CN110437590B - Composite nano material modified starch-based biodegradable food packaging film and preparation method thereof - Google Patents
Composite nano material modified starch-based biodegradable food packaging film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite nano material modified starch-based biodegradable food packaging film, which adopts a composite nano material, starch is subjected to superfine refinement through physical and mechanical effects, a composite bio-based material is adopted, and simultaneously, the types and the formula of raw materials are greatly optimized, so that the interface compatibility of the starch and the bio-based material is improved, and the tensile strength and the elongation at break of the film are improved; the starch-based biodegradable food packaging film is prepared by adopting a double-screw extrusion and film blowing process, can be produced in common plastic film production equipment, and is easy for industrial production and popularization. Compared with the existing bio-based packaging film, the starch-based biodegradable food packaging film prepared by the invention has obviously improved tensile strength, elongation at break and the like.
Description
Technical Field
The invention belongs to the technical field of food packaging materials, and particularly relates to a composite nano material modified starch-based biodegradable food packaging film and a preparation method thereof.
Background
Currently, a large amount of plastic is used for food packaging. Polyethylene (PE), polyvinyl chloride (PVC) and polyvinylidene chloride (PVDC) are the most widely used food packaging materials, and the film materials have the function of preventing oxygen from permeating and can achieve the effect of food fresh-keeping packaging. However, plastic films have serious social problems of poor safety, poor environmental performance, and strong dependence on non-renewable petroleum resources, and are increasingly limited in the field of food packaging. On one hand, polyvinyl chloride has poor thermal stability and light resistance, hydrogen chloride gas harmful to human bodies begins to be decomposed at the temperature of more than 100 ℃ and after long-time sun exposure, and meanwhile, plasticizers, namely adipic acid Diester (DEHA) and the like used in polyvinyl chloride films belong to environmental hormone substances which interfere endocrine, and can induce canceration; on the other hand, plastic films are wasted in natural environments and are difficult to degrade automatically, particularly PE films can be degraded for hundreds of years, and serious white pollution is caused to ecological environments; meanwhile, the plastic film raw material is petroleum which belongs to non-renewable resources, and the energy crisis is aggravated by using a large amount of plastic films. Therefore, the search for substitutes of plastic films and the research of bio-based food packaging films taking natural materials or biosynthetic materials as raw materials gradually realize the requirements of no pollution and no trace of food packaging waste in China.
The method comprises the steps of adding polylactic acid, corn starch, hemp fiber, a silane coupling agent kh-550, glycerol, epichlorohydrin, polyethylene glycol, montmorillonite, graphene oxide, vinyl triethoxysilane and other raw materials into polylactic acid for hydrophobic modification, dispersing uniformly, improving the hydrophobicity greatly to improve the barrier property of a coating, improving the thermal stability of the film, CN201810993983.1 discloses a controllable starch-based biodegradable agricultural mulching film which is prepared by adding PBAT + P L A or PBAT + P L A + MTPS or PBAT + P L A + MTPS + bagasse cellulose, a chain extender, a release agent into a film forming biological degradable mulching film which is prepared by mixing PBAT + P L A or PBAT + P675A + MTPS or PBAT + P L A + bagasse cellulose, stirring at 355, adding a starch stabilizer into a starch film prepared by stirring, stirring at 355 ℃ and stirring, adding a starch, stirring at 355-0.5C, adding a starch, stirring, adding a collagen, a starch, a collagen, a starch, a collagen, a starch, a cellulose, a starch, a collagen, a starch, a cellulose, a starch, a cellulose.
At present, most of biological materials used by biodegradable food preservative films prepared at home and abroad are hydrophilic substances, and have poor water-proof and oil-proof properties, are easy to crack and difficult to store; the cost for manufacturing the edible packaging film is high, and the edible packaging film cannot compete with the common plastic food packaging film in the market; no thermoplasticity, only can be formed by a film coating, film spraying or tape casting process (namely a wet method), and the thickness and the uniformity of a product are difficult to control; the process is incomplete, and the equipment is not matched. Therefore, the physical and chemical green modification technology is adopted to modify the starch, so that the waterproof, oil-proof and mechanical properties of the starch are improved; the method selects a novel biological material to be physically blended with starch to realize performance complementation, develops a novel nano material (such as graphene, graphene oxide, nano zinc oxide, nano titanium oxide and the like) to improve the interface compatibility of a high molecular polymer and a starch blending material, adopts film blowing process forming to reduce the production cost and improve the performance of a film, and is the direction and development trend of domestic and foreign research.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a composite nano material (graphene, nano TiO)2Nano Zno and nano SiO2) Compared with the prior art, the starch-based biodegradable food packaging film composed of the micronized starch (600-1200 meshes) and the composite bio-based material (P L A, PBAT and PC L) has better mechanical strength.
