CN113502058A - Biodegradable vinasse protein film and preparation method and application thereof - Google Patents
Biodegradable vinasse protein film and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a biodegradable vinasse protein film and a preparation method and application thereof, wherein the vinasse protein film is obtained by processing protein-modified vinasse protein through a film forming process, wherein a vinasse protein component subjected to protein modification comprises vinasse protein, a plasticizer, a cross-linking agent, a chain extender, a dihydric alcohol oligomer and a water repellent agent, and the preparation method and the application of the biodegradable vinasse protein film are further provided. The vinasse protein isolate is modified, so that the vinasse protein has the processability of traditional plastics, the water resistance and the mechanical strength of the vinasse protein film are improved, the vinasse protein film is more consistent with the characteristics of a film packaging material, the vinasse protein film is used for replacing the traditional non-degradable plastic film, the problem of pollution of the traditional plastics is solved, and the application range of vinasse is expanded.
Description
Technical Field
The invention belongs to the field of processing of biodegradable biopolymer materials, and particularly relates to a biodegradable vinasse protein film and a preparation method and application thereof.
Background
All over the world including China, a plurality of wine product manufacturers exist, and the vinasse is used as a byproduct in the wine making process, so that the yield is extremely high. The beer is used as water and tea, the world consumption of the third beverage is high, the beer yield is 3411.1 ten thousand liters in 2020 in China, the produced beer vinasse has ten thousand tons, and white spirit, yellow wine and the like occupy important positions in the alcoholic beverage industry in China, for example, the total yield of the white spirit in 2020 is 740.73 thousand liters in China, the byproduct white spirit vinasse also exceeds one hundred million tons, and the treatment, processing and reutilization of the vinasse also become a big problem. Until now, the vinasse is mainly applied to producing feed, chemical raw materials (such as phytic acid, glycerol, xylitol and the like) or fuels, and the added value of the vinasse is still worth being developed continuously.
Along with the upgrade of human consumption concept, the rise of vegetarian culture and the responsibility of our to environmental problems and animals, plant-based food and plant-based raw materials are more and more promoted, and the vinasse protein and other animal-based proteins (such as milk protein and the like) have the advantages that the vinasse protein is a plant source and meets the requirements of the era and the future society better, and in addition, compared with other plant-based protein films, the vinasse protein film has better mechanical properties, slow brightness and root sense, and in the research on the influence and mechanism of oleic acid and glycerol on the mechanical properties of the zein film, the fact that the zein is plasticized and modified is described, the tensile strength is maintained at about 12MPa at most; chenyiyong, Xuyu, in "study on characteristics of peanut protein film", it is described that the strength of peanut protein film is only about 1.4MPa at the highest under different heat treatments; the modified soybean protein isolate membrane is described in the research on the film forming property of the soybean protein isolate, the tensile strength of the soybean protein isolate membrane is only 7.97MPa in the optimal formula, and the mechanical strength of the vinasse protein membrane is closer to that of the traditional plastic, so that the application of the vinasse protein can be developed in a wider range, the vinasse protein membrane has higher potential to replace the traditional plastic, and disposable packaging film materials such as plastic bags, plastic packaging bags, food packaging bags and the like can be used.
At present, protein films in the research field are more concentrated on soybean protein and casein, waste vinasse is used as a development direction, the vinasse protein films are applied to packaging materials, the vinasse is changed into valuable, products with higher added values are realized, the application range of the waste vinasse is expanded, the thin film materials prepared from the vinasse are suitable for the outer packaging of various products, the vinasse protein is easy to extract and low in price, molecules have unique structural characteristics, side chains contain rich high-activity groups and are convenient to modify, but the mechanical property and the moisture resistance of the vinasse protein films are often lower than those of synthetic plastics, and the functional requirements of different products are difficult to meet.
Therefore, the biodegradable vinasse protein film and the preparation method and the application thereof are provided.
Disclosure of Invention
The invention aims to solve the problems and provides a biodegradable vinasse protein film and a preparation method and application thereof.
The invention realizes the purpose through the following technical scheme:
the biodegradable vinasse protein film is obtained by processing protein-modified vinasse protein through a film forming process, wherein the protein-modified vinasse protein component comprises vinasse protein, a plasticizer, a cross-linking agent, a chain extender, a dihydric alcohol oligomer and a water repellent agent.
As a further optimized scheme of the invention, the film forming process is casting film forming, casting film forming or film blowing.
