw materials into a high-speed stirrer according to a certain sequence, wherein the addition sequence is PBAT, modified starch, polypropylene carbonate, talcum powder, erucamide, calcium stearate, ethylene bis-stearamide and sorbitol liquid; the mixing speed is started to be high, and the materials can be discharged after being stirred for about 10 minutes at high speed;
(4) Adding the mixed raw materials into a hopper of a double-screw extruder, setting the processing temperature of each temperature zone of the extruder, controlling the operation temperature to be 80-160 ℃, and obtaining the blown film modified resin through bracing, air-cooling and granulating;
(5) And (3) putting the film blowing modified resin into a film blowing machine for film blowing processing, wherein the temperature of each temperature zone of the film blowing machine is 145-175 ℃, and finally obtaining the fully-degradable film.
Example 2
(1) Weighing 98.1 parts of starch, 1.5 parts of maleic anhydride and 0.4 part of aluminate coupling agent; the adding sequence is starch, maleic anhydride and aluminate coupling agent in turn; the mixing speed is increased to high speed, the mixture is stirred to 90 ℃ at high speed, and the mixture is continuously stirred for about 3 minutes to obtain the modified starch;
(2) 52 parts of PBAT, 20 parts of modified starch, 16 parts of polypropylene carbonate, 8 parts of sorbitol liquid, 2.5 parts of talcum powder, 0.5 part of erucamide, 0.5 part of calcium stearate and 0.5 part of ethylene bisstearamide are weighed;
(3) Adding the raw materials into a high-speed stirrer according to a certain sequence, wherein the addition sequence is PBAT, modified starch, polypropylene carbonate, talcum powder, erucamide, calcium stearate, ethylene bis-stearamide and sorbitol liquid; the mixing speed is started to be high, and the materials can be discharged after being stirred for about 10 minutes at high speed;
(4) Adding the mixed raw materials into a hopper of a double-screw extruder, setting the processing temperature of each temperature zone of the extruder, controlling the operation temperature to be 80-160 ℃, and obtaining the blown film modified resin through bracing, air-cooling and granulating;
(5) And (3) putting the film blowing modified resin into a film blowing machine for film blowing processing, wherein the temperature of each temperature zone of the film blowing machine is 145-175 ℃, and finally obtaining the fully-degradable film.
Example 3
(1) Weighing 98.1 parts of starch, 1.5 parts of maleic anhydride and 0.4 part of silane coupling agent (KH 550); the adding sequence is starch, maleic anhydride and silane coupling agent in turn; the mixing speed is increased to high speed, the mixture is stirred to 90 ℃ at high speed, and the mixture is continuously stirred for about 3 minutes to obtain the modified starch;
(2) Weighing 48 parts of PBAT, 18 parts of modified starch, 22 parts of polypropylene carbonate, 8 parts of sorbitol liquid, 2.5 parts of talcum powder, 0.5 part of erucamide, 0.5 part of calcium stearate and 0.5 part of ethylene bisstearamide;
(3) Adding the raw materials into a high-speed stirrer according to a certain sequence, wherein the addition sequence is PBAT, modified starch, polypropylene carbonate, talcum powder, erucamide, calcium stearate, ethylene bis-stearamide and sorbitol liquid; the mixing speed is started to be high, and the materials can be discharged after being stirred for about 10 minutes at high speed;
(4) Adding the mixed raw materials into a hopper of a double-screw extruder, setting the processing temperature of each temperature zone of the extruder, controlling the operation temperature to be 80-160 ℃, and obtaining the blown film modified resin through bracing, air-cooling and granulating;
(5) And (3) putting the film blowing modified resin into a film blowing machine for film blowing processing, wherein the temperature of each temperature zone of the film blowing machine is 145-175 ℃, and finally obtaining the fully-degradable film.
Example 4
(1) Weighing 98.1 parts of starch, 1.5 parts of maleic anhydride and 0.4 part of titanate coupling agent; the adding sequence is starch, maleic anhydride and titanate coupling agent in turn; the mixing speed is increased to high speed, the mixture is stirred to 90 ℃ at high speed, and the mixture is continuously stirred for about 3 minutes to obtain the modified starch;
(2) Weighing 44 parts of PBAT, 17 parts of modified starch, 28 parts of polypropylene carbonate, 7.5 parts of sorbitol liquid, 2.4 parts of talcum powder, 0.1 part of erucamide, 0.5 part of calcium stearate and 0.5 part of ethylene bis-stearamide;
(3) Adding the raw materials into a high-speed stirrer according to a certain sequence, wherein the addition sequence is PBAT, modified starch, polypropylene carbonate, talcum powder, erucamide, calcium stearate, ethylene bis-stearamide and sorbitol liquid; the mixing speed is started to be high, and the materials can be discharged after being stirred for about 10 minutes at high speed;
(4) Adding the mixed raw materials into a hopper of a double-screw extruder, setting the processing temperature of each temperature zone of the extruder, controlling the operation temperature to be 80-160 ℃, and obtaining the blown film modified resin through bracing, air-cooling and granulating;
(5) And (3) putting the film blowing modified resin into a film blowing machine for film blowing processing, wherein the temperature of each temperature zone of the film blowing machine is 145-175 ℃, and finally obtaining the fully-degradable film.
