CN115449171A - Preparation method of high-strength and high-toughness starch-based pH-responsive intelligent indicating film - Google Patents
Preparation method of high-strength and high-toughness starch-based pH-responsive intelligent indicating film Download PDFInfo
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- 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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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
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- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/80—Indicating pH value
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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
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/02—Starch; Degradation products thereof, e.g. dextrin
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
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- G01N2021/775—Indicator and selective membrane
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Abstract
The invention discloses a preparation method of a high-strength and high-toughness starch-based pH-responsive intelligent indicating film. The visual intelligent indicating film prepared from the purple cabbage pigment is sensitive to pH value change in the environment, can accurately feed back freshness information of meat products, is expected to be applied to real-time freshness monitoring of the meat products, is improved in mechanical property compared with a starch-based film with a single component, has degradability, is non-toxic and harmless, and has a wide application prospect.
Description
Technical Field
The invention relates to the technical field of intelligent packaging and food quality detection, in particular to a preparation method of a high-strength high-toughness starch-based pH-responsive intelligent indicating film.
Background
In the national food safety standard fresh (frozen) livestock and poultry products (GB 2707-2016), freshness becomes an important judgment index for meat product quality. However, in order to prolong the shelf life of meat products, the meat products are usually stored in a sealed package in a supermarket, the freshness of the meat products is difficult to directly judge through sense organ, and even part of the meat packaged food may deteriorate before the shelf life due to storage, transportation and the like. Therefore, the quick nondestructive testing of the freshness of the meat products in the sealed package has important practical value.
The meat food is rich in protein, and under the decomposition action of bacteria, the nitrogenous amino acid undergoes decarboxylation or deamination to generate ammonia/amine, namely volatile basic total nitrogen (TVB-N). The existing TVB-N testing method is mainly carried out according to a chemical titration method (GB/T5009.44-2003), needs to be operated by professional technicians, is complex in flow and long in time consumption, and cannot meet the requirement of real-time detection. The freshness indicating film has the advantages of small volume, degradability, high strength, visualization and the like, and can react with ammonia/amine in meat products to cause the color change of the indicating film, thereby indicating the freshness of the food products.
However, the existing smart indicator film has the following problems:
(1) When the natural anthocyanin is compounded with other substances, the problems of poor stability, easy degradation under the action of light, easy oxidation by oxygen and the like exist, and the popularization and the application of the natural anthocyanin are limited.
(2) The mechanical property, degradability and stability of the intelligent indicating film are poor, and the comprehensive performance needs to be further improved.
(3) Currently, the commonly used chemically synthesized freshness indicators such as bromocresol green, methyl red, bromocresol purple and the like contain certain toxicity and have potential safety hazards.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a high-strength and high-toughness starch-based pH-responsive intelligent indicating film, which solves the problems of low strength, easy mildew generation and complicated preparation steps of the starch-based intelligent indicating film in the prior art and also solves the problems of environmental protection and safety of common chemically synthesized freshness indicators such as bromocresol green, methyl red, bromocresol purple and the like.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a high-strength and high-toughness starch-based pH-responsive intelligent indicating film specifically comprises the following steps:
(1) Putting starch and polyvinyl alcohol into a heating container, adding glycerol, pouring distilled water, and uniformly mixing to prepare a starch-polyvinyl alcohol solution; the glycerol accounts for 20% of the total mass of the starch and the polyvinyl alcohol, and after the volume is fixed, the mass fraction of the starch-polyvinyl alcohol in the starch-polyvinyl alcohol solution is 10%.
The starch is used as a polyhydroxy natural polymer material, has rich resources, low price and good biocompatibility and biodegradability. The polyvinyl alcohol and starch are selected for blending to prepare the membrane, because the PVA is used as a synthesized water-soluble polymer material, has a single C-C main chain and a polyhydroxy strong hydrogen bond molecular structure, and has good toughness, biocompatibility and mechanical property. The glycerol has the functions of enhancing the gas barrier performance of the starch-based film and improving the transparency, and the transparency is highest when the addition amount of the glycerol is 20 percent of the total mass of the starch-polyvinyl alcohol. The starch adopted is soluble starch, the PVA specification is 1788 type, and the solubility is 88%.