As a further optimization scheme of the invention, the protein-modified vinasse protein component comprises, by mass, 60-85 parts of vinasse protein, 5-15 parts of a plasticizer, 0.3-2 parts of a cross-linking agent, 0.3-2 parts of a chain extender, 10-30 parts of a diol oligomer and 0.3-1 part of a water repellent agent.
As a further optimization scheme of the invention, the plasticizer is formamide, glycerol, deionized water or polyethylene glycol with molecular weight of 200-2000; the cross-linking agent is mixed anhydride, glutaraldehyde, carbodiimide or isocyanate.
As a further optimization scheme of the invention, the chain extender is ethylene glycol, propylene glycol, diethanolamine or triethanolamine.
As a further optimization scheme of the invention, the diol oligomer is polyester diol or polyether diol, wherein the hydroxyl value of the polyester diol is 40-50 mgKOH/g.
As a further optimization scheme of the invention, the water repellent agent is polyamide wax, hydroxyl silicone oil, polyamide polyurea or alkenyl succinic anhydride.
The preparation method of the vinasse protein film mainly comprises the following steps:
(1) modification of vinasse protein: the protein-modified vinasse protein component of claim 3, wherein the vinasse protein is put into an internal mixer, then the chain extender, the diol oligomer, the cross-linking agent, the plasticizer and the water repellent agent are sequentially put into the internal mixer, and the mixture reacts for 30-50min at the temperature of 80-110 ℃ and the rotating speed of 20-50rpm to obtain the modified protein for later use;
(2) film forming: processing the modified protein obtained in the step (1) according to the film forming process of claim 2 to obtain the vinasse protein film.
The application of the thin film of the vinasse protein in preparing a packaging material is to package food, package toiletries, package electronic products or print label paper.
Film forming mechanism of vinasse protein
The vinasse mainly comprises organic substances such as water, rice hulls, sugar, starch, protein and the like, but the types and the contents of nutrient components in the vinasse are different due to the difference of raw materials and production processes, and the vinasse protein and natural protein are consistent and form a stable structure by means of the interaction of hydrogen bonds, ionic bonds, disulfide bonds, water resistance and dipole interaction in molecules. However, when subjected to heat, acid, alkali, or salt, the subunits dissociate, and the intramolecular or intermolecular interactions of the protein are altered, thereby denaturing the protein. After denaturation, the molecular chain of the protein is opened, the hydrophobic groups in the protein can be exposed to form a new network structure, and then the moisture-resistant film with certain strength can be obtained through modification, grafting and subsequent film-forming processes.
Packing Properties of distillers' grains protein
The vinasse protein is mainly used as a packaging material to pay attention to the mechanical property, the moisture resistance, the oil resistance, the oxygen resistance and the like. The mechanical strength of the protein film is usually measured by Tensile Strength (TS), elongation at break (EB) and the like, the moisture resistance is expressed by a water vapor transmission coefficient (WVP), the larger the WVP value is, the poorer the moisture resistance is, and the moisture resistance can also be measured by the reduction rate of the mechanical property under high humidity (80% RH), the oil resistance can be expressed by referring to the swelling rate of the film in an oily liquid, the larger the swelling rate is, the poorer the oil resistance is, the main factors influencing the performance of the protein film are pH, heat treatment, a plasticizer, a water repellent agent and the like of the protein film, for example, the increase of the amount of the plasticizer increases the movement of chains, so that the air permeability is increased, and the barrier property to oxygen is reduced.
The invention has the beneficial effects that:
the vinasse protein isolate is modified, so that the vinasse protein not only has the processability of traditional plastics, but also improves the water resistance and the mechanical strength of a vinasse protein film, so that the vinasse protein film is more in line with the characteristics of a film packaging material, is used for replacing the traditional non-degradable plastic film, helps to solve the pollution problem of the traditional plastics, and simultaneously expands the application range of vinasse.
Detailed Description
The present application is described in further detail below, and it should be noted that the following detailed description is provided for further explanation of the present application only, and should not be construed as limiting the scope of the present application, and that the person skilled in the art can make modifications and adaptations of the present application based on the above-mentioned content.
