CN113005771A - Preparation method of hydrophobic starch food packaging film - Google Patents
Preparation method of hydrophobic starch food packaging film Download PDFInfo
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- CN113005771A CN113005771A CN202110188339.9A CN202110188339A CN113005771A CN 113005771 A CN113005771 A CN 113005771A CN 202110188339 A CN202110188339 A CN 202110188339A CN 113005771 A CN113005771 A CN 113005771A
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- 229920002472 Starch Polymers 0.000 title claims abstract description 191
- 239000008107 starch Substances 0.000 title claims abstract description 191
- 235000019698 starch Nutrition 0.000 title claims abstract description 191
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 70
- 235000013305 food Nutrition 0.000 title claims abstract description 68
- 239000012785 packaging film Substances 0.000 title claims abstract description 45
- 229920006280 packaging film Polymers 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000012528 membrane Substances 0.000 claims abstract description 95
- 239000002121 nanofiber Substances 0.000 claims abstract description 80
- 238000009987 spinning Methods 0.000 claims abstract description 72
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 35
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 35
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000008117 stearic acid Substances 0.000 claims abstract description 35
- 238000004806 packaging method and process Methods 0.000 claims abstract description 25
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
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- 238000012986 modification Methods 0.000 claims abstract description 10
- 239000011664 nicotinic acid Substances 0.000 claims abstract description 10
- PGXWDLGWMQIXDT-UHFFFAOYSA-N methylsulfinylmethane;hydrate Chemical compound O.CS(C)=O PGXWDLGWMQIXDT-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 80
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 42
- 239000007864 aqueous solution Substances 0.000 claims description 17
- KYIDJMYDIPHNJS-UHFFFAOYSA-N ethanol;octadecanoic acid Chemical compound CCO.CCCCCCCCCCCCCCCCCC(O)=O KYIDJMYDIPHNJS-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 24
- 239000000835 fiber Substances 0.000 abstract description 11
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- 239000001913 cellulose Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
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- 102000004169 proteins and genes Human genes 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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Abstract
The invention discloses a preparation method of a hydrophobic starch food packaging film, which comprises the following steps: dissolving starch in dimethyl sulfoxide water solution to form spinning solution; performing electrostatic spinning on the spinning solution to prepare a starch nanofiber membrane; and (3) carrying out stearic acid modification on the starch nanofiber membrane to form a bionic hydrophobic coating on the surface of the membrane, and reacting to obtain the hydrophobic starch food packaging membrane. According to the invention, the starch nanofiber membrane is prepared by using the electrostatic spinning method, so that the operation is simple, the reaction is mild, the prepared nanofiber membrane has a smoother and more uniform fiber network compared with a common starch membrane, the membrane performance is improved, more reaction sites are provided for subsequent stearic acid modification, and the hydrophobic property is improved; through stearic acid treatment of the starch nanofiber membrane, a barrier is formed on the surface of the starch nanofiber membrane, water infiltration is avoided, and the water resistance of the food packaging membrane is improved.
Description
Technical Field
The invention relates to the technical field of food packaging, in particular to a preparation method of a hydrophobic starch food packaging film.
Background
The food packaging film is mainly petroleum-based plastic packaging films, such as Polyethylene (PE) and polyvinylidene chloride (PVDC). Although plastic has good mechanical properties and sealing performance as one of the most widely used materials for food packaging, the plastic is difficult to biodegrade and easily causes white pollution. With the increasing awareness of environmental protection, the development of green and natural food packaging films becomes a research hotspot.
In recent years, some degradable natural renewable resources, such as starch, chitosan, cellulose, protein, etc., have attracted extensive research interest. The starch has the advantages of wide source, large reserve, low price and the like, is expected to be applied to the field of green food packaging, and replaces the traditional petroleum-based plastic to solve the problem of environmental pollution. However, starch films have the disadvantage of poor water-blocking properties.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a hydrophobic starch food packaging film, and aims to prepare a starch food packaging film with good water resistance.
In order to achieve the purpose, the invention provides a preparation method of a hydrophobic starch food packaging film, which comprises the following steps:
dissolving starch in dimethyl sulfoxide water solution to form spinning solution;
performing electrostatic spinning on the spinning solution to prepare a starch nanofiber membrane;
and (3) carrying out stearic acid modification on the starch nanofiber membrane to form a bionic hydrophobic coating on the surface of the membrane, and reacting to obtain the hydrophobic starch food packaging membrane.
Alternatively, the step of dissolving the starch in an aqueous solution of dimethyl sulfoxide to form a spinning solution is carried out at 65 ℃ to 75 ℃.