(2) Gelatinizing in a water bath, adding CNC, continuously heating and stirring until the solution is semitransparent, and stopping heating; preferably, gelatinization is carried out in a 95 ℃ water bath for 1h.
The CNC can be used as a reinforcing agent to reinforce the strength of the composite material, effectively improve the performance of the starch film and reduce the water absorption. The digital display heating constant temperature water bath is adopted for heating, and the heat collection type magnetic stirrer is adopted for stirring.
(3) And after cooling to room temperature, adding the purple cabbage pigment into the mixed solution, and performing ultrasonic dispersion by using a 100W ultrasonic cleaning machine.
The purple cabbage pigment mainly comprises anthocyanin, wherein the acylated anthocyanin is higher in proportion and higher in stability than other sources, and the purple cabbage pigment is also a non-toxic and harmless natural pigment and can show different colors along with the change of pH value. And (4) oscillating by adopting an ultrasonic cleaning machine.
(4) And pouring 25mL of the mixed solution B into a plastic culture dish to form a film, drying in a constant-temperature drying oven, removing the film, and storing for later use.
According to the preparation method of the high-strength high-toughness starch-based pH-responsive intelligent indicating membrane, the plastic culture dish is square, and the side length is 13cm.
According to the preparation method of the high-strength and high-toughness starch-based pH-responsive intelligent indicating film, the starch is soluble starch, the PVA specification is 1788 type, and the solubility is 88%.
In the preparation method of the high-strength high-toughness starch-based pH-responsive intelligent indicating film, in the step (1), the ratio of starch to polyvinyl alcohol is 4; the glycerol is used as a plasticizer, so that the plasticizer has a good plasticizing effect, and the material has relatively good comprehensive performance.
In the step (2), the content of the cellulose nanocrystals is 6% of the sum of the mass of the starch and the mass of the polyvinyl alcohol, so that the preparation method of the high-strength and high-toughness starch-based pH-responsive intelligent indicating film is beneficial to improving the physical property of the indicating film and accelerating the degradation speed of the indicating film.
In the preparation method of the high-strength and high-toughness starch-based pH-responsive intelligent indicator film, in the step (3), the content of the purple cabbage pigment is 5% of the total mass of the starch and the polyvinyl alcohol.
In the preparation method of the high-strength and high-toughness starch-based pH-responsive intelligent indicating film, in the step (4), the oven temperature is 50 ℃, and the drying time is 24 hours.
The high-strength and high-toughness starch-based pH-responsive intelligent indicating film prepared by the preparation method is disclosed.
According to the high-strength high-toughness starch-based pH-responsive intelligent indicating film prepared by the preparation method, when the pH value is 3, the color of the indicating film material is dark pink; when the pH value is 5, the color of the indicating film material gradually changes to light red; when the pH value is 7, the color of the indicating film material is blue purple; when the pH value is 9-11, the color of the indicating film material gradually changes into green; at pH 13, the indicator film appeared pale yellow.
The high-strength and high-toughness starch-based pH-responsive intelligent indicating film prepared by the preparation method does not mildew or spot within 100 days under the environment with the relative humidity of 50%.
According to the high-strength high-toughness starch-based pH-responsive intelligent indicating film prepared by the preparation method, when the content of the purple cabbage pigment is 3-7% of the sum of the mass of the starch and the mass of the polyvinyl alcohol, the tensile strength is 142-156 MPa, and the elongation at break is 7.57-10.27%; when the CNC content of the cellulose nanocrystals is 4-6% of the mass sum of the starch and the polyvinyl alcohol, the tensile strength is 112-148 Mpa, and the elongation at break is 10.25-16.75%.
