CN106317723B - Preparation method of degradable nano double-layer packaging film with antibacterial function - Google Patents

Preparation method of degradable nano double-layer packaging film with antibacterial function Download PDF

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CN106317723B
CN106317723B CN201610755780.XA CN201610755780A CN106317723B CN 106317723 B CN106317723 B CN 106317723B CN 201610755780 A CN201610755780 A CN 201610755780A CN 106317723 B CN106317723 B CN 106317723B
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CN106317723A (en
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王清
朱广宏
钟宇
邓云
岳进
庄晨俊
江永利
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Gaoyou Red Sun Food Co ltd
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Abstract

The invention relates to a preparation method of a degradable nano double-layer packaging film with an antibacterial function, which can be used for keeping freshness of foods such as duck eggs and the like, and belongs to the field of food packaging. The method comprises respectively preparing sodium alginate nano-cellulose antibacterial film solution and polyvinyl alcohol-chitosan nano TiO2Antibacterial film liquid; pouring the first layer of nano sodium alginate antibacterial membrane liquid into a mold, drying, pouring a calcium chloride solution for curing, then pouring the second layer of polyvinyl alcohol-chitosan nano antibacterial membrane liquid, drying and uncovering the membrane to obtain the nano sodium alginate antibacterial membrane. The method is simple and easy to operate, and the obtained double-layer film has excellent barrier property and antibacterial capacity, can effectively prolong the shelf life of eggs, and improves the economic benefit of enterprises.