Optionally, in the step of dissolving starch in a dimethyl sulfoxide aqueous solution to form a spinning solution, the mass fraction of starch in the spinning solution is 20% to 30%.
Optionally, in the step of dissolving starch in an aqueous dimethyl sulfoxide solution to form the spinning solution, the volume percentage concentration of the aqueous dimethyl sulfoxide solution is 90% to 97%.
Optionally, the starch nanofiber membrane is modified with stearic acid to form a bionic hydrophobic coating on the surface of the membrane, and the step of reacting to obtain the hydrophobic starch food packaging membrane comprises:
soaking the starch nanofiber membrane in a stearic acid ethanol solution, and reacting at 50-70 ℃ to enable stearic acid to form a bionic hydrophobic coating on the surface of the starch nanofiber membrane in a self-assembly manner, so as to obtain a mixed solution;
and washing the mixed solution by using absolute ethyl alcohol, and drying the precipitate to obtain the hydrophobic starch food packaging film.
Optionally, the concentration of stearic acid in the stearic acid ethanol solution is 0.025mol/L to 0.15 mol/L.
According to the technical scheme provided by the invention, the starch nanofiber membrane is prepared by using an electrostatic spinning method, so that the operation is simple, the reaction is mild, the prepared nanofiber membrane has a smoother and more uniform fiber network compared with a common starch membrane, the membrane performance is improved, more reaction sites are provided for subsequent stearic acid modification, and the hydrophobic property is improved; through stearic acid treatment of the starch nanofiber membrane, a barrier is formed on the surface of the starch nanofiber membrane, water infiltration is avoided, and the water resistance of the food packaging membrane is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an SEM image of a starch nanofiber membrane prepared in comparative example 1;
FIG. 2 is an SEM image of a starch nanofiber membrane prepared in example 1;
FIG. 3 is an SEM image of a starch nanofiber membrane prepared in example 2;
FIG. 4 is an SEM image of a starch nanofiber membrane prepared in example 3;
FIG. 5 is an SEM image of a starch nanofiber membrane prepared in example 2;
FIG. 6 is an SEM image of a hydrophobic starch food packaging film prepared in comparative example 2;
FIG. 7 is an SEM photograph of the hydrophobic starch food packaging film prepared in example 2;
FIG. 8 is an SEM photograph of the hydrophobic starch food packaging film prepared in example 4;
FIG. 9 is an SEM photograph of the hydrophobic starch food packaging film prepared in example 5;
FIG. 10 is an SEM photograph of the hydrophobic starch food packaging film prepared in example 6;
FIG. 11 is an X-ray photoelectron spectroscopy analysis of starch;
FIG. 12 is a graph of X-ray photoelectron spectroscopy analysis of a starch nanofiber film prepared in example 2;
FIG. 13 is an X-ray photoelectron spectroscopy analysis chart of the hydrophobic starch food packaging film prepared in example 2;
FIG. 14 is a macroscopic view of the starch nanofiber film and the hydrophobic starch food packaging film prepared in example 2 after encountering water;
FIG. 15 is a macroscopic image of the starch nanofiber film prepared in example 2 and the hydrophobic starch food packaging films prepared in examples 2, 4-6 and comparative example 2 when contacted with water;
fig. 16 is a graph showing stearic acid concentration-water contact angle changes when the starch nanofiber film prepared in example 2 and the hydrophobic starch food packaging films prepared in examples 2, 4-6 and comparative example 2 are contacted with water.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The food packaging film is mainly petroleum-based plastic packaging films, such as Polyethylene (PE) and polyvinylidene chloride (PVDC). Although plastic has good mechanical properties and sealing performance as one of the most widely used materials for food packaging, the plastic is difficult to biodegrade and easily causes white pollution. With the increasing awareness of environmental protection, the development of green and natural food packaging films becomes a research hotspot.
In recent years, some degradable natural renewable resources, such as starch, chitosan, cellulose, protein, etc., have attracted extensive research interest. The starch has the advantages of wide source, large reserve, low price and the like, is expected to be applied to the field of green food packaging, and replaces the traditional petroleum-based plastic to solve the problem of environmental pollution. However, starch films have the disadvantage of poor water-blocking properties.
In view of the above, the invention provides a preparation method of a hydrophobic starch food packaging film. The preparation method of the hydrophobic starch food packaging film comprises the following steps:
and step S10, dissolving starch in dimethyl sulfoxide water solution to form spinning solution.