The above purpose is realized by the following technical scheme:
a composite nano material modified starch-based biodegradable food packaging film is prepared from the following raw materials in parts by weight:
100 parts of composite bio-based material;
20-50 parts of starch;
2-10 parts of composite nano material;
1-3 parts of a processing aid;
0.2-2 parts of aluminate;
0.2 to 0.8 portion of lauryl amine,
the composite bio-based material consists of P L A, PBAT and PC L;
the composite nano material is prepared from graphene and nano TiO2Nano ZnO and nano SiO2Composition is carried out;
the processing aid consists of polyethylene wax, stearic acid and paraffin;
preferably, the weight ratio of the P L A, the PBAT and the PC L is 1: 4: 1.
Preferably, the particle size of the composite nano material is 5-80nm, and graphene and nano TiO in the composite nano material2Nano ZnO and nano SiO2The weight ratio of the four is 0.1: 2: 1: 1.
preferably, the weight ratio of the polyethylene wax to the stearic acid to the paraffin wax is 1: 2: 1.
a method for preparing the composite nanomaterial modified starch-based biodegradable food packaging film comprises the following steps:
1) carrying out ultrafine refining on starch to 600-1200 meshes by using an airflow crusher, then placing the starch into a high-speed stirrer, adding aluminate, and stirring the mixture for 10-30 minutes at 80-100 ℃ to obtain modified micronized starch;
2) stirring the composite nano material and dodecylamine for 10-30 minutes under the ultrasonic condition to fully disperse the nano composite material to obtain a modified composite nano material;
3) mixing the modified micronized starch obtained in the step 1), the modified composite nano material obtained in the step 2), the composite bio-based material and the processing aid in a high-speed mixer at 70-90 ℃ for 10-30 minutes to obtain a mixed material;
4) and (3) extruding the mixed material in the step 3) in a double-screw extruder, shaping by a die, cooling, drawing and cutting, and finally blowing the film on a film blowing machine to obtain the film.
Preferably, the heating temperature T1-T10 of each section of the double-screw extruder is 80 ℃, 100 ℃, 110 ℃, 130 ℃, 150 ℃, 170 ℃, 160 ℃, 150 ℃ and 110 ℃, the rotating speed of a main machine is 15-30 r/min, and the material pressure is 2.1-3.5 MPA; the film blowing conditions are as follows: the heating temperature T1-T4 and the die head of each section are respectively 120 ℃, 170 ℃, 160 ℃ and 150 ℃, the traction speed is 4.3 r/min, and the winding speed is 8.15 r/min.
The invention has the beneficial effects that:
the invention adopts composite nano material (graphene: nano TiO)2: nano ZnO and nano SiO2) Starch is subjected to superfine refining through physical and mechanical effects, a composite biological base material is adopted, the types and the formula of the raw materials are greatly optimized, the interface compatibility of the starch and the biological base material is improved, and a double-screw extrusion and film blowing process is adopted to prepare the starch-based biodegradable food packaging film, so that the tensile strength and the elongation at break of the film are improved.
Compared with the existing bio-based packaging film, the starch-based biodegradable food packaging film prepared by the invention has the advantages that the tensile strength, the elongation at break and the like are obviously improved, the improvement rate of the tensile strength is more than 50-150%, and the improvement rate of the elongation at break is more than 200-500%. The invention also has the characteristics of simple process, low cost and the like.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
A composite nano material modified starch-based biodegradable food packaging film is prepared from the following raw materials:
the preparation method comprises the following steps:
1) carrying out superfine refining on starch to 600 meshes by using an airflow crusher, then putting the starch into a high-speed stirrer, adding aluminate, and stirring the mixture for 10 minutes at 100 ℃ to obtain modified micronized starch;
2) stirring the composite nano material with the particle size of 5-80nm and dodecylamine for 10 minutes under the ultrasonic condition to fully disperse the nano composite material to obtain a modified composite nano material;
3) mixing the modified micronized starch obtained in the step 1), the modified composite nano material obtained in the step 2), the bio-based composite material and the processing aid in a high-speed mixer at 70 ℃ for 30 minutes to obtain a mixed material;
4) and (3) extruding the mixed material in the step 3) in a double-screw extruder, shaping by a die, cooling, drawing and cutting, and finally blowing the film on a film blowing machine to obtain the film.
