CN113214615A - Ternary complete biodegradable film and preparation method thereof - Google Patents
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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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- 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, the modifier is citric acid or maleic anhydride, and the modified starch 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, through the addition of the modified starch and the selection and content limitation of the auxiliary agent, the prepared completely-degradable film has the advantages of good mechanical property, complete biodegradation and 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 petroleum-based plastics cause increasingly serious environmental pollution, and the petroleum-based plastics are urgently needed to replace fully-degradable plastics. Polybutylene terephthalate-adipate (PBAT) is a fully degradable plastic which is widely researched at home and abroad. However, films prepared from pure PBAT are relatively soft, have relatively low strength and relatively high cost, and are limited in many application fields. Therefore, PBAT is typically modified by blending with other materials during application processing to improve its application properties.
In the prior art, the material cost can be greatly reduced by blending and modifying the starch, the starch is a degradable natural polymer, the cost of the polybutylene terephthalate-adipate/starch film modified by blending is greatly reduced, but the film has poor water resistance and is not resistant to a damp environment.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a ternary complete biodegradable film and a preparation method thereof, wherein the ternary complete biodegradable film has good mechanical properties, water resistance and moisture resistance.
In order to achieve the aim, 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, the modifier is citric acid or maleic anhydride, and the modified starch 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, through the addition of the modified starch, the selection of the auxiliary agent and the limitation of the content, the prepared completely-degradable film has good mechanical properties, has the advantage of complete biodegradation, can be completely degraded into water and carbon dioxide in soil, is beneficial to environmental protection, and has wide application value.
Preferably, the 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 an opening agent, 1-2 parts of a lubricant, 5-10 parts of a plasticizer and 2-4 parts of talcum powder.
In the invention, the modified starch is preferably modified by a modifier, and preferably, the modifier and the starch are mixed for modification treatment to obtain the modified starch.
Preferably, the modified starch is modified corn starch or tapioca starch.
Preferably, the weight ratio of the starch to the modifier in the modified starch is (97-99): (1-3).
The modifier is preferably citric acid or maleic anhydride, mixed with one of a titanate coupling agent, an aluminate coupling agent and a silane coupling agent.
In the preferable aspect of the present invention, in the modifier, the weight ratio of citric acid or maleic anhydride to one of a titanate coupling agent, an aluminate coupling agent and a silane coupling agent is 1: (0.2 to 1).
In a preferred embodiment of the present invention, the weight average molecular weight of the polypropylene carbonate is 6X 104～5×105g/mol。
The invention provides a preparation method of the ternary complete 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, an opening agent, a lubricant and a plasticizer to obtain resin for blown film;
s3) carrying out film blowing on the film blowing resin to obtain the ternary complete biodegradable film.
The invention preferably selects the extrusion temperature of 80-160 ℃, the screw rotation speed of 200-350 r/min and the processing temperature of blown film of 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, the modifier is citric acid or maleic anhydride, and the modified starch 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, through mixing the polybutylene terephthalate-adipate resin with the modified starch, the polypropylene carbonate and other auxiliary agents and combining the specific mixture ratio, due to the compatibilization effect among the polybutylene terephthalate-adipate resin, the starch and the polypropylene carbonate by the mixture of citric acid or maleic anhydride and titanate coupling agent, aluminate coupling agent or silane coupling agent, the film prepared from the finally prepared composition has the advantages of high tensile and tearing strength, good elastic modulus, good elongation at break, good barrier property, good degradation performance, strong water resistance and moisture resistance and the like. And due to the addition of low-cost starch, plasticizer and talcum powder, the film cost is greatly reduced, the prices of biodegradable films 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 following examples are provided to describe the ternary complete biodegradable film and the preparation method thereof in detail.
PBAT in the following examples was purchased from polyester GmbH, blue Shantun, N.Y., with model number TH 801T; starch is purchased from Shandong Shouguang giant energy gold corn development Co., Ltd; the polypropylene carbonate is from the subject group of the King red donator of the Changchun applied chemistry research institute of Chinese academy of sciences, is prepared by copolymerizing carbon dioxide and propylene oxide under the action of a catalyst according to the method disclosed in the granted Chinese invention patent CN101402726B, and has the weight-average molecular weight of 3.0 multiplied by 105G/mol; talcum powder, available from Liaoning essence New materials GmbH, model SK-98; the opening agent is erucamide, purchased from grease chemical company Limited of Weike, Jiangxi; the lubricant is ethylene bis stearamide, purchased from Sichuan Tianyu oil and fat chemical Co., Ltd; other adjuvants are not limited to the source of purchase. Film stretching in the following examplesThe performance is tested by the standard of GB/T1010.3-2006; the tear strength was tested according to QB/T1130-91; the surface contact angle is a film sample tested by a DSA100 contact angle measuring instrument from Kruss, germany.