The high-strength and high-toughness starch-based pH-responsive intelligent indicating film is used for indicating the freshness of meat products, and indicating that meat begins to deteriorate when the color of the indicating film is changed into purple.
The mechanism of the purple cabbage pigment as the indicator is that in the putrefaction process of meat, protein decomposition can generate a large amount of volatile organic amines such as trimethylamine and the like to cause the increase of the pH value in a packaging space, and the anthocyanin is a non-toxic and harmless natural pigment and can present different colors along with the change of the pH value. The purple cabbage is a herb, and is composed of a plurality of anthocyanins, wherein the main components of the anthocyanins are high in pelargonidin pigment content, contain flavonoids, and can be used as a color developing agent for meat freshness.
The invention has the beneficial effects that: compared with anthocyanin from grape skins and the like, the purple cabbage pigment with high content of acylated anthocyanin is more stable than anthocyanin from grape skins; the polyvinyl alcohol is added, so that the toughness of the indicating film can be improved; the strength and the antibacterial property of the film can be improved by adding the Cellulose Nanocrystalline (CNC), the problem that the common starch film is easy to mildew is solved, and the degradation speed of the film can be improved; meanwhile, the preparation method is simpler, has no special requirements on equipment, can greatly reduce the cost of the indicating membrane, and is convenient for large-scale popularization and use; the purple cabbage pigment, the starch, the polyvinyl alcohol and the cellulose nanocrystalline are used together, compatibility among different components of the film is improved, and further flatness of the film is improved.
Drawings
FIG. 1 is a graph showing the color change response results of a high-strength and high-toughness starch-based pH-responsive intelligent indicator film under different pH conditions.
Fig. 2 is a scanning electron microscope image of the surface of a high-strength and high-toughness starch-based pH-responsive smart indicator film according to the present invention.
FIG. 3 is a graph showing the results of biodegradability of a high-strength and high-toughness starch-based pH-responsive smart indicator film according to the present invention.
FIG. 4 is a graph of the mechanical property test results of high-strength and high-toughness starch-based pH-responsive intelligent indicator films prepared by using different purple cabbage pigment addition ratios.
Fig. 5 is a graph of mechanical property test results of high-strength and high-toughness starch-based pH-responsive smart indicator films prepared at different CNC addition ratios.
FIG. 6 is a graph showing the results of stability analysis of a high-strength and high-toughness starch-based pH-responsive smart indicator film according to the present invention.
Detailed Description
In the PSCA indicator film of the present invention, P: PVA; s: starch; c: cellulose nanocrystals; a: purple cabbage pigment.
Example 1
A preparation method of a high-strength and high-toughness starch-based pH-responsive intelligent indicating film comprises the following steps:
(1) Putting starch and polyvinyl alcohol into a heating container according to a certain mass ratio, specifically, the ratio of the starch to the polyvinyl alcohol is 4.
(2) Heating and stirring in a water bath kettle at 95 ℃, gelatinizing for 1h, and then adding a certain amount of CNC (computerized numerical control), wherein the mass fraction of the cellulose nanocrystal is 6% of the sum of the mass of the starch and the mass of the polyvinyl alcohol. And continuously heating and stirring until the solution is semitransparent, and stopping heating to obtain a mixed solution A.
(3) And after cooling to room temperature, adding a certain amount of purple cabbage pigment into the mixed solution, wherein the mass fraction of the purple cabbage pigment is 5% of the sum of the mass of the starch and the mass of the polyvinyl alcohol. And ultrasonic vibration dispersing is carried out by an ultrasonic cleaning machine to obtain a mixed solution B.
(4) And pouring 25mL of the mixed solution B into a plastic culture dish to form a film, drying in a constant-temperature drying oven, removing the film, and storing for later use. In this embodiment, the inventor dried the solvent in an oven at 50 ℃, for 24 hours, and for 30min. In order to specify the size and shape of the membrane, the plastic petri dish was square with a side length of 13cm in this example.