In this example, starch was added to an aqueous solution of dimethyl sulfoxide, stirred to dissolve the starch to form a solution, and then the solution was allowed to stand for deaeration to obtain a spinning solution. Specifically, in order to ensure that the starch is fully dissolved, in the embodiment, the starch is added into the aqueous solution of dimethyl sulfoxide, and the mixture is stirred at 65-75 ℃ to dissolve the starch; wherein the concentration of the aqueous solution of the dimethyl sulfoxide is 90-97%. In addition, in order to ensure that a fiber network structure can be formed smoothly during subsequent electrostatic spinning, the mass fraction of starch in the spinning solution is 20-30%.
And step S20, performing electrostatic spinning on the spinning solution to obtain the starch nanofiber membrane.
The embodiment adopts an electrostatic spinning method, the spinning solution is prepared into the starch nanofiber membrane, the starch membrane has a smooth and uniform fiber structure through the electrostatic spinning method, the film forming performance of the food packaging membrane is improved, more reaction sites are provided for subsequent stearic acid modification, and the hydrophobic property is improved. In specific implementation, the technological parameters of electrostatic spinning can be adjusted according to actual requirements, for example, in this embodiment, the technological parameters of electrostatic spinning can be set as: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h.
And step S30, performing stearic acid modification on the starch nanofiber membrane to form a bionic hydrophobic coating on the surface of the membrane, and reacting to obtain the hydrophobic starch food packaging membrane.
In the embodiment, stearic acid modification is performed on the starch nanofiber membrane prepared in the step S20, so that stearic acid is self-assembled on the surface of the starch nanofiber membrane to form a bionic hydrophobic coating, and stearic acid has a longer hydrophobic carbon chain, so that stearic acid existing on the surface of the starch nanofiber membrane plays a role in 'barrier', water drop penetration is avoided, the hydrophobic starch food packaging membrane has a higher contact angle, and excellent waterproof performance is shown.
In a specific implementation, step S30 may be implemented as follows:
step S31, soaking the starch nanofiber membrane in a stearic acid ethanol solution, and reacting at 50-70 ℃ to enable stearic acid to form a bionic hydrophobic coating on the surface of the starch nanofiber membrane in a self-assembly mode, so that a mixed solution is obtained.
The inventor finds that the concentration of stearic acid in the stearic acid ethanol solution can influence the water contact angle size of the formed hydrophobic starch food packaging film, and through multiple experiments, the concentration of stearic acid in the stearic acid ethanol solution is further set to be 0.025 mol/L-0.15 mol/L, and when the concentration of stearic acid is in the range, the concentration value is smaller or larger, and the water contact angle of the obtained hydrophobic starch food packaging film is larger; and when the concentration of stearic acid is 0.1mol/L, the water contact angle reaches the maximum value, so that the hydrophobic property of the hydrophobic starch food packaging film is greatly improved.
And step S32, washing the mixed solution by using absolute ethyl alcohol, and drying the precipitate to obtain the hydrophobic starch food packaging film.
According to the technical scheme provided by the invention, the starch nanofiber membrane is prepared by using an electrostatic spinning method, so that the operation is simple, the reaction is mild, the prepared nanofiber membrane has a smoother and more uniform fiber network compared with a common starch membrane, and the membrane performance is improved; through stearic acid treatment of the starch nanofiber membrane, a barrier is formed on the surface of the starch nanofiber membrane, water infiltration is avoided, and the water resistance of the food packaging membrane is improved.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
Accurately weighing 2.0g of starch, adding the starch into 10mL of 95% dimethyl sulfoxide aqueous solution, magnetically stirring at 70 ℃ to prepare 20% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
And soaking the prepared starch nanofiber membrane in a stearic acid ethanol solution with the concentration of 0.1mol/L, reacting at 60 ℃ for 1h, taking out, washing with absolute ethanol, and airing at room temperature to obtain the hydrophobic starch food packaging membrane.
Example 2
Accurately weighing 2.5g of starch, adding the starch into 10mL of 95% dimethyl sulfoxide aqueous solution, magnetically stirring at 70 ℃ to prepare 25% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
And soaking the prepared starch nanofiber membrane in a stearic acid ethanol solution with the concentration of 0.1mol/L, reacting at 60 ℃ for 1h, taking out, washing with absolute ethanol, and airing at room temperature to obtain the hydrophobic starch food packaging membrane.
Example 3
Accurately weighing 3.0g of starch, adding the starch into 10mL of 95% dimethyl sulfoxide aqueous solution, magnetically stirring at 70 ℃ to prepare 30% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
And soaking the prepared starch nanofiber membrane in a stearic acid ethanol solution with the concentration of 0.1mol/L, reacting at 60 ℃ for 1h, taking out, washing with absolute ethanol, and airing at room temperature to obtain the hydrophobic starch food packaging membrane.
