CN115386115A - Preparation process of high-mechanical-strength soybean protein isolate composite membrane - Google Patents
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- CN115386115A CN115386115A CN202211039954.4A CN202211039954A CN115386115A CN 115386115 A CN115386115 A CN 115386115A CN 202211039954 A CN202211039954 A CN 202211039954A CN 115386115 A CN115386115 A CN 115386115A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K2003/2241—Titanium dioxide
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention provides a preparation process of a high-mechanical-strength soybean protein isolate composite membrane, and relates to the technical field of food processing. The preparation process of the high-mechanical-strength soybean protein isolate composite membrane mainly comprises the following steps: nano TiO 2 2 The method comprises the steps of ultrasonic dispersion, nano particle and heating composite modification treatment of protein, drying and film forming and the like. The invention improves the defects of the existing film forming technology, provides a preparation process of a soybean protein isolate film with high mechanical strength, solves the problems of poor mechanical strength, poor water resistance and oxygen permeability of the soybean protein isolate film and the like, and simultaneously improves the application of the soybean protein isolate in the technical field of food processingThe combined development of the material and soybean processing industry aims to realize the comprehensive full utilization of the soybean processing industry.
Description
The invention relates to the technical field of food material processing, in particular to a preparation process of a high-mechanical-strength soybean protein isolate composite membrane.
Background
The film preservation technology of food is developed very rapidly in recent decades due to its unique superiority. The fresh-keeping method can inhibit gas exchange between food and the environment, reduce evaporation of water in the food, prevent oxidation between oxygen in the air and the food, and prevent breeding of microorganisms, thereby better maintaining the nutritive value, color, fragrance, taste and shape of the food and prolonging the shelf life of the food. At present, the research on edible films mainly focuses on material selection, processes, equipment and the like, and achieves industrial success. However, edible films of polysaccharides have been mainly studied, and edible protein films have been studied less frequently, especially in large sizeThe protein film based on the bean protein isolate is lack of systematic research and practical application. Nanotechnology has revolutionized almost all areas of science and technology, particularly the food packaging industry. Thus, some nanoparticles may be used in food contact materials to preserve food for longer periods of time. Inorganic Nanoparticles (NPs) are three extremely important properties, low volatility, stability and broad spectrum anti-foodborne pathogen activity. To date, many inorganic and metallic nanoparticles have been used to synthesize active food packaging materials and extend the shelf life of food. Packaging with nanocomposites containing these nanoparticles can enhance the physicochemical properties of the film, such as enhancing the mechanical properties, water-blocking properties and antibacterial and antioxidant properties of the protein film, reducing the use of preservatives and increasing the reaction rate for inhibiting microbial growth. Nano titanium dioxide (TiO) 2 ) The nano-particle is an economic and stable metal oxide nano-particle, is one of the most actively researched inorganic nano-materials at present, and is known as a functional nano-filler which can be used for manufacturing biodegradable food packaging films due to the excellent biocompatibility, photocatalysis and antibacterial properties. Dispersing treated nanometer TiO with soybean protein isolate as main film matrix and glycerin as plasticizer 2 The soybean protein isolate membrane with high mechanical strength is prepared for the modifier, so that the performance of the soybean protein-based membrane is improved and the soybean protein-based membrane is applied to the field of food preservation. The composite film can meet the needs of consumers, further improve the practicability of the composite film, enable the composite film to be commercially produced on a large scale, and promote the novel material of the health food of high-quality vegetable protein in the healthy diet of the whole people.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation process of a high-mechanical-strength soybean protein isolate composite membrane, which solves the problems that a soybean protein isolate membrane is low in tensile strength, poor in elongation and easy to cause bacterial breeding and the like, improves the mechanical strength of the obtained soybean protein isolate-based membrane, realizes the maximization embodiment of the nutrition and health advantages of vegetable protein, increases the industrial production value of the membrane, and hopes that the membrane can be produced on a large scale in the near future to innovate a safe method for using nano particles in food contact materials, thereby creating favorable conditions for the actual production and industrialized application of the soybean protein isolate-based membrane.
