CN112649426B - Preparation method and application of 3D printing freshness monitoring and freshness keeping integrated label - Google Patents
Preparation method and application of 3D printing freshness monitoring and freshness keeping integrated label Download PDFInfo
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- 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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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/153—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of liquids or solids
- A23B7/154—Organic compounds; Microorganisms; Enzymes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
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- B33Y10/00—Processes of additive manufacturing
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- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
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Abstract
The invention discloses a preparation method and application of a 3D printing freshness monitoring and freshness keeping integrated label. The method comprises the following steps: adding sodium alginate, carrageenan and anthocyanin into the nano-cellulose solution, and uniformly mixing to obtain 3D printing ink; dissolving chitosan in a lactic acid solution, adding 1-methylcyclopropene powder, and mixing uniformly to obtain a mixed solution; the 3D printing ink is used as an outer layer material, the mixed liquid is used as an inner layer material, coaxial 3D printing is carried out, a printing material is obtained, and the 3D printing label is obtained after solidification and freeze-drying. The label realizes real-time monitoring of fruit freshness through the pH response color change function of anthocyanin, and the 3D prints the slow release of 1-methylcyclopropene of the hollow shell core fiber structure that constructs, realizes long-acting freshness preservation, solves the problem that the existing intelligent food package can not realize both freshness monitoring and food freshness preservation functions simultaneously, and then makes up the defects that the existing fruit package function is single and can not meet the actual application requirements.
Description
Technical Field
The invention belongs to the field of intelligent food packaging, and particularly relates to a preparation method and application of a 3D printing freshness monitoring and freshness keeping integrated label.
Background
Recently, the requirements of consumers for food safety and quality are increasing, and research on intelligent food packaging is receiving attention to ensure the safety and quality of food. Conventional food quality detection methods fail to provide real-time information about freshness and food quality and are destructive. Besides, many specialized instruments and equipment are required for detection. Therefore, there is a great market demand for developing intelligent packaging systems for food monitoring. The intelligent packaging system can provide real-time quantitative or qualitative information to the consumer regarding environmental conditions and the quality of packaged food products at various points in the supply chain. Especially, natural pH response visual monitoring materials based on anthocyanin are favored because of the advantages of no damage, nature, no toxicity and the like. Zhang et al prepared pH responsive smart films using Hibiscus anthocyanosides for visual monitoring of pork freshness (Zhang, J.; zou, X.; zhai, X.; huang, X.; jiang, C.; holmes, M., preparation of an animal pH film based on bioirregular polymers and roselle anticyclines for monitoring of meat freshness. Food Chem 2019,272, 306-312.). However, the existing food freshness monitoring material based on anthocyanin does not have the functions of keeping freshness and prolonging the shelf life of food. For the fresh food which is not stored endurably, the simple freshness monitoring can not meet the actual application requirement, so that the intelligent food packaging label integrating the freshness monitoring of the collected fruits and the fresh-keeping function is urgently needed to be developed.
Coaxial 3D printing technology enables the precise design and construction of core-shell fiber structures. Therefore, inner and outer layer function partitioning of the material is realized by coaxial 3D printing, so that the freshness monitoring accuracy is guaranteed while the preservation function is realized, and mutual interference caused by simple blending of anthocyanin and ethylene receptor inhibitor 1-methylcyclopropene is prevented. In addition, 1-methylcyclopropene is volatile and unstable, and the shell-core fiber with the hollow micro-pipeline obtained by 3D printing has a certain encapsulation effect on 1-methylcyclopropene, so that the 1-methylcyclopropene is slowly released for a long time to realize long-acting preservation.
The nanocellulose is a natural polysaccharide, has excellent shear thinning performance, is suitable for serving as a substrate of 3D printing ink, but the viscoelasticity of pure nanocellulose is insufficient to meet the 3D printing requirement.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a 3D printing nanocellulose-based fruit freshness monitoring and fresh-keeping integrated label and a preparation method and application thereof.
The 3D printing nanocellulose-based fruit freshness monitoring and fresh-keeping integrated label provided by the invention is non-toxic, can monitor fruit freshness by generating color change response to the pH of the environment in a package, and can release 1-methylcyclopropene to delay the decay of fruits and prolong the shelf life of the fruits.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a 3D printing nanocellulose-based fruit freshness monitoring and fresh-keeping integrated label and a preparation method and application thereof. The 3D printing nanocellulose-based fruit freshness monitoring and fresh keeping integrated label is prepared by a coaxial 3D printing technology, the outer layer of the label adopts nanocellulose as a matrix, sodium alginate and carrageenan as rheological reinforcing agents, anthocyanin is a pH response color changing functional component, and the inner layer of the label is a mixed solution of chitosan and 1-methylcyclopropene. The material takes nanocellulose as a matrix, the dual functions of fruit freshness monitoring and fresh keeping are integrated by compounding natural dye anthocyanin and ethylene receptor inhibitor 1-methylcyclopropene, one-step batch construction is realized by using a coaxial 3D printing technology, and meanwhile, the slow and continuous release of the 1-methylcyclopropene is realized by a unique hollow shell core fiber structure formed by coaxial 3D printing through a physical limiting effect. The problem that the existing food freshness monitoring material is single in function and cannot meet the requirements of practical application is solved.