Example 4
Accurately weighing 2.5g of starch, adding the starch into 10mL of 95% dimethyl sulfoxide aqueous solution, magnetically stirring at 70 ℃ to prepare 25% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
And soaking the prepared starch nanofiber membrane in a stearic acid ethanol solution with the concentration of 0.025mol/L, reacting at 60 ℃ for 1h, taking out, washing with absolute ethanol, and airing at room temperature to obtain the hydrophobic starch food packaging membrane.
Example 5
Accurately weighing 2.5g of starch, adding the starch into 10mL of 95% dimethyl sulfoxide aqueous solution, magnetically stirring at 70 ℃ to prepare 25% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
And soaking the prepared starch nanofiber membrane in a stearic acid ethanol solution with the concentration of 0.05mol/L, reacting at 60 ℃ for 1h, taking out, washing with absolute ethanol, and airing at room temperature to obtain the hydrophobic starch food packaging membrane.
Example 6
Accurately weighing 2.5g of starch, adding the starch into 10mL of 95% dimethyl sulfoxide aqueous solution, magnetically stirring at 70 ℃ to prepare 25% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
And soaking the prepared starch nanofiber membrane in a stearic acid ethanol solution with the concentration of 0.15mol/L, reacting at 60 ℃ for 1h, taking out, washing with absolute ethanol, and airing at room temperature to obtain the hydrophobic starch food packaging membrane.
Example 7
Accurately weighing 2.5g of starch, adding the starch into 10mL of 90% dimethyl sulfoxide aqueous solution, magnetically stirring at 65 ℃ to prepare 25% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
And soaking the prepared starch nanofiber membrane in a stearic acid ethanol solution with the concentration of 0.1mol/L, reacting at 70 ℃ for 1h, taking out, washing with absolute ethanol, and airing at room temperature to obtain the hydrophobic starch food packaging membrane.
Example 8
Accurately weighing 2.5g of starch, adding the starch into 10mL of 97% dimethyl sulfoxide aqueous solution, magnetically stirring at 75 ℃ to prepare 25% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
And soaking the prepared starch nanofiber membrane in a stearic acid ethanol solution with the concentration of 0.1mol/L, reacting at 50 ℃ for 1h, taking out, washing with absolute ethanol, and airing at room temperature to obtain the hydrophobic starch food packaging membrane.
Comparative example 1
Accurately weighing 1.5g of starch, adding the starch into 10mL of 95% dimethyl sulfoxide aqueous solution, magnetically stirring at 70 ℃ to prepare 15% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
Comparative example 2
Accurately weighing 2.5g of starch, adding the starch into 10mL of 95% dimethyl sulfoxide aqueous solution, magnetically stirring at 70 ℃ to prepare 25% (w/v) of starch solution, and standing at room temperature for defoaming to obtain the spinning solution.
Setting the spinning parameters as follows: the spinning environment temperature is 60 ℃, the electrostatic field voltage is 20kV, the spinning distance is about 15cm, and the flow rate of the spinning solution is l mL/h. The starch nanofiber membrane is prepared by an electrostatic spinning method.
And soaking the prepared starch nanofiber membrane in a stearic acid ethanol solution with the concentration of 0.01mol/L, reacting at 60 ℃ for 1h, taking out, washing with absolute ethanol, and airing at room temperature to obtain the hydrophobic starch food packaging membrane.
Performance testing
(one) observation of the starch nanofiber films obtained in examples 1 to 3 and the starch nanofiber film obtained in comparative example 1 by an electron microscope showed that the results are shown in FIGS. 1 to 4.
As can be seen from the figure, in comparative example 1, the entanglement among the starch molecular chains is insufficient, the interaction force is weak, the electric field force is not balanced enough, the stable electrostatic jet flow is formed, and the fiber structure or the beaded fiber cannot be formed; in examples 1-3, a fiber network structure was formed, and in examples 2 and 3, nanofibers with smooth and uniform surfaces were formed, and the diameter of the fibers in example 2 was 365 ± 97nm, which was smaller than that in examples 2 and 3.
(II) the starch nanofiber films prepared in example 2 and the hydrophobic starch food packaging films prepared in example 2, example 4 to example 6 and comparative example 2 were taken for electron microscope observation, and the results are shown in FIGS. 5 to 10. The arrows in the figure show the length direction of the nanofibers.