In order to achieve the above purpose, the technical scheme of the invention is realized by the following technical scheme:
(1) Mixing nanometer TiO 2 Adding into deionized water in a beaker, and performing ultrasonic dispersion by using an ultrasonic processor (JRA-650, china) and a probe (20 kHz, phi 6); (2) Adding SPI and glycerol into the nanoparticle dispersion solution; (3) Stirring at room temperature until the mixture is completely mixed, and adjusting the pH value by using a buffer solution; (4) Placing the mixed membrane liquid in a digital display constant-temperature water bath kettle for heat treatment, and stirring at a constant rotating speed; (5) standing the mixed membrane liquid at room temperature; (6) And pouring the film forming solution into a flat plastic culture dish, and drying at constant temperature. (7) And taking the dried membrane out of the culture dish, and placing the membrane in a constant temperature and humidity incubator for 2 days to obtain the soybean protein isolate basement membrane product. Preferably, the nano TiO in the step (1) 2 Adding into 100mL deionized water and performing ultrasonic dispersion for 15min, wherein the concentration is controlled at 0%, 1%, 3%, 5%, 7%, 9% (w/w SPI). Preferably, 4g of SPI and 1.2g of glycerol are added to the nanoparticle dispersion solution in step (2). Preferably, in step (3), stirring is carried out at room temperature for 40min until mixing is complete, and the pH is adjusted to 10.0 with a hydrochloric acid buffer solution (2M). Preferably, the temperature of the water bath of the mixed membrane solution in the step (4) is 60 ℃, the rotating speed is 1100r/min, and the reaction time is set to be 60min. Preferably, in the step (5), the mixed membrane solution is allowed to stand at room temperature for 30min to remove air bubbles and cooled to room temperature. Preferably, step (6) takes 15mL of the film-forming solution and pours it into a flat plastic petri dish and dries it at 60 ℃ for 3h. Preferably, step (7) removes the dried film from the petri dish and places it under controlled conditions of 25 ℃ and 50% Relative Humidity (RH) for 2d. Preferably, the nano TiO with the concentration of 7% (w/w SPI) 2 And carrying out composite treatment on the soybean protein and 4g of soybean protein, heating and stirring to obtain a mixed membrane liquid, and drying to obtain the soybean protein-based film, wherein the heating temperature of the mixed membrane liquid is 60 ℃, the rotating speed is 1100r/min, the mixed membrane liquid is heated in a water bath for 60min, and the drying time is 60min.
The invention provides a high machineCompared with the prior art, the preparation process of the composite membrane of the soybean protein isolate with mechanical strength has the advantages that: (1) The invention uses different nano particles for preparing the soy isolate protein composite film, does not relate to toxic chemical raw materials, is safe, green and pollution-free, and provides theoretical and technical support for expanding the application of the soy isolate protein biomass resources. (2) The soy protein-based film with higher mechanical strength and application performance is preferably selected by a fixed preparation method. The invention adopts nano TiO 2 The soybean protein isolate is modified, and the hydrophobic bond, the hydrogen bond and the disulfide bond of the film product are recombined, so that the mechanical strength and the related performance of the obtained composite film are obviously improved. (3) The invention realizes the prominent mechanical property of the nano particle composite membrane by improving and optimizing the membrane structure and the performance through physical-chemical interaction, and provides reference for creating a blend membrane product with comprehensive functions.
Drawings
FIG. 1 effect of nanoparticle concentration on tensile strength of soy isolate protein based films;
FIG. 2 effect of nanoparticle concentration on elongation at break of soy protein isolate-based films;
FIG. 3 the effect of nanoparticle concentration on oxygen permeability of soy protein isolate-based films;
FIG. 4 effect of nanoparticle concentration on water permeability of soy protein isolate-based films;
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 are described below clearly and completely in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
A preparation process of a high-mechanical-strength soybean protein isolate composite membrane comprises the following steps: (1) Mixing nanometer TiO 2 Added to deionized water in a beaker, sonicated using a sonicator (JRA-650,china) and a probe (20 kHz, phi 6) are subjected to ultrasonic dispersion; (2) Adding SPI and glycerol into the nano particle dispersion solution; (3) Stirring at room temperature until the mixture is completely mixed, and adjusting the pH value by using a buffer solution; (4) Placing the mixed membrane liquid in a digital display constant-temperature water bath kettle for heat treatment, and stirring at a constant rotating speed; (5) standing the mixed membrane liquid at room temperature; (6) And pouring the film forming solution into a flat plastic culture dish, and drying at constant temperature. (7) And taking out the dried membrane from the culture dish, and placing the membrane in a constant temperature and humidity incubator for 2 days to obtain the soybean protein isolate composite membrane product.