Example 2
A preparation method of a high-strength and high-toughness starch-based pH-responsive intelligent indicating film comprises the following steps:
(1) Putting starch and polyvinyl alcohol into a beaker according to a certain mass ratio, specifically, the ratio of the starch to the polyvinyl alcohol is 2.
(2) Heating and stirring in a water bath kettle at 95 ℃, gelatinizing for 1h, and then adding a certain amount of CNC (computerized numerical control), wherein the mass fraction of the cellulose nanocrystal is 4% of the sum of the mass of the starch and the mass of the polyvinyl alcohol. And continuously heating and stirring until the solution is semitransparent, and stopping heating to obtain a mixed solution A.
(3) And after cooling to room temperature, adding a certain amount of purple cabbage pigment (the adding amount is the mass ratio of starch to polyvinyl alcohol), wherein the mass fraction of the purple cabbage pigment is 3% of the sum of the mass of the starch and the polyvinyl alcohol. And ultrasonic vibration dispersing is carried out by an ultrasonic cleaning machine to obtain a mixed solution B.
(4) And pouring 25mL of the mixed solution B into a plastic culture dish to form a film, drying in a constant-temperature drying oven, removing the film, and storing for later use. In this embodiment, the inventor dried the solvent in an oven at 50 ℃, for 24 hours, and for 30min. In this example, the plastic petri dish was square with a side length of 13cm, in order to specify the size and shape of the membrane.
Example 3
A preparation method of a high-strength and high-toughness starch-based pH-responsive intelligent indicating film comprises the following steps:
(1) Putting starch and polyvinyl alcohol into a beaker according to a certain mass ratio, specifically, the ratio of the starch to the polyvinyl alcohol is 3.
(2) Heating and stirring in a water bath kettle at 95 ℃, gelatinizing for 1h, and then adding a certain amount of CNC (computerized numerical control), wherein the mass fraction of the cellulose nanocrystal is 5% of the sum of the mass of the starch and the mass of the polyvinyl alcohol. And continuously heating and stirring until the solution is semitransparent, and stopping heating to obtain a mixed solution A.
(3) And after cooling to room temperature, adding a certain amount of purple cabbage pigment (the adding amount is the mass ratio of starch to polyvinyl alcohol), wherein the mass fraction of the purple cabbage pigment is 7% of the sum of the mass of the starch and the polyvinyl alcohol. And ultrasonic vibration dispersing is carried out by an ultrasonic cleaning machine to obtain a mixed solution B.
(4) And pouring 25mL of the mixed solution B into a plastic culture dish to form a film, drying in a constant-temperature drying oven, removing the film, and storing for later use. In this embodiment, the inventor dries the solvent by using an oven, the temperature of the oven is set to 50 ℃, the drying time is set to 24h, and the ultrasonic time is set to 30min. In this example, the plastic petri dish was square with a side length of 13cm, in order to specify the size and shape of the membrane.
Example 4
(1) pH value responsiveness analysis of PSCA indicating membrane
The PSCA indicating film prepared in example 1 was cut into a size of 1cm × 3cm, soaked in pH buffer solutions of pH 3, pH 5, pH 7, pH 9, pH 11 and pH 13 for 1min, and recorded by photographing, and the result is shown in FIG. 1. As can be seen from fig. 1, the indicating membrane material exhibits different colors at different pH values, which illustrates the good response characteristics of the indicating membrane material to pH values. When the pH value is 3, the color of the indicating film material is dark pink; when the pH value is 5, the color of the indicating film material gradually changes into light red; when the pH value is 7, the color of the indicating film material is blue purple; when the pH value is 9-11, the color of the indicating film material gradually changes into green; at pH 13, the indicator film appeared light yellow, indicating meat deterioration when the indicator film turned purple or green, and meat could no longer be consumed when the indicator film turned light yellow.