Description

Preparation method of degradable nano double-layer packaging film with antibacterial function
Technical Field
The invention belongs to the field of degradable food packaging, and particularly relates to a preparation method of a degradable nano double-layer packaging film with an antibacterial function.
Background
The 'white pollution' brought by plastic packaging seriously threatens the natural environment and increasingly becomes a world public nuisance. In addition, limited petroleum resources have also restricted the development of the plastics industry. Therefore, the preparation of biodegradable materials from natural polymer materials has attracted much attention from researchers in all countries around the world. Among a plurality of natural substances, chitosan and sodium alginate are marine polysaccharides, so that the marine polysaccharide packaging material is rich in resources, low in price, excellent in film forming property and most widely applied as a packaging raw material. Polyvinyl alcohol is a water-soluble polymer resin, and is widely applied to degradable packaging due to the characteristics of good degradability, biocompatibility, physical stability and the like.
With the continuous development of nano materials in recent years, a new leading-edge technology is provided for the packaging industry, and the method becomes a research hotspot in the field of food packaging. Among them, nanocellulose as a natural degradable reinforcing agent has incomparable advantages of inorganic fillers, such as various types, reproducibility, low price, excellent processing performance, easy recycling and the like. And nano-sized TiO2The antibacterial food packaging material has the advantages of aging resistance, high temperature resistance, excellent comprehensive performance, stable antibacterial property and the like, is commonly used for antibacterial food packaging, enlarges the application range and improves the application grade.
At present, the development of degradable packaging mainly focuses on the development of a composite single-layer packaging material with an optimized film forming formula. Studies have shown that the gas or water vapor barrier properties of double-layer packages are apparently due to single-layer packages when the same amount of material is used for both single-layer and double-layer packages.
Disclosure of Invention
The invention aims to provide a preparation method of a degradable nano double-layer packaging film with an antibacterial function. The technical scheme adopted by the invention for realizing the purpose is as follows: a preparation method of a degradable nanometer double-layer packaging film with an antibacterial function is characterized by comprising the following steps: the method comprises the following steps:
the first step is as follows: preparing a sodium alginate nano cellulose antibacterial membrane solution;
the second step is that: pouring the sodium alginate nano-cellulose antibacterial membrane liquid prepared in the first step into a leveling mold, drying, and pouring a calcium chloride solution with a certain concentration for curing;
the third step: preparation of polyvinyl alcohol-Chitosan Nano TiO2Antibacterial film liquid;
the fourth step: pouring the polyvinyl alcohol-chitosan nano TiO prepared in the third step2Drying the antibacterial film liquid, and then uncovering the film to obtain the degradable nano double-layer packaging film with the antibacterial function.
The preparation method of the sodium alginate nano-cellulose antibacterial membrane liquid in the first step comprises the following steps:
dissolving sodium alginate in water to prepare a solution, sequentially adding nano-cellulose, glycerol, tween 80 and sodium ethylparaben into the sodium alginate solution, stirring for a period of time, homogenizing, adjusting the pH value, and performing vacuum degassing to obtain the sodium alginate nano-cellulose antibacterial membrane solution.
The mass concentration of the sodium alginate solution is 5-25 g/L, and 0.025-0.5% of nano-cellulose, 0.1-0.75% of glycerol, 0.01-0.5% of Tween 80 and 0.01-0.5% of ethylparaben sodium are added.
The stirring time is 1-5 h, the pH is adjusted to 4-8, and vacuum degassing is performed for 0.5-2 h.
In the second step, the sodium alginate nano-cellulose antibacterial film liquid is poured into a leveling die and then dried for 8-24 hours at the temperature of 30-50 ℃; the mass fraction of the calcium chloride solution is 0.25-1%.
In the third step, polyvinyl alcohol-chitosan nano TiO2The preparation method of the antibacterial film liquid comprises the following steps:
step 1: dissolving polyvinyl alcohol in water to prepare solution, and sequentially adding glycerol, Tween 80 and nano TiO into the polyvinyl alcohol solution2Stirring for a period of time in a water bath, and homogenizing to obtain a solution a;
step 2: dissolving chitosan in acetic acid to obtain a solution, and sequentially adding glycerol, tween 80 and nano TiO into the chitosan solution2Stirring for a period of time at room temperature, and homogenizing to obtain a solution b;
and 3, step 3: uniformly mixing the solution a and the solution b according to the proportion, and vacuum degassing to obtain the polyvinyl alcohol-chitosan nano TiO2And (3) antibacterial film liquid.
In the step 1, the mass concentration of the polyvinyl alcohol solution is 30-70 g/L, 0.4-2.1% of glycerol, 0.01-0.5% of Tween 80 and 0.1-0.5% of nano TiO are added2(ii) a The temperature of the water bath is 80-95 ℃, and the stirring is carried out for 1-5 h.
In the step 2, the chitosan is dissolved in acetic acid with the volume fraction of 0.5-2% to prepare a solution with the mass concentration of 10-40 g/L, and 0.2-1.2% of glycerol, 0.2-1% of Tween 80 and 0.05-0.5% of nano TiO are added2And stirring for 2-4 h.
And in the step 3, the solution a and the solution b are uniformly mixed according to the volume ratio of (1-4) to 1, and vacuum degassing is carried out for 0.5-2 h.
And in the fourth step, drying for 8-24 hours at the temperature of 30-50 ℃, and then uncovering the film.
The invention adopts an autonomous loading technology, and prepares the sodium alginate nano-cellulose/polyvinyl alcohol-chitosan nano TiO by using safe and nontoxic degradable base materials and nano additives2An antibacterial bilayer film. The packaging film prepared by the method has good mechanical property, excellent barrier capability and good slow-release antibacterial capability, and can effectively prolong the shelf life of goods and improve the economic benefit of related industries when being applied to the preservation of foods such as eggs.
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Fig. 1 is a schematic view of a preparation process of the degradable nano double-layer packaging film with an antibacterial function of the invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment relates to a preparation method of a degradable nano double-layer packaging film with an antibacterial function, which has a flow schematic diagram shown in fig. 1 and specifically comprises the following steps:
the first step is as follows: dissolving sodium alginate in water to obtain a solution with a mass concentration of 5g/L, adding 0.025% of nano-cellulose, 0.1% of glycerol, 0.01% of tween 80 and 0.01% of sodium ethylparaben by mass, stirring for 1h, homogenizing, adjusting pH to 4, and vacuum degassing for 0.5 h;
the second step is that: pouring the sodium alginate nano cellulose antibacterial membrane liquid prepared in the first step into a leveling mold, drying for 24 hours at the temperature of 30 ℃, and then pouring a calcium chloride solution with the mass fraction of 0.25% for curing;
the third step: dissolving polyvinyl alcohol in water to obtain a solution with a mass concentration of 30g/L, and adding 0.4% of glycerol, 0.01% of Tween 80 and 0.1% of nano TiO in mass fraction2Stirring in 80 deg.C water bath for 5 hr, and homogenizing; dissolving chitosan in 0.5% acetic acid to obtain 10g/L solution, adding 0.2% glycerol, 0.2% Tween 80 and 0.05% nanometer TiO2Stirring for 2h, and homogenizing; uniformly mixing polyvinyl alcohol and chitosan solution according to a ratio of 4:1, and vacuum degassing for 0.5h to obtain polyvinyl alcohol-chitosan nano membrane solution;
the fourth step: and pouring the polyvinyl alcohol-chitosan nano film liquid into a mould, drying for 24h at the temperature of 30 ℃, and then uncovering the film to obtain the degradable nano double-layer packaging film with the antibacterial function.
Example 2
The embodiment relates to a preparation method of a degradable nano double-layer packaging film with an antibacterial function, which has a flow schematic diagram shown in fig. 1 and specifically comprises the following steps:
the first step is as follows: dissolving sodium alginate in water to obtain solution with mass concentration of 12.5g/L, adding 0.25% of nanocellulose, 0.25% of glycerol, 0.175% of tween 80 and 0.125% of ethylparaben, stirring for 3 hr, homogenizing, adjusting pH to 4.5, and vacuum degassing for 1 hr;
the second step is that: pouring the sodium alginate nano cellulose antibacterial membrane liquid into a leveling mold, drying for 16h at 40 ℃, and then pouring a calcium chloride solution with the mass fraction of 0.75% for curing;
the third step: dissolving polyvinyl alcohol in water to prepare a solution with the mass concentration of 50g/L, and adding 1% of glycerol, 0.1% of Tween 80 and 0.1% of nano TiO by mass fraction2Stirring in water bath at 85 deg.C for 3 hr, and homogenizing; dissolving chitosan in 1% by volume of ethanolPreparing solution with mass concentration of 20g/L in acid, adding glycerol with mass fraction of 0.4%, Tween 80 with mass fraction of 0.1% and nanometer TiO with mass fraction of 0.1%2Stirring for 3h, and homogenizing; uniformly mixing polyvinyl alcohol and chitosan solution according to the ratio of 2:1, and vacuum degassing for 1h to obtain polyvinyl alcohol-chitosan nano membrane solution;
the fourth step: pouring the polyvinyl alcohol-chitosan nano film liquid into a mould, drying for 16h at 40 ℃, and then uncovering the film to obtain the degradable nano double-layer packaging film with the antibacterial function.
Example 3
The embodiment relates to a preparation method of a degradable nano double-layer packaging film with an antibacterial function, which has a flow schematic diagram shown in fig. 1 and specifically comprises the following steps:
the first step is as follows: dissolving sodium alginate in water to obtain a solution with a mass concentration of 25g/L, adding 0.5% of nano-cellulose, 0.75% of glycerol, 0.5% of tween 80 and 0.5% of ethylparaben by mass, stirring for 5h, homogenizing, adjusting pH to 8, and vacuum degassing for 2 h;
the second step is that: pouring the sodium alginate nano cellulose antibacterial membrane liquid into a leveling mold, drying for 8 hours at 50 ℃, and then pouring a calcium chloride solution with the mass fraction of 1% for curing;
the third step: dissolving polyvinyl alcohol in water to prepare a solution with the mass concentration of 70g/L, and adding 2.1% of glycerol, 0.5% of Tween 80 and 0.5% of nano TiO by mass fraction2Stirring for 1h in a water bath at 95 ℃, and homogenizing; dissolving chitosan in 2% acetic acid to obtain 40g/L solution, adding 1.2% glycerol, 1% Tween 80 and 0.5% nanometer TiO2Stirring for 4h, and homogenizing; uniformly mixing polyvinyl alcohol and chitosan solution according to a ratio of 1:1, and vacuum degassing for 2 hours to obtain polyvinyl alcohol-chitosan nano membrane solution;
the fourth step: pouring the polyvinyl alcohol-chitosan nano film liquid into a mould, drying for 8h at 50 ℃, and then uncovering the film to obtain the degradable nano double-layer packaging film with the antibacterial function.
The basic properties of the two-layer films described in the above examples were measured, and the results are shown in table 1.
Wherein, the film thickness measurement: the 5 spots were randomly measured on the membrane using a digital micrometer screw.
Tensile strength and elongation at break measurements: according to GB1040-79, the films were cut into 1.5X 10cm strips and measured using a texture analyzer.
And (3) measuring the water vapor transmission rate: the relative humidity difference between the inside and the outside of the film is 0/100% by adopting a cup-like method.
And (3) determination of antibacterial activity: escherichia coli and Listeria were inoculated into LB liquid medium and TSB liquid medium, respectively, and activated at 37 ℃ for 12 hours at 200 rpm. Four patches 1X 1cm in size were added to 50mL of bacterial suspension in 4 pieces each, and the original bacterial suspension without patches was used as a control. All bacterial suspensions were incubated at 37 ℃ and 200rpm for 4 hours and examined for bacteriostatic activity.
And (3) water solubility determination: after immersing the weighed film sample in distilled water for 24h, the remaining film was dried to constant weight, with water solubility as a percentage of mass loss.
TABLE 1 comparison of basic Properties of two-layer films
Figure BDA0001099375060000041
Figure BDA0001099375060000051
As can be seen from table 1, the mechanical strength of the bilayer film increases significantly with increasing substrate concentration, while the water solubility decreases significantly. The higher the added amount of sodium alginate, the more negative charge groups are subjected to electrostatic interaction with chitosan to form-NH 3 +. RCOO-groups, and the crosslinking-like effect enables the double-layer membrane to be tightly combined, so that the mechanical property is improved. However, the hydrophilicity of sodium alginate is very strong, and the comprehensive effect brought by the simultaneous increase of the electrostatic acting force and the hydrophilicity is that the water resistance of the double-layer film is reduced. With the increase of the concentration content of chitosan and ethylparaben sodium, the antibacterial property of the double-layer membrane is enhanced, and the inhibiting effect of the membrane on listeria is more obvious.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.