Example 1:
a preparation process of a high-mechanical-strength soybean protein isolate composite membrane comprises the following steps: step (1) nanometer TiO 2 Adding into deionized water in a beaker, and performing ultrasonic dispersion for 15min by using an ultrasonic processor (JRA-650, china) and a probe (20 kHz, phi 6); step (2) adding 4g of SPI and 1.2g of glycerol into the nano TiO 2 Dispersing in the solution; stirring at room temperature for 40min until the components are completely mixed, and adjusting the pH value to 10.0 by using a hydrochloric acid buffer solution (2M); placing the mixed membrane liquid in a digital display constant-temperature water bath kettle for heat treatment at 60 ℃, and stirring at a constant rotation speed of 1100r/min for 60min; standing the mixed membrane liquid at room temperature for 30min to remove bubbles and cooling to room temperature; pouring 15mL of film forming solution into a flat plastic dish, and drying at constant temperature; and (7) taking the membrane out of the culture dish, placing the membrane in a constant temperature and humidity incubator, and obtaining the soybean protein isolate basement membrane product under the control conditions of 25 ℃ and 50% Relative Humidity (RH) for 2d. Wherein, the nano TiO 2 Concentrations were set at 0%, 1%, 3%, 5%, 7%, 9% (w/w SPI), respectively.
The following parameters are set: each film was cut into 500X 100mm rectangles, measured with a texture analyser (model TA-XT2 texture analyser), set at 50mm separation of the initial grip of the film fixing and stretched at a cross speed of 5 mm/s. The tensile strength of different film products was tested and the results are shown in figure 1.
Example 2:
preparation of high-mechanical-strength soybean protein isolate composite membraneThe preparation process comprises the following steps: step (1) nanometer TiO 2 Adding into deionized water in a beaker, and performing ultrasonic dispersion for 15min by using an ultrasonic processor (JRA-650, china) and a probe (20 kHz, phi 6); step (2) adding 4g of SPI and 1.2g of glycerol into the nano TiO 2 Dispersing in the solution; stirring at room temperature for 40min until the components are completely mixed, and adjusting the pH value to 10.0 by using a hydrochloric acid buffer solution (2M); placing the mixed membrane liquid in a digital display constant-temperature water bath kettle for heat treatment at 60 ℃, and stirring at a constant rotation speed of 1100r/min for 60min; standing the mixed membrane liquid at room temperature for 30min to remove bubbles and cooling to room temperature; pouring 15mL of film forming solution into a flat plastic dish, and drying at constant temperature; and (7) taking the membrane out of the culture dish, placing the membrane in a constant temperature and humidity incubator, and obtaining the soybean protein isolate basement membrane product under the control conditions of 25 ℃ and 50% Relative Humidity (RH) for 2d. Wherein, the nanometer TiO 2 Concentrations were set at 0%, 1%, 3%, 5%, 7%, 9% (w/w SPI), respectively.
The following parameters are set: each film was cut into 500X 100mm rectangles, measured with a texture analyser (model TA-XT2 texture analyser), set at 50mm separation of the initial grip of the film fixing and stretched at a cross speed of 5 mm/s. The elongation at break of the different film products was measured and the results are shown in figure 2.