A method for preparing a biodegradable vinasse protein film comprises the following steps,
(1) extracting vinasse protein: adding a certain amount of sodium hydroxide and alcohol mixed solution into the ground and crushed fresh vinasse for leaching, performing centrifugal/spin-drying separation after leaching to obtain vinasse residues and a leaching solution, performing secondary leaching on the vinasse residues, merging the leaching solution, adding a hydrochloric acid solution, adjusting PH, performing deionized water cleaning, performing centrifugal separation, repeating for three times, and performing spray drying to obtain vinasse protein;
(2) modification of vinasse protein: the proportion of protein modification comprises, by mass, 60-85 parts of vinasse protein, 5-15 parts of plasticizer, 0.3-2 parts of cross-linking agent, 0.3-2 parts of chain extender, 10-30 parts of diol oligomer and 0.3-1 part of water repellent agent, the vinasse protein is firstly put into an internal mixer, then the chain extender, the diol oligomer, the cross-linking agent, the plasticizer and the water repellent agent are sequentially put into the internal mixer, and the reaction is carried out for 30-50min at the temperature of 80-110 ℃ and the rotating speed of 20-50rpm to obtain the modified protein for later use.
(3) Film forming: processing the modified protein according to a pouring film forming, tape casting film forming or film blowing process to obtain a thin film of the protein in the distilled grains;
firstly, casting and film forming: adding 200-400 parts of deionized water into 100 parts of modified protein, dropwise adding alkaline solutions such as sodium hydroxide or triethylamine, controlling the pH to be 6-10 or dropwise adding acidic solutions such as hydrochloric acid and acetic acid, controlling the pH to be 3-7, pouring the protein into a mold after the protein is completely dissolved, and placing the mold into an oven at 50-80 ℃ for drying and molding.
Casting film forming/film blowing: the specific parameter settings are shown in table 1;
TABLE 1 cast/blown film parameter settings
Example 1
The embodiment provides a preparation method of a biodegradable vinasse protein film, which mainly comprises the following steps:
(1) modification of vinasse protein: the protein modified raw materials are proportioned, according to the mass parts, 60 parts of vinasse protein, 15 parts of plasticizer, 0.3 part of cross-linking agent, 2 parts of chain extender, 10 parts of dihydric alcohol oligomer and 1 part of water repellent agent, the vinasse protein is firstly put into an internal mixer, then the chain extender, the dihydric alcohol oligomer, the cross-linking agent, the plasticizer and the water repellent agent are sequentially put into the internal mixer, and the mixture reacts for 50min at the temperature of 90 ℃ and the rotating speed of 35rpm to obtain modified protein for later use;
(2) and (2) casting the modified protein obtained in the step (1) into a film to obtain the vinasse protein film.
Example 2
The embodiment provides a preparation method of a biodegradable vinasse protein film, which mainly comprises the following steps:
(1) modification of vinasse protein: the protein modified raw materials are proportioned, according to the mass parts, 85 parts of vinasse protein, 5 parts of plasticizer, 2 parts of cross-linking agent, 0.3 part of chain extender, 30 parts of dihydric alcohol oligomer and 0.3 part of water repellent agent, the vinasse protein is firstly put into an internal mixer, then the chain extender, the dihydric alcohol oligomer, the cross-linking agent, the plasticizer and the water repellent agent are sequentially put into the internal mixer, and the mixture reacts for 50min at the temperature of 90 ℃ and the rotating speed of 35rpm to obtain modified protein for later use;
(2) and (2) carrying out casting film forming processing on the modified protein obtained in the step (1) to obtain the vinasse protein film.
Example 3
The embodiment provides a preparation method of a biodegradable vinasse protein film, which mainly comprises the following steps:
(1) modification of vinasse protein: protein modified raw materials are proportioned, according to the mass parts, 62.9 parts of vinasse protein, 12 parts of plasticizer, 0.8 part of cross-linking agent, 0.5 part of chain extender, 23 parts of dihydric alcohol oligomer and 0.8 part of water repellent agent, the vinasse protein is put into an internal mixer, then the chain extender, the dihydric alcohol oligomer, the cross-linking agent, the plasticizer and the water repellent agent are put into the internal mixer in sequence, and the mixture reacts for 50min at the temperature of 90 ℃ and the rotating speed of 35rpm to obtain modified protein for later use;
(2) and (2) carrying out film blowing processing on the modified protein obtained in the step (1) to obtain the vinasse protein film.