Claims (3)

1. A preparation method of a degradable nanometer double-layer packaging film with an antibacterial function is characterized by comprising the following steps: the method comprises the following steps:
the first step is as follows: the preparation method of the sodium alginate nano-cellulose antibacterial membrane solution comprises the following steps:
dissolving sodium alginate in water to prepare a solution, sequentially adding nano-cellulose, glycerol, tween 80 and sodium ethylparaben into the sodium alginate solution, stirring for a period of time, homogenizing, adjusting the pH, and performing vacuum degassing to obtain a sodium alginate nano-cellulose antibacterial membrane solution; the mass concentration of the sodium alginate solution is 5-25 g/L, and 0.025-0.5% of nano-cellulose, 0.1-0.75% of glycerol, 0.01-0.5% of Tween 80 and 0.01-0.5% of ethylparaben sodium are added; the stirring time is 1-5 h, the pH is adjusted to 4-8, and vacuum degassing is carried out for 0.5-2 h;
the second step is that: pouring the sodium alginate nano-cellulose antibacterial membrane liquid prepared in the first step into a leveling mold, drying, and pouring a calcium chloride solution with a certain concentration for curing;
the third step: preparation of polyvinyl alcohol-Chitosan Nano TiO2The preparation method of the antibacterial membrane liquid comprises the following steps:
step 1: dissolving polyvinyl alcohol in water to prepare solution, and sequentially adding glycerol, Tween 80 and nano TiO into the polyvinyl alcohol solution2Stirring for a period of time in a water bath, and homogenizing to obtain a solution a;
step 2: dissolving chitosan in acetic acid to obtain a solution, and sequentially adding glycerol, tween 80 and nano TiO into the chitosan solution2Stirring for a period of time at room temperature, and homogenizing to obtain a solution b;
and 3, step 3: uniformly mixing the solution a and the solution b according to the proportion, and vacuum degassing to obtain the polyvinyl alcohol-chitosan nano TiO2Antibacterial film liquid;
in the step 1, the mass concentration of the polyvinyl alcohol solution is 30-70 g/L, 0.4-2.1% of glycerol, 0.01-0.5% of Tween 80 and 0.1-0.5% of nano TiO are added2(ii) a The temperature of the water bath is 80-95 ℃, and stirring is carried out for 1-5 h;
in the step 2, the chitosan is dissolved in acetic acid with the volume fraction of 0.5-2% to prepare a solution with the mass concentration of 10-40 g/L, and 0.2-1.2% of glycerol, 0.2-1% of Tween 80 and 0.05-0.5% of nano TiO are added2Stirring for 2-4 h;
in the step 3, the solution a and the solution b are uniformly mixed according to the volume ratio of (1-4) to 1, and vacuum degassing is carried out for 0.5-2 h;
the fourth step: pouring the polyvinyl alcohol-chitosan nano TiO prepared in the third step into a mould2Drying the antibacterial film liquid, and then uncovering the film to obtain the degradable nano double-layer packaging film with the antibacterial function.
2. The preparation method of the degradable nanometer double-layer packaging film with the antibacterial function according to claim 1, characterized in that: in the second step, the sodium alginate nano-cellulose antibacterial film liquid is poured into a leveling die and then dried for 8-24 hours at the temperature of 30-50 ℃; the mass fraction of the calcium chloride solution is 0.25-1%.
3. The preparation method of the degradable nanometer double-layer packaging film with the antibacterial function according to claim 1, characterized in that: and in the fourth step, drying for 8-24 hours at the temperature of 30-50 ℃, and then uncovering the film.
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CN109134942B (en) * 2018-07-16 2021-07-09 浙江大学宁波理工学院 Transparent nano-cellulose antibacterial paper and preparation method thereof
CN109021276B (en) * 2018-09-03 2021-04-16 上海大觉包装制品有限公司 Biodegradable composite film for edible mushroom fresh-keeping packaging and preparation method thereof
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