Example 3:
a preparation process of a high-mechanical-strength soybean protein isolate composite membrane comprises the following steps: step (1) nanometer TiO 2 Adding into deionized water in a beaker, and performing ultrasonic dispersion for 15min by using an ultrasonic processor (JRA-650, china) and a probe (20 kHz, phi 6); step (2) adding 4g of SPI and 1.2g of glycerol into the nano TiO 2 Dispersing in the solution; stirring at room temperature for 40min until the components are completely mixed, and adjusting the pH value to 10.0 by using a hydrochloric acid buffer solution (2M); step (4) placing the mixed membrane liquid in a digital display constant temperature water bath for 60 ℃ heat treatment, and stirring for 60min at a constant rotation speed of 1100 r/min; standing the mixed membrane liquid at room temperature for 30min to remove bubbles and cooling to room temperature; pouring 15mL of film forming solution into a flat plastic dish, and drying at constant temperature; step (ii) of(7) And taking the membrane out of the culture dish, placing the membrane in a constant temperature and humidity incubator, and obtaining the soybean protein isolate-based membrane product of the invention under the control conditions of 25 ℃ and 50% Relative Humidity (RH) for 2 days. Wherein, the nanometer TiO 2 Concentrations were set at 0%, 1%, 3%, 5%, 7%, 9% (w/w SPI), respectively. Finally, the oxygen transmission rates were measured for the different film samples, and the results are shown in FIG. 3.
Determination of oxygen permeability of the film: the flask was charged with 1mL linoleic acid and sealed with a film. The oxygen transmission rate OP of the material was measured at a temperature of 23 ℃ and a relative humidity of 50%, wherein: OTR is expressed as oxygen transmission rate (g/m) 2 D), Δ P is the vapor pressure difference (kPa) between the two sides of the film to be measured, and D is the average thickness (m) of the film. The calculation formula is as follows:
example 4:
a preparation process of a high-mechanical-strength soybean protein isolate composite membrane comprises the following steps: step (1) adding nano TiO 2 Adding into deionized water in a beaker, and performing ultrasonic dispersion for 15min by using an ultrasonic processor (JRA-650, china) and a probe (20 kHz, phi 6); step (2) adding 4g of SPI and 1.2g of glycerol into the nano TiO 2 Dispersing in the solution; stirring at room temperature for 40min until the mixture is completely mixed, and adjusting the pH value to 10.0 by using a hydrochloric acid buffer solution (2M); placing the mixed membrane liquid in a digital display constant-temperature water bath kettle for heat treatment at 60 ℃, and stirring at a constant rotation speed of 1100r/min for 60min; standing the mixed membrane liquid at room temperature for 30min to remove bubbles and cooling to room temperature; pouring 15mL of film forming solution into a flat plastic dish, and drying at constant temperature; and (7) taking the membrane out of the culture dish, placing the membrane in a constant temperature and humidity incubator, and obtaining the soybean protein isolate basement membrane product under the control conditions of 25 ℃ and 50% Relative Humidity (RH) for 2d. Wherein, the nano TiO 2 Concentrations were set at 0%, 1%, 3%, 5%, 7%, 9% (w/w SPI), respectively. Finally, the water permeability of the different film samples was measured and the results are shown in FIG. 4。
Determination of water permeability of the film: 1.5g of anhydrous CaCl is added into a weighing bottle 2 To maintain a relative humidity of 0% in the weighing flask. Each vial was sealed at the mouth with a film. The weighed bottle was then placed in a constant temperature and humidity incubator set at 25 ℃ and a humidity of 83% RH 7d and weighed once every 24h until a constant weight was reached. The water permeability (WVP) is calculated according to the following formula:
according to the experimental results of the drawings in the specification, the nano TiO can be found 2 The concentration is improved, and the tensile strength TS is along with the nano TiO 2 May be increased due to the increase of nano-TiO 2 As an effective filler in the matrix, the soybean protein film has large surface area, is uniformly embedded in the amorphous area of the soybean protein film, establishes strong interface interaction with the peptide chain side chain of the soybean protein film, and has elongation at break E along with nano TiO 2 Increase and decrease, and these results all indicate that nano TiO 2 The mechanical property of the SPI basal membrane is obviously improved by adding the (5). For edible polymer films in food packaging, water and oxygen permeability are important properties, and it can be seen from figure 3 that the water permeability of the composite film shows a significant difference compared to the SPI film (P)<0.05 Significantly decreased). This is because of the nano TiO 2 When the using amount is low, the nano