Example 4
In order to verify the influence of different cross-linking agents on the performance of the thin film of the distillers 'grains protein, the embodiment provides a preparation method of a biodegradable thin film of the distillers' grains protein, which mainly comprises the following steps:
the protein modified raw material formula 1 comprises, by mass, 62.9 parts of vinasse protein, 12 parts of glycerol, 0.8 part of polycarbodiimide, 0.5 part of triethanolamine, 23 parts of polyester diol and 0.8 part of polyamide wax;
formula 2 differs from formula 1 in that the crosslinking agent is isocyanate;
formula 3 differs from formula 1 in that the crosslinking agent is glutaraldehyde;
(1) weighing protein modified raw materials according to the formulas 1, 2 and 3, putting the vinasse protein into an internal mixer, then putting the chain extender, the diol oligomer, the cross-linking agent, the plasticizer and the water repellent agent into the internal mixer in sequence, and reacting for 50min at the temperature of 90 ℃ and the rotating speed of 35rpm to obtain 3 groups of modified proteins for later use;
(2) film forming: and (2) casting the 3 groups of modified proteins obtained in the step (1) into a film, and processing the film to the thickness of 0.1mm to obtain the 3 groups of vinasse protein films.
The tensile strength test was performed on 3 groups of thin films of distillers' grains protein, and the results are shown in Table 2,
TABLE 2 Effect of different crosslinking Agents on tensile Strength of thin films of distillers' grains protein
| Formulation of | Crosslinking agent | Tensile Strength (MPa) | Elongation at Break (%) |
| 1 | Polycarbodiimide | 12.94 | 13.47 |
| 2 | Isocyanates | 10.22 | 19.82 |
| 3 | Glutaraldehyde | 8.76 | 24.49 |
The data result shows that when the polycarbodiimide is used as the crosslinking agent, the prepared vinasse protein film has the largest tensile strength and the lowest elongation at break in a test group, and different crosslinking agents can be selected to modify the vinasse protein according to the application requirements of different packaging materials.
Example 5
In order to verify the influence of the content of the polyester diol on the performance of the thin film of the vinasse protein, the embodiment provides a preparation method of the biodegradable thin film of the vinasse protein, which mainly comprises the following steps:
the protein modified raw material formula 1 comprises, by mass, 76.9 parts of vinasse protein, 12 parts of glycerol, 0.8 part of polycarbodiimide, 0.5 part of triethanolamine, 9 parts of polyester diol and 0.8 part of polyamide wax;
the difference between the formula 2 and the formula 1 is that 69.9 parts of vinasse protein and 16 parts of polyester dihydric alcohol;
the difference between the formula 3 and the formula 1 is that the formula comprises 62.9 parts of vinasse protein and 23 parts of polyester dihydric alcohol;
the formula 4 is different from the formula 1 in that 85.9 parts of vinasse protein and 0 part of polyester dihydric alcohol are added;
(1) weighing protein modified raw materials according to the formulas 1, 2, 3 and 4 in sequence, putting the vinasse protein into an internal mixer, then putting the chain extender, the diol oligomer, the cross-linking agent, the plasticizer and the water repellent agent in sequence, and reacting for 50min at the temperature of 90 ℃ and the rotating speed of 35rpm to obtain 4 groups of modified proteins for later use;
(2) film forming: and (2) carrying out casting film forming on the 4 groups of modified proteins obtained in the step (1) until the thickness is 0.1mm, and obtaining a 3 group of vinasse protein film.
The 3 groups of thin films of distillers' grains protein were subjected to a strength test, and the results are shown in Table 3,
TABLE 3 Effect of different polyester diol contents on the film strength of distillers' grains protein
| Formulation of | Polyester diol (portion) | Tensile Strength (MPa) | Elongation at Break (%) |
| 1 | 9 | 16.49 | 2.96 |
| 2 | 16 | 14.87 | 7.72 |
| 3 | 23 | 13.86 | 14.56 |
| 4 | 0 | 20.15 | 0.96 |
The data result shows that in the protein modification, the tensile strength is reduced to a certain extent and the brittleness is increased with the increase of the addition amount of the polyester diol, but the elongation at break is obviously improved and the flexibility is obviously improved, so that the brittleness of the film can be obviously improved and the ductility and the toughness of the film can be improved by the polyester diol with a proper addition amount.
Example 6
In order to verify the influence of a water repellent agent on the performance of a thin film of distillers 'grains protein, the embodiment provides a preparation method of a biodegradable thin film of distillers' grains protein, which mainly comprises the following steps:
the protein modified raw material formula 1 comprises, by mass, 62.9 parts of vinasse protein, 12 parts of glycerol, 0.8 part of polycarbodiimide, 0.5 part of triethanolamine, 9 parts of polyester diol and 0 part of polyamide wax;
formulation 2 differs from formulation 1 in that 0.4 part of polyamide wax is present
Formulation 3 differs from formulation 1 in that 0.8 parts of polyamide wax;
(1) weighing protein modified raw materials according to the formulas 1 and 2, putting the vinasse protein into an internal mixer, then putting the chain extender, the diol oligomer, the cross-linking agent, the plasticizer and the water repellent agent into the internal mixer in sequence, and reacting for 50min at the temperature of 90 ℃ and the rotating speed of 35rpm to obtain 3 groups of modified proteins for later use;
(2) film forming: and (2) processing the 3 groups of modified proteins obtained in the step (1) to the thickness of 0.1mm by film blowing to obtain the 3 groups of vinasse protein films.