The invention provides a preparation method of a 3D printing nanocellulose-based fruit freshness monitoring and freshness retaining integrated label (namely, the 3D printing freshness monitoring and freshness retaining integrated label), which comprises the following steps:
(1) Adding sodium alginate and carrageenan into the nano-cellulose solution under the stirring condition, and uniformly mixing to obtain a mixed system (the mixed system of the sodium alginate, the carrageenan and the nano-cellulose);
(2) Adding anthocyanin into the mixed system in the step (1) under the condition of stirring, uniformly mixing, filling into a printing container, and carrying out centrifugal treatment to eliminate bubbles to obtain mixed printing ink (mixed printing ink of nano-cellulose, sodium alginate, carrageenan and anthocyanin);
(3) Adding chitosan into pure water at room temperature, mixing uniformly to obtain a chitosan solution, then adding lactic acid (fully dissolving chitosan in water), and mixing uniformly to obtain a chitosan-lactic acid solution;
(4) Adding 1-methylcyclopropene powder into the chitosan lactic acid solution obtained in the step (3) under the condition of stirring, and uniformly mixing to obtain a chitosan/1-methylcyclopropene mixed solution;
(5) Taking the mixed printing ink in the step (2) as an outer-layer printing material, taking the chitosan/1-methylcyclopropene mixed solution in the step (4) as an inner-layer printing material, and performing coaxial 3D printing to obtain a 3D printing product (wet 3D printing nanocellulose-based fruit freshness monitoring and freshness keeping integrated label);
(6) Dissolving calcium chloride and potassium chloride in water, and stirring until the calcium chloride and the potassium chloride are completely dissolved to obtain a calcium chloride/potassium chloride curing agent;
(7) And (3) spraying the calcium chloride/potassium chloride curing agent in the step (6) on the surface of the 3D printing product in the step (5), curing, and freeze-drying to obtain the 3D printing nanocellulose-based fruit freshness monitoring and fresh-keeping integrated label.
Further, the concentration of the nano-cellulose solution in the step (1) is 0.03-0.10g/mL; the mass ratio of the sodium alginate to the carrageenan is 1.2-1; the mass ratio of the total mass of the sodium alginate and the carrageenan to the mass of the nano-cellulose solution is (1-1).
Preferably, the sodium alginate is sodium alginate dry powder, and the purity level of the sodium alginate is analytically pure.
Preferably, the carrageenan is carrageenan dry powder, and the purity grade of the carrageenan is analytical purity.
Further, the mass ratio of the anthocyanin to the mixed system in the step (2) is 1; the speed of the centrifugal treatment is 2000-8000rpm, and the time of the centrifugal treatment is 1-10min.
Further, the concentration of the chitosan solution in the step (3) is 1-10g/L; the volume of the lactic acid is 0.5-2.0% (volume fraction) of the volume of the chitosan solution.
Further, in the step (4), the mass ratio of the 1-methylcyclopropene to the chitosan lactic acid solution is 1.
Further, the printing pressure of the coaxial 3D printing in the step (5) is 0.1-0.5MPa; the printing speed of the outer layer is 1-10mm/s; the inner layer printing speed is 1-5mL/h.
Further, the mass ratio of the calcium chloride to the potassium chloride in the step (6) is 1; in the calcium chloride/potassium chloride curing agent, the concentrations of calcium chloride and potassium chloride are both 0.01-0.10g/mL.
Further, the mass-to-volume ratio of the 3D printed product (wet weight) to the calcium chloride/potassium chloride solution in the step (7) is 0.5-1.5g/mL; the time of the curing treatment is 5-50s.
Further, the 3D printed product obtained in the step (5) does not need to be dried, and the calcium chloride/potassium chloride solution is directly and uniformly sprayed on the 3D printed product in the step (6) to carry out curing treatment.
The invention provides a 3D printing nanocellulose-based fruit freshness monitoring and freshness keeping integrated label prepared by the preparation method.
The invention provides application of a 3D printing nanocellulose-based fruit freshness monitoring and freshness keeping integrated label in fruit freshness monitoring and freshness keeping.
The 3D printing nanocellulose-based fruit freshness monitoring and freshness retaining integrated label provided by the invention has sensitive fruit freshness monitoring capability and can be used for remarkably prolonging the shelf life of fruits. The 3D printed nanocellulose-based fruit freshness monitoring and fresh-keeping integrated label provided by the invention can indicate the fruit spoilage process in real time through color change, and can remarkably prolong the shelf life of kiwi fruits at 25 ℃ and 75% humidity.