(2) Performance testing of PSCA indicator films and comparative films
According to the preparation method of the embodiment 1, the polyvinyl alcohol and the starch are respectively added under the same other conditions; polyvinyl alcohol, starch, purple cabbage pigment; polyvinyl alcohol, starch, cellulose nanocrystals; polyvinyl alcohol, starch, cellulose nanocrystal and purple cabbage pigment; four films of PS, PSA, PSC and PSCA are respectively prepared, and the prepared sample film is cut as required.
1. SEM scanning Electron microscopy analysis of sample films
Observing the microstructure of the cut sample film by adopting a scanning electron microscope and taking a picture, wherein the method specifically comprises the following steps: after drying the sample film of 1cm × 1cm, the surface was treated by spraying gold at an accelerating voltage of 2KV and a magnification of 10K, and the results are shown in fig. 2. SEM images mainly reflect the interfacial morphology and microstructure of the composite system, generally speaking, if the chemical compatibility between substances is high, the surface is relatively flat, whereas relatively coarse small particulate substances are present. As can be seen from FIG. 2, the PSCA indicating film surface is more smooth, which shows that the purple cabbage pigment has a certain effect of improving the compatibility among starch, polyvinyl alcohol and cellulose nanocrystals.
2. Determination and analysis of biodegradability of sample film
Cutting the four sample films into about 5cm multiplied by 5cm, drying in a constant temperature drying oven to constant weight, and burying in soil respectively. Taking out every 3d, removing dust, drying and weighing, and calculating the weight loss rate W% according to the formula (1) to represent the biodegradation performance of the material:
W％＝(W 0 -W 1 )/W 0 × 100％ (1)
in the formula, W 0 Mass of sample before degradation, unit g; w 1 The mass of the degraded sample is given in g.
The weight loss data for the four types of sample films at 7day and 27day are shown in table 1, while PSCA indicates that the films were taken as shown in fig. 3 at day 1, 7, 17 and 27. With increasing days of soil burial, this indicates a higher and higher degree of membrane degradation, which is almost 2/3 of the degradation on day 27.
(3) Mechanical property analysis of PSCA indicating film
1. Influence of purple cabbage pigment content on indicating membrane mechanical property
According to the preparation method of the example 1, the purple cabbage pigment with the mass fractions of 0%, 3%, 5%, 7% and 9% is added respectively under the same conditions to prepare PSCA indicating films with different purple cabbage pigment contents. The tensile mechanical properties of the indicating film, namely Tensile Strength (TS) and elongation at break (EB), were measured using a computer tensile tester. The test sample size is 130mm multiplied by 15mm, the nominal distance is 90mm, the stretching speed is 300mm/min, the test method is referred to national standard GB/T1040.3-2006, and the test result is shown in figure 4 and table 2.
Tensile strength TS: from the results, it can be seen that when the content of the purple cabbage pigment is 0 to 7%, the tensile strength is gradually increased as the amount of the purple cabbage pigment added is increased, and when the amount of the purple cabbage pigment added is more than 7%, defects such as micropores are increased on the surface of the film due to the precipitation of a part of small molecules of the pigment, and the tensile strength is rapidly decreased. The significant change in TS is likely related to the crystalline formation of the film and the interatomic forces.
Elongation at break EB: for the elongation at break, when the amount of purple cabbage pigment added is not more than 7%, EB increases as the amount of pigment added increases. The number of EBs increased significantly, possibly due to the reduced intermolecular forces with the film-forming substrate by the purple cabbage pigment, and the number of mobile polymer chains increased. As the amount of the dye added continued to increase, EB slightly decreased.