The heating temperature T1-T10 of each section of the double-screw extruder is 80 ℃, 100 ℃, 110 ℃, 130 ℃, 150 ℃, 170 ℃, 160 ℃, 150 ℃ and 110 ℃, the rotating speed of a main machine is 15-30 r/min, and the material pressure is 2.1-3.5 MPA. The film blowing conditions are as follows: the heating temperature T1-T4 and the die head of each section are respectively 120 ℃, 170 ℃, 160 ℃ and 150 ℃, the traction speed is 4.3 r/min, and the winding speed is 8.15 r/min.
Example 2
A composite nano material modified starch-based biodegradable food packaging film is prepared from the following raw materials:
the preparation method comprises the following steps:
1) micronizing starch to 1200 meshes by using an airflow pulverizer, then placing the starch into a high-speed stirrer, adding aluminate ester at the same time, and stirring the mixture for 30 minutes at 80 ℃ to obtain modified micronized starch;
2) stirring the composite nano material with the particle size of 5-80nm and dodecylamine for 15 minutes under the ultrasonic condition to fully disperse the nano composite material to obtain a modified composite nano material;
3) mixing the modified micronized starch obtained in the step 1), the modified composite nano material obtained in the step 2), the composite bio-based material and the processing aid in a high-speed mixer at 90 ℃ for 10 minutes to obtain a mixed material;
4) and (3) extruding the mixed material in the step 3) in a double-screw extruder, shaping by a die, cooling, drawing and cutting, and finally blowing the film on a film blowing machine to obtain the film.
Example 3
A composite nano material modified starch-based biodegradable food packaging film is prepared from the following raw materials:
the preparation method comprises the following steps:
1) carrying out superfine refining on starch to 1000 meshes by using an airflow crusher, then putting the starch into a high-speed stirrer, adding aluminate, and stirring the mixture for 15 minutes at 90 ℃ to obtain modified micronized starch;
2) stirring the composite nano material with the particle size of 5-80nm and dodecylamine for 30 minutes under the ultrasonic condition to fully disperse the nano composite material to obtain a modified composite nano material;
3) mixing the modified micronized starch obtained in the step 1), the modified composite nano material obtained in the step 2), the bio-based composite material and the processing aid in a high-speed mixer at 80 ℃ for 15 minutes to obtain a mixed material;
4) and (3) extruding the mixed material in the step 3) in a double-screw extruder, shaping by a die, cooling, drawing and cutting, and finally blowing the film on a film blowing machine to obtain the film.
Comparative example 1
A composite nano material modified starch-based biodegradable food packaging film is prepared from the following raw materials:
the preparation method is the same as in example 3.
Comparative example 2
A composite nano material modified starch-based biodegradable food packaging film is prepared from the following raw materials:
the preparation method is the same as in example 3.
Comparative example 3
The starch was not subjected to the micronizing treatment, and the other steps were the same as in example 3.
Comparative example 4
The preparation method is the same as in example 3.
1. Measurement of mechanical Strength
The detection method comprises the following steps: reference is made to GB/T1040.1-2006.
And (3) detection results: see table 1.
TABLE 1 measurement results of mechanical strength of biodegradable film
| Tensile strength/MPa | Elongation at break/% | |
| Example 1 | 35.9 | 478 |
| Example 2 | 36.6 | 481 |
| Example 3 | 49.5 | 551 |
| Comparative example 1 | 21.5 | 189 |
| Comparative example 2 | 23.8 | 156 |
| Comparative example 3 | 18.3 | 167 |
| Comparative example 4 | 21.8 | 188 |
2. Detection of degradation effects
The detection method comprises the following steps: reference is made to GB/T19277.