particles are uniformly dispersed in the amorphous area of the soybean protein film and interact with the side chain of the peptide chain of the soybean protein, so that the formed composite film is compact and uniform, the permeation path of water molecules in the film is changed, and the water resistance of the composite film is enhanced; when nano TiO 2 When the amount is too high (9%), secondary agglomeration of the nanoparticles is enhanced, so that the compactness of the composite membrane is deteriorated and the water permeability is increased. Because the protein molecules are arranged more closely and the SPI membrane structure is more compact, the membrane has better oxygen resistance and oxygen molecules are difficult to pass through. In contrast, with nano TiO 2 The oxygen permeability of the composite film is increased continuously when the addition amount is continuously added, because the nano TiO 2 A mesoporous structure is provided for the surface of the SPI film, and the fact that the nano material can be better combined with an organic phase under the film forming condition is proved. In conclusion, the nano TiO is selected 2 The concentration of the mixture is 7 percent,
although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A preparation process of a soy protein isolate composite film with high mechanical strength is characterized by comprising the following steps: (1) Mixing nanometer TiO 2 Adding into deionized water in a beaker, and performing ultrasonic dispersion by using an ultrasonic processor (JRA-650, china) and a probe (20 kHz, phi 6); (2) Adding SPI and glycerol into the nano particle dispersion solution; (3) Stirring at room temperature until the mixture is completely mixed, and adjusting the pH value by using a buffer solution; (4) Placing the mixed membrane liquid in a digital display constant-temperature water bath kettle for heat treatment, and stirring at a constant rotating speed; (5) standing the mixed membrane liquid at room temperature; (6) And pouring the film forming solution into a flat plastic culture dish, and drying at constant temperature. (7) And taking the membrane out of the culture dish, and placing the membrane in a constant temperature and humidity incubator for 2 days to obtain the soybean protein isolate composite membrane product.
2. The process for preparing a soy protein isolate composite film with high mechanical strength as claimed in claim 1, wherein: in the step (1), nano TiO 2 Added into 100mL deionized water and ultrasonically dispersed for 15min, and the concentration is controlled at 7% (w/w SPI).
3. The process for preparing a soy protein isolate composite film with high mechanical strength as claimed in claim 1, wherein: in the step (2), 4g of SPI and 1.2g of glycerin were added to the nanoparticle dispersion solution.
4. The process for preparing a soy protein isolate composite film with high mechanical strength as claimed in claim 1, wherein: in step (3), stirring was carried out at room temperature for 40min until complete mixing, and the pH was adjusted to 10.0 with hydrochloric acid buffer solution (2M).
5. The process for preparing the soy protein isolate composite film with high mechanical strength as claimed in claim 1, wherein: in the step (4), the water bath temperature of the mixed membrane solution is 60 ℃, the rotating speed is 1100r/min, and the reaction time is set to be 60min.
6. The process for preparing a soy protein isolate composite film with high mechanical strength as claimed in claim 1, wherein: and (5) standing the mixed membrane liquid at room temperature for 30min to remove bubbles and cooling to room temperature.
7. The process for preparing a soy protein isolate composite film with high mechanical strength as claimed in claim 1, wherein: step (6) 15mL of the film forming solution was poured into a flat plastic petri dish and dried at 60 ℃ for 3h.
8. The process for preparing a soy protein isolate composite film with high mechanical strength as claimed in claim 1, wherein: step (7) the dried film was removed from the petri dish and placed under controlled conditions of 25 ℃ and 50% Relative Humidity (RH) for 2d.
9. The process for preparing a soy protein isolate composite film with high mechanical strength as claimed in claim 1, wherein: the mixture contains 7 percent (w/w SPI) concentration of nano TiO 2 And (2) carrying out composite treatment on the soybean protein and 4g of soybean protein, heating and stirring to obtain a mixed membrane liquid, and drying to obtain the soybean protein isolate composite membrane, wherein the heating temperature of the mixed membrane liquid is 60 ℃, the rotating speed is 1100r/min, the membrane liquid is heated in a water bath for 60min, and the drying time is 60min.
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| CN116284899B (en) * | 2023-01-17 | 2023-10-20 | 哈尔滨商业大学 | Preparation method of soybean protein isolate composite membrane |
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