Performance measurement:
the mechanical properties of the prepared fully degradable film were measured, and the results are shown in table 1:
TABLE 1 Properties of the materials prepared in examples 1 to 4
| Performance of | Example 1 | Example 2 | Example 3 | Example 4 |
| Transverse tensile Strength (MPa) | 17.6 | 17.1 | 17.3 | 15.5 |
| Elongation at break in transverse direction (%) | 558 | 550 | 610 | 541 |
| Transverse tear Strength (KN/m) | 103.1 | 124.7 | 111.1 | 119.8 |
| Longitudinal tensile Strength (MPa) | 20.4 | 18.5 | 17.1 | 17.6 |
| Elongation at break in machine direction (%) | 348 | 325 | 307 | 377 |
| Longitudinal tear Strength (KN/m) | 97.8 | 112.2 | 107.8 | 99.0 |
| Surface contact angle (°) | 70.48 | 72.14 | 73.45 | 74.81 |
As can be seen from table 1, as the content of the polypropylene carbonate is increased from 9% to 28%, the tensile strength, the tearing strength and the elongation at break are all kept at relatively high values, the film has better comprehensive mechanical properties, and the mutual interfacial bonding capability between the polybutylene terephthalate and the adipic acid/the starch/the polypropylene carbonate can be obviously improved due to the effect of the maleic anhydride and the coupling agent, the plasticizing effect on the starch can be effectively improved under the plasticizing effect of the plasticizer, and the mechanical properties of the material are obviously improved; the surface contact angle is obviously improved, the hydrophobicity of the film is enhanced, and the addition of the polypropylene carbonate improves the moisture resistance of the starch-containing film and can improve the shelf life of the film. Under the synergistic effect of a plurality of auxiliary agents, the ternary blend has better compatibility. The film has simple processing technology and low cost, has complete biodegradability, can replace a polyethylene non-degradable film, can be applied to film bag products such as shopping bags, garbage bags, mulching films and the like, is beneficial to environmental protection, and has very important application value.
The invention provides a completely biodegradable film and a preparation method thereof, which mainly comprise polybutylene terephthalate-adipic acid/starch/polypropylene carbonate and an auxiliary agent thereof, and can be realized by appropriately improving process parameters by a person skilled in the art by referring to the content of the invention.
It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and they are intended to be within the scope of the present invention. The method and application of the present invention have been described by means of preferred embodiments, the description of which is only intended to aid in understanding the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (9)
1. The ternary completely biodegradable film is characterized by comprising the following raw materials:
40-65 parts of polybutylene terephthalate-adipate resin, 15-30 parts of modified starch, 9-40 parts of polypropylene carbonate, 0.1-1 part of an opening agent, 0.5-2 parts of a lubricant, 3-13 parts of a plasticizer and 1-5 parts of talcum powder;
the modified starch is modified starch by a modifier, and the modifier is citric acid or maleic anhydride, and is mixed with one of a titanate coupling agent, an aluminate coupling agent and a silane coupling agent;
the opening agent is erucamide;
the lubricant is one or more of ethylene bis stearamide and calcium stearate;
the plasticizer is one or more of glycerol and sorbitol.
2. The ternary full biodegradable film according to claim 1, wherein the modified starch is modified corn starch or tapioca starch.
3. The ternary full biodegradable film according to claim 1, characterized in that the weight ratio of starch and modifier in the modified starch is (97-99): (1-3).
4. The ternary full biodegradable film according to claim 1, wherein the weight ratio of citric acid or maleic anhydride to one of titanate coupling agent, aluminate coupling agent and silane coupling agent in the modifying agent is 1: (0.2-1).
5. The ternary full biodegradable film according to claim 1, characterized in that the polypropylene carbonate has a weight average molecular weight of 6 x 10 4 ～5×10 5 g/mol。
6. The ternary full biodegradable film according to claim 1, characterized in that its raw materials comprise:
45-60 parts of polybutylene terephthalate-adipate resin, 20-25 parts of modified starch, 15-35 parts of polypropylene carbonate, 0.2-0.5 part of a pore opener, 1-2 parts of a lubricant, 5-10 parts of a plasticizer and 2-4 parts of talcum powder.
7. The method for preparing the ternary full biodegradable film according to any one of claims 1 to 6, comprising the following steps:
s1) mixing starch with a modifier for modification treatment to obtain modified starch;
s2) mixing and extruding polybutylene terephthalate-adipate resin, modified starch, polypropylene carbonate, talcum powder, a pore-forming agent, a lubricant and a plasticizer to obtain resin for film blowing;
s3) film blowing is carried out on the resin for film blowing, and the ternary full biodegradable film is obtained.
8. The method according to claim 7, wherein the extrusion temperature is 80 to 160℃and the screw rotation speed is 200 to 350 rpm.
9. The method of claim 7, wherein the blown film is processed at a temperature of 145 to 175 ℃.
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