And (3) detection results: see table 2.
TABLE 2 degradation rate measurement results of biodegradable film
| Degradation Rate (%) | |
| Example 1 | 92 |
| Example 2 | 97 |
| Example 3 | 99 |
| Comparative example 1 | 71 |
| Comparative example 2 | 75 |
| Comparative example 3 | 72 |
| Comparative example 4 | 75 |
3. Food fresh-keeping effect measurement
The detection method comprises the following steps: the preservation effect is determined by the total number of colonies, and the specific method refers to GB 47892-2010.
And (3) detection results: see table 3.
TABLE 3 fresh-keeping effect of biodegradable film on beef jerky (25 ℃ C.)
| Longest fresh-keeping time (moon) | |
| Example 1 | 24 |
| Examples2 | 25 |
| Example 3 | 30 |
| Comparative example 1 | 11 |
| Comparative example 2 | 9 |
| Comparative example 3 | 8 |
| Comparative example 4 | 10 |
The experimental results show that the invention adopts the composite nano material, carries out ultramicro refinement and modification treatment on the starch, adopts the composite bio-based material, simultaneously carries out massive optimization on the types and the formulas of the raw materials, and improves the interface compatibility of the bio-based composite material, thereby improving the mechanical strength of the biological film, having full degradation performance and having excellent fresh-keeping effect on food.
Claims (2)
1. The composite nano material modified starch-based biodegradable food packaging film is characterized by being prepared from the following raw materials in parts by weight:
100 parts of composite bio-based material;
20-50 parts of starch;
2-10 parts of composite nano material;
1-3 parts of a processing aid;
0.2-2 parts of aluminate;
0.2 to 0.8 portion of lauryl amine,
the composite bio-based material consists of P L A, PBAT and PC L, wherein the weight ratio of the P L A to the PBAT to the PC L is 1: 4: 1;
the composite nano material is prepared from graphene and nano TiO2Nano ZnO and nano SiO2The particle size of the composite nano material is 5-80nm, and graphene and nano TiO in the composite nano material2Nano ZnO and nano SiO2The weight ratio of the four is 0.1: 2: 1: 1;
the processing aid consists of polyethylene wax, stearic acid and paraffin, wherein the weight ratio of the polyethylene wax to the stearic acid to the paraffin is 1: 2: 1,
the preparation method comprises the following steps:
1) carrying out ultrafine refining on starch to 600-1200 meshes by using an airflow crusher, then placing the starch into a high-speed stirrer, adding aluminate, and stirring the mixture for 10-30 minutes at 80-100 ℃ to obtain modified micronized starch;
2) stirring the composite nano material and dodecylamine for 10-30 minutes under the ultrasonic condition to fully disperse the nano composite material to obtain a modified composite nano material;
3) mixing the modified micronized starch obtained in the step 1), the modified composite nano material obtained in the step 2), the composite bio-based material and the processing aid in a high-speed mixer at 70-90 ℃ for 10-30 minutes to obtain a mixed material;
4) and (3) extruding the mixed material in the step 3) in a double-screw extruder, shaping by a die, cooling, drawing and cutting, and finally blowing the film on a film blowing machine to obtain the film.
2. The composite nanomaterial-modified starch-based biodegradable food packaging film of claim 1, wherein: the heating temperature T1-T10 of each section of the double-screw extruder is 80 ℃, 100 ℃, 110 ℃, 130 ℃, 150 ℃, 170 ℃, 160 ℃, 150 ℃ and 110 ℃, the rotating speed of a main machine is 15-30 r/min, and the material pressure is 2.1-3.5 MPA; the film blowing conditions are as follows: the heating temperature T1-T4 and the die head of each section are respectively 120 ℃, 170 ℃, 160 ℃ and 150 ℃, the traction speed is 4.3 r/min, and the winding speed is 8.15 r/min.
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| CN112550930A (en) * | 2021-01-04 | 2021-03-26 | 安徽沪通环保包装科技有限公司 | Convenient square-bottom bag and manufacturing method thereof |
| CN113005641A (en) * | 2021-02-08 | 2021-06-22 | 武汉轻工大学 | Preparation method of antioxidant starch composite nanofiber food packaging film |
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