2. Influence of cellulose nanocrystalline CNC content on mechanical performance of indicating film
According to the preparation method of the example 1, the cellulose nanocrystalline CNC with the mass fractions of 0%, 2%, 4%, 6% and 8% is added respectively without changing other conditions, so as to prepare PSCA indicating films with different CNC contents. The tensile mechanical properties of the indicating film, namely Tensile Strength (TS) and elongation at break (EB), were measured using a computer tensile tester. The test sample size is 130mm multiplied by 15mm, the nominal distance is 90mm, the stretching speed is 300mm/min, the test method refers to the national standard GB/T1040.3-2006, and the test results are shown in figure 5 and table 3.
Tensile strength TS: as can be seen from the figure, when the CNC content is 0 to 6%, the tensile strength of the film is indicated to increase slowly with increasing CNC content, and the tensile strength is greatly increased when the CNC content is 6%. The reason is that the CNC surface has high hydroxyl number content, and a rigid network structure is formed through interaction with starch molecules, so that the strength of the material is improved. When the CNC is added in an amount of 6 to 8%, the tensile strength of the indicating film material is significantly reduced as the CNC content is increased, generally because when the CNC is excessively dosed, the CNC is unevenly distributed in the starch matrix and is more prone to agglomeration, so that the tensile strength of the indicating film material is significantly reduced.
Elongation at break EB: it can be seen from the figure that when the CNC content is 0-6% of the sum of the mass of the starch and the polyvinyl alcohol, the elongation at break of the film is indicated to increase slowly as the CNC content increases, and the elongation at break is greatly increased when the CNC content is 6%. When the addition amount of the CNC is 6-8% of the sum of the mass of the starch and the mass of the polyvinyl alcohol, the elongation at break of the indicating film material is obviously reduced along with the increase of the content of the CNC.
In conclusion, in the experiment, when the content of the purple cabbage pigment is 5% of the sum of the mass of the starch and the mass of the polyvinyl alcohol, and when the content of the CNC is 6%, the material shows the mechanical properties of high strength and high toughness.
(4) Measurement and analysis of PSCA indicator film stability
In order to examine the stability of the PSCA indicator film, the indicator film prepared in example 1 was placed in a desiccator having a relative humidity of 50%, and after the 50 th and 100 th days, the film was taken out and observed, and the physical pattern thereof is shown in fig. 6, indicating that no mold, spots, or the like was present on the surface of the indicator film.
The invention discloses a preparation method of a high-strength high-toughness starch-based pH-responsive intelligent indicating film. The visual intelligent indicating film prepared from the purple cabbage pigment is sensitive to pH value change in the environment, can accurately feed back freshness information of meat products, is expected to be applied to real-time freshness monitoring of the meat products, and has high-strength and high-toughness mechanical properties, degradability, no toxicity, no harm and wide application prospect compared with a single-material starch-based film.
The above description is intended to be illustrative of the present invention and should not be taken as limiting the invention, as the invention is intended to cover various modifications, equivalents, improvements, and equivalents, which may be made within the spirit and scope of the present invention.
TABLE 1 weight loss ratio of sample films
TABLE 2 influence of purple cabbage pigment content on the mechanical properties of the indicator membrane
| Purple cabbage pigment content (%) | Tensile strength (Mpa) | Elongation at Break (%) |
| 0 | 96 | 6.19 |
| 3 | 142 | 7.57 |
| 5 | 152 | 10.55 |
| 7 | 156 | 10.27 |
| 9 | 96 | 10.19 |
TABLE 3 influence of CNC content of cellulose nanocrystals on the mechanical properties of the indicated films
| CNC content (%) | Tensile strength (Mpa) | Elongation at Break (%) |
| 0 | 105 | 9.14 |
| 2 | 109 | 9.19 |
| 4 | 112 | 10.25 |
| 6 | 148 | 16.75 |
| 8 | 37 | 11.27 |
Claims (10)
1. A preparation method of a high-strength high-toughness starch-based pH-responsive intelligent indicating film is characterized by comprising the following steps: the method comprises the following steps:
(1) Putting starch and polyvinyl alcohol (PVA) into a heating container, adding glycerol, pouring distilled water, and mixing uniformly to prepare a starch-polyvinyl alcohol solution;
(2) Gelatinizing in a water bath, adding a cellulose nanocrystalline CNC, continuously heating and stirring until the solution is semitransparent, and stopping heating to obtain a mixed solution A;
(3) After cooling to room temperature, adding purple cabbage pigment into the mixed solution A, and performing ultrasonic dispersion by using an ultrasonic cleaner to obtain a mixed solution B;
(4) Pouring the mixed solution B into a flat-bottomed container to form a film, drying the film in a constant-temperature drying oven, and then uncovering the film to store for later use.