Example 1
(1) Weighing 98.1 parts of starch, 1.5 parts of maleic anhydride and 0.4 part of titanate coupling agent; adding starch, maleic anhydride and titanate coupling agent in sequence; the mixing speed is increased to a high speed, the mixture is stirred at the high speed to 90 ℃, and the mixture can be discharged after being continuously stirred for about 3 minutes, so that the modified starch is obtained;
(2) weighing 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 bis-stearamide;
(3) adding the raw materials into a high-speed stirrer according to a certain sequence, wherein the raw materials are sequentially added with PBAT, modified starch, polypropylene carbonate, talcum powder, erucamide, calcium stearate, ethylene bis-stearamide and sorbitol liquid; the mixing speed is increased to a high speed, and the materials can be discharged after being stirred at the high speed for about 10 minutes;
(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, wherein the operating temperature is 80-160 ℃, and carrying out bracing, air cooling and grain cutting to obtain blown film modified resin;
(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; adding starch, maleic anhydride and an aluminate coupling agent in sequence; the mixing speed is increased to a high speed, the mixture is stirred at the high speed to 90 ℃, and the mixture can be discharged after being continuously stirred for about 3 minutes, so that the modified starch is obtained;
(2) weighing 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 bis stearamide;
(3) adding the raw materials into a high-speed stirrer according to a certain sequence, wherein the raw materials are sequentially added with PBAT, modified starch, polypropylene carbonate, talcum powder, erucamide, calcium stearate, ethylene bis-stearamide and sorbitol liquid; the mixing speed is increased to a high speed, and the materials can be discharged after being stirred at the high speed for about 10 minutes;
(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, wherein the operating temperature is 80-160 ℃, and carrying out bracing, air cooling and grain cutting to obtain blown film modified resin;
(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); adding starch, maleic anhydride and a silane coupling agent in sequence; the mixing speed is increased to a high speed, the mixture is stirred at the high speed to 90 ℃, and the mixture can be discharged after being continuously stirred for about 3 minutes, so that the modified starch is obtained;
(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 bis stearamide;
(3) adding the raw materials into a high-speed stirrer according to a certain sequence, wherein the raw materials are sequentially added with PBAT, modified starch, polypropylene carbonate, talcum powder, erucamide, calcium stearate, ethylene bis-stearamide and sorbitol liquid; the mixing speed is increased to a high speed, and the materials can be discharged after being stirred at the high speed for about 10 minutes;
(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, wherein the operating temperature is 80-160 ℃, and carrying out bracing, air cooling and grain cutting to obtain blown film modified resin;
(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; adding starch, maleic anhydride and titanate coupling agent in sequence; the mixing speed is increased to a high speed, the mixture is stirred at the high speed to 90 ℃, and the mixture can be discharged after being continuously stirred for about 3 minutes, so that the modified starch is obtained;
(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 raw materials are sequentially added with PBAT, modified starch, polypropylene carbonate, talcum powder, erucamide, calcium stearate, ethylene bis-stearamide and sorbitol liquid; the mixing speed is increased to a high speed, and the materials can be discharged after being stirred at the high speed for about 10 minutes;
(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, wherein the operating temperature is 80-160 ℃, and carrying out bracing, air cooling and grain cutting to obtain blown film modified resin;
(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.
And (3) 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 1-4
| Performance of | Example 1 | Example 2 | Example 3 | Example 4 |
| Transverse tensile Strength (MPa) | 17.6 | 17.1 | 17.3 | 15.5 |
| Transverse elongation at Break (%) | 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 longitudinal 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 polypropylene carbonate is increased from 9% to 28%, the tensile strength, the tear strength and the elongation at break are all kept at relatively high values, the film has better comprehensive mechanical properties, the mutual interface bonding capability between the polybutylene terephthalate-adipate/the starch/the polypropylene carbonate can be obviously improved due to the action of the maleic anhydride and the coupling agent, and the plasticizing effect on the starch can be effectively improved under the plasticizing action of the plasticizer, so that the mechanical properties of the material are obviously improved; the surface contact angle is obviously improved, the hydrophobicity of the film is enhanced, the moisture resistance of the starch-containing film is improved by adding the polypropylene carbonate, and the shelf life of the film can be prolonged. Under the synergistic action of a plurality of auxiliary agents, the ternary blend has better compatibility. The film has simple processing technology, low cost and complete biodegradation performance, 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 comprises polybutylene terephthalate-adipate/starch/polypropylene carbonate and auxiliary agents thereof, and can be realized by appropriately improving process parameters by referring to the content.
It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. The method and application of the present invention have been described in terms of preferred embodiments, which are only described to aid understanding of the method and its core ideas. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (9)
1. A ternary complete 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, the modifier is citric acid or maleic anhydride, and the modified starch 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 fully biodegradable film according to claim 1, wherein said modified starch is a modified corn starch or tapioca starch.
3. The ternary fully biodegradable film according to claim 1, wherein the weight ratio of starch to modifier in said modified starch is (97-99): (1-3).
4. The ternary fully 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 said modifier is 1: (0.2 to 1).
5. The ternary completely biodegradable film according to claim 1, wherein said poly (propylene carbonate) has a weight average molecular weight of 6 x 104～5×105g/mol。
6. The ternary complete 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 an opening agent, 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 complete 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, an opening agent, a lubricant and a plasticizer to obtain resin for blown film;
s3) carrying out film blowing on the film blowing resin to obtain the ternary complete biodegradable film.
8. The method of claim 7, wherein the extrusion temperature is 80 to 160 ℃ and the screw rotation speed is 200 to 350 rpm.
9. The method according to claim 7, wherein the blown film is processed at a temperature of 145 to 175 ℃.
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| CN114836012A (en) * | 2022-04-14 | 2022-08-02 | 水发信达(山东)再生资源科技有限公司 | Completely biodegradable garbage bag film material and preparation method of garbage bag film |
| CN114836012B (en) * | 2022-04-14 | 2024-05-28 | 荣成汇发再生资源有限公司 | Completely biodegradable garbage bag film material and preparation method of garbage bag film |
| CN115197547A (en) * | 2022-06-24 | 2022-10-18 | 杭实科技发展(杭州)有限公司 | Special agricultural mulching film for reducing pesticide and controlling grass biodegradation of rice |
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