Comparing the length directions of the nanofibers in fig. 5 and 6, it can be seen that the nanofibers begin to bend after being modified with stearic acid. Further, comparing fig. 5 to 10, the microstructure of the starch nanofiber film appeared as a smooth, continuous and uniform fiber structure, while the fiber structure of the obtained hydrophobic starch food packaging film after being treated with the stearic acid solution gradually disappeared, the surface began to become rough, and the roughness increased as the concentration of stearic acid increased, and even when the concentration of stearic acid reached 0.05mol/L or more, the surface began to appear irregular "petaloid". This not only confirms the self-assembly behavior of stearic acid on the surface of the starch nanofiber membrane, but the increase in roughness is beneficial to increase the hydrophobicity of the membrane.
(III) X-ray photoelectron spectroscopy (XPS) was performed on starch, the starch nanofiber film prepared in example 2, and the hydrophobic starch food packaging film, and the results are shown in FIGS. 11 to 13.
As can be seen from the figure, the surface chemical compositions of the starch and the starch nanofiber membrane are substantially the same, which indicates that electrostatic spinning has no significant effect on the original chemical composition of the starch, while the XPS spectrum of the hydrophobic starch food packaging film shows new O-C ═ O chemical ester structure functional groups, which confirms that stearic acid is on the surface of the starch nanofiber, which is consistent with the SEM results obtained in test (ii).
(IV) the starch nanofiber film and the hydrophobic starch food packaging film prepared in example 2 were dropped with one drop of water on each of the two films, and the observation results are shown in FIG. 14. Wherein, a picture is a macroscopic image of the starch nanofiber membrane, and b picture is a macroscopic image of the hydrophobic starch food packaging membrane.
After comparison, the starch nanofiber membrane is obviously corroded by water and damaged, the shape of water drops on the hydrophobic starch food packaging film is round and smooth, the membrane is not permeated by the water drops, and the good waterproof performance is shown.
(V) the starch nanofiber films prepared in example 2 and the hydrophobic starch food packaging films prepared in examples 2, 4-6 and 2 were measured for water contact angle, and the results are shown in FIGS. 15 and 16. In FIG. 15, a is the starch nanofiber film prepared in example 2, and b to f are the hydrophobic starch food packaging films treated with stearic acid concentrations of 0.01mol/L, 0.025mol/L, 0.05mol/L, 0.1mol/L and 0.15mol/L in sequence; g shows the change of the starch nanofiber film prepared in example 2 when it was contacted with water droplets.
As can be seen from the figure, the water contact angle is basically kept unchanged after the water contact angle is gradually increased along with the increase of the stearic acid concentration, and when the stearic acid concentration is 0.1mol/L, the water contact angle of the starch nanofiber membrane reaches the maximum value, namely 134.7 degrees, and the starch nanofiber membrane shows higher hydrophobic performance.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.
Claims (6)
1. The preparation method of the hydrophobic starch food packaging film is characterized by comprising the following steps:
dissolving starch in dimethyl sulfoxide water solution to form spinning solution;
performing electrostatic spinning on the spinning solution to prepare a starch nanofiber membrane;
and (3) carrying out stearic acid modification on the starch nanofiber membrane to form a bionic hydrophobic coating on the surface of the membrane, and reacting to obtain the hydrophobic starch food packaging membrane.
2. The method of preparing a hydrophobic starch food packaging film according to claim 1, wherein the step of dissolving the starch in an aqueous solution of dimethyl sulfoxide to form a spinning solution is performed at 65 ℃ to 75 ℃.
3. The method for preparing the hydrophobic starch food packaging film according to claim 1, wherein in the step of dissolving the starch in the aqueous solution of dimethyl sulfoxide to form the spinning solution, the mass fraction of the starch in the spinning solution is 20% to 30%.
4. The method for preparing the hydrophobic starch food packaging film according to claim 1, wherein in the step of dissolving the starch in the aqueous dimethyl sulfoxide solution to form the spinning solution, the volume percentage concentration of the aqueous dimethyl sulfoxide solution is 90-97%.
5. The method for preparing the hydrophobic starch food packaging film according to claim 1, wherein the step of modifying the starch nanofiber film with stearic acid to form a bionic hydrophobic coating on the surface of the film and reacting to obtain the hydrophobic starch food packaging film comprises the following steps:
soaking the starch nanofiber membrane in a stearic acid ethanol solution, and reacting at 50-70 ℃ to enable stearic acid to form a bionic hydrophobic coating on the surface of the starch nanofiber membrane in a self-assembly manner, so as to obtain a mixed solution;
and washing the mixed solution by using absolute ethyl alcohol, and drying the precipitate to obtain the hydrophobic starch food packaging film.
6. The method for preparing the hydrophobic starch food packaging film according to claim 5, wherein the concentration of stearic acid in the stearic acid ethanol solution is 0.025mol/L to 0.15 mol/L.
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