The 2 groups of vinasse protein films are subjected to tensile strength tests under different humidity environments, the results are shown in Table 4,
TABLE 4 Effect of Water repellents on moisture resistance of thin films of distillers' grains protein
The data result shows that in the protein modification, after the water repellent agent polyamide wax is added, the tensile strength of the vinasse protein film can be maintained at a relatively high level when the test is carried out in an environment with high humidity of 80% RH, and the polyamide wax has an obvious effect on the moisture resistance of the film.
As used in the specification and claims, certain terms are used to refer to particular components or methods. As one skilled in the art will appreciate, different regions may refer to a component by different names. The present specification and claims do not intend to distinguish between components that differ in name but not in name. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect. The description which follows is a preferred embodiment of the present application, but is made for the purpose of illustrating the general principles of the application and not for the purpose of limiting the scope of the application. The scope of protection of the present application shall be determined by the claims appended hereto.
It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a commodity or system that includes the element.
While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The biodegradable vinasse protein film is characterized by being obtained by processing protein-modified vinasse protein through a film forming process, wherein the protein-modified vinasse protein comprises the vinasse protein, a plasticizer, a cross-linking agent, a chain extender, a diol oligomer and a water repellent agent.
2. The biodegradable thin film of distillers' grains protein as claimed in claim 1, wherein said film-forming process is casting, casting or blowing.
3. The biodegradable thin film of distillers ' grains protein as claimed in claim 1, wherein the fraction of the protein-modified distillers ' grains protein component includes, by weight, 60-85 parts of distillers ' grains protein, 5-15 parts of plasticizer, 0.3-2 parts of cross-linking agent, 0.3-2 parts of chain extender, 10-30 parts of diol oligomer, and 0.3-1 part of water repellent agent.
4. The biodegradable thin film of distillers' grains protein as claimed in claim 3, wherein the plasticizer is formamide, glycerol, deionized water or polyethylene glycol with molecular weight of 200-2000; the cross-linking agent is mixed anhydride, glutaraldehyde, carbodiimide or isocyanate.
5. The biodegradable thin film of distillers' grains protein as claimed in claim 3, wherein said chain extender is selected from the group consisting of ethylene glycol, propylene glycol, diethanolamine and triethanolamine.
6. The biodegradable thin film of distillers' grains protein as claimed in claim 3, wherein said diol oligomer is polyester diol or polyether diol, and the hydroxyl value of polyester diol is 40-50 mgKOH/g.
7. The biodegradable thin film of distiller's grain protein of claim 3, wherein the water repellent is polyamide wax, hydroxy silicone oil, polyamide polyurea or alkenyl succinic anhydride.
8. The method for preparing the thin film of the distillers' grains protein according to any one of claims 1-7, comprising the steps of:
(1) modification of vinasse protein: the protein-modified vinasse protein component proportioning method of claim 3, comprising the steps of putting vinasse protein into an internal mixer, sequentially adding a chain extender, a diol oligomer, a cross-linking agent, a plasticizer and a water repellent agent, and reacting at 80-110 ℃ and 20-50rpm for 30-50min to obtain modified protein for later use;
(2) film forming: and (2) processing the modified protein obtained in the step (1) through a film forming process to obtain the vinasse protein film.
9. Use of a thin film of a distillers' grains protein according to any one of claims 1-7 for the preparation of a packaging material, wherein: the packaging material is food packaging, toiletries packaging, electronic product outer packaging or printable label paper.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114196216A (en) * | 2021-12-27 | 2022-03-18 | 杭州靡特洛新材料科技有限公司 | Full-biodegradable thermoplastic water-soluble film based on vinasse waste and preparation method and application thereof |
| CN114306186A (en) * | 2021-12-31 | 2022-04-12 | 中国农业科学院特产研究所 | Hydrogel mask with vinasse protein melanin and poplar bud total flavonoids as main raw materials and preparation method thereof |
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| CN114306186B (en) * | 2021-12-31 | 2023-07-14 | 中国农业科学院特产研究所 | Hydrogel mask with distillers' grains protein melanin and Yang Shuya total flavonoids as main raw materials and preparation method thereof |
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