2. The preparation method of the high-strength high-toughness starch-based pH-responsive intelligent indicator film according to claim 1, wherein the preparation method comprises the following steps:
in the step (1), starch and polyvinyl alcohol are placed in a heating container, glycerol accounting for 15-25% of the mass sum of the starch and the polyvinyl alcohol is added, distilled water is poured and mixed uniformly, the volume is constant, and a starch-polyvinyl alcohol solution with the mass fraction of 7-13% is prepared, wherein the mass ratio of the starch to the polyvinyl alcohol is 2-4;
in the step (2), CNC with the mass sum of 4-6% of the starch and the polyvinyl alcohol is added;
in the step (3), after cooling to room temperature, adding purple cabbage pigment accounting for 3-7% of the mass sum of the starch and the polyvinyl alcohol into the mixed solution A, and performing ultrasonic dispersion by using an ultrasonic cleaning machine to obtain a mixed solution B.
3. The preparation method of the high-strength and high-toughness starch-based pH-responsive intelligent indicator film according to claim 2, wherein the preparation method comprises the following steps: in the step (1), the glycerol accounts for 20% of the total mass of the starch and the polyvinyl alcohol, and after the volume is fixed, the mass fraction of the starch-polyvinyl alcohol in the starch-polyvinyl alcohol solution is 10%.
4. The preparation method of the high-strength and high-toughness starch-based pH-responsive intelligent indicator film according to claim 2, wherein the preparation method comprises the following steps: in the step (2), the mixture is gelatinized for 1 hour in a water bath kettle at the temperature of 95 ℃, and then cellulose nanocrystals with the mass sum of 6 percent of the starch and the polyvinyl alcohol are added.
5. The preparation method of the high-strength high-toughness starch-based pH-responsive intelligent indicator film according to claim 2, wherein the preparation method comprises the following steps: in the step (3), purple cabbage pigment accounting for 5% of the total mass of the starch and the polyvinyl alcohol is added into the mixed solution A after the mixed solution A is cooled to room temperature.
6. The preparation method of the high-strength and high-toughness starch-based pH-responsive intelligent indicator film according to claim 1, wherein the preparation method comprises the following steps: in the step (1), the mass ratio of the starch to the polyvinyl alcohol is 4.
7. The preparation method of the high-strength and high-toughness starch-based pH-responsive intelligent indicator film according to claim 1, wherein the preparation method comprises the following steps: the starch is soluble starch, the PVA specification is 1788 type, and the solubility is 88%.
8. The preparation method of the high-strength and high-toughness starch-based pH-responsive intelligent indicator film according to claim 1, wherein the preparation method comprises the following steps: in the step (4), the oven temperature is 50 ℃ and the drying time is 24h.
9. The high-strength high-toughness starch-based pH-responsive intelligent indicator film prepared by the preparation method according to any one of claims 1 to 8, wherein when the pH value is 3, the color of the indicator film material is dark pink; when the pH value is 5, the color of the indicating film material gradually changes into light red; when the pH value is 7, the color of the indicating film material is blue purple; when the pH value is 9-11, the color of the indicating film material gradually changes into green; at pH 13, the indicator film appeared light yellow.
10. The high-strength high-toughness starch-based pH-responsive smart indicator film according to claim 9, wherein the change of the color of the indicator film from red to purple indicates the deterioration of meat.
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