The 3D printed nanocellulose-based fruit freshness monitoring and freshness retaining integrated label provided by the invention can be applied to fruit intelligent packaging.
The 3D printing nanocellulose-based fruit freshness monitoring and freshness retaining integrated label (namely, the 3D printing freshness monitoring and freshness retaining integrated label) prepared by the preparation method has good fruit freshness monitoring sensitivity and freshness retaining effect.
The invention realizes the subarea integration of the double functions of fruit freshness monitoring and fresh keeping by utilizing a coaxial 3D printing technology, constructs the double-function integrated food intelligent packaging label in one step, prepares a natural, non-toxic and degradable fruit freshness monitoring and fresh keeping integrated label, and has the potential of mass large-scale production. The invention makes up the problem that the existing food freshness monitoring material has single function and cannot meet the requirement of practical application, and expands the application of the 3D printing technology in the field of food intelligent packaging.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The preparation method provided by the invention comprises the following raw materials: the nano-cellulose, the sodium alginate, the carrageenan, the anthocyanin and the chitosan have the advantages of safety, no toxicity, environmental friendliness and wide sources; no toxic and harmful substances are generated in the preparation process, and the preparation method is green and environment-friendly;
(2) According to the preparation method provided by the invention, the shell-core fiber with the hollow structure is designed and constructed by utilizing the coaxial 3D printing technology, so that mutual interference caused by simple blending of anthocyanin and 1-methylcyclopropene is avoided; the method realizes the partition integration of the double functions of fruit freshness monitoring and fruit fresh keeping and the one-step construction of the dual-function integrated food intelligent packaging label; the preparation method has the advantages of simple preparation process, batch production, applicability to large-scale industrial production and technical mobility;
(3) The encapsulation effect of the core-shell fiber structure on the 1-methylcyclopropene solves the problem that the 1-methylcyclopropene is volatile and unstable, and realizes the long-acting fresh-keeping function;
(4) The 3D printed nanocellulose-based fruit freshness monitoring and freshness keeping label provided by the invention not only has a sensitive fruit freshness monitoring function, but also has an excellent fruit freshness keeping function, and the problems that the intelligent fruit packaging function is single and the actual application requirements cannot be met are solved.
Drawings
Fig. 1 is a fiber cross-sectional electron microscope image of the 3D printed nanocellulose-based fruit freshness monitoring and freshness retaining integrated label obtained in embodiment 3.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically detailed, are all those that can be realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
A preparation method of a 3D printing nanocellulose-based fruit freshness monitoring and freshness keeping integrated label comprises the following steps:
(1) Under the condition of room temperature, adding 0.5g of sodium alginate powder and 0.1g of carrageenan powder into 6g of nano-cellulose solution with the concentration of 0.03g/mL, and uniformly mixing to obtain a mixed system of nano-cellulose, sodium alginate and carrageenan;
(2) Adding 12mg of anthocyanin into a mixed system of nano-cellulose, sodium alginate and carrageenan at room temperature, uniformly mixing, then filling into a 3D printing needle cylinder, carrying out centrifugal treatment to eliminate bubbles, wherein the speed of the centrifugal treatment is 2000rpm, and the time of the centrifugal treatment is 1min to obtain mixed printing ink;
(3) Adding 0.01g of chitosan into 10mL of pure water, stirring uniformly to uniformly disperse the chitosan in the water, then adding 0.05mL of lactic acid, mixing uniformly to completely dissolve the chitosan to obtain a chitosan-lactic acid solution;
(4) Adding 5.0g of 1-methylcyclopropene powder into the chitosan lactic acid solution in the step (3), and uniformly mixing to obtain a chitosan/1-methylcyclopropene mixed solution;
(5) Taking the mixed printing ink in the step (2) as an outer layer material, taking the chitosan/1-methylcyclopropene mixed solution in the step (4) as an inner layer material, and carrying out coaxial 3D printing, wherein the pressure of the coaxial 3D printing is 0.1MPa, the printing speed of the inner layer is 1mL/h, and the printing speed of the outer layer is 1mm/s, so as to obtain a 3D printing product;
(6) Mixing 1.0g of calcium chloride and 0.2g of potassium chloride, adding 100mL of pure water, stirring and dissolving to obtain a calcium chloride/potassium chloride mixed solution;
(7) Uniformly spraying the calcium chloride/potassium chloride mixed solution obtained in the step (6) on the surface of the 3D printing product obtained in the step (5), wherein the mass-to-volume ratio of the 3D printing product (wet weight) to the calcium chloride/potassium chloride mixed solution is 0.5g/mL, carrying out curing treatment for 50s, and then carrying out freeze drying to obtain the 3D printing nanocellulose-based integrated label for monitoring and preserving the freshness of the fruits.
The 3D printing nanocellulose based fruit freshness monitoring and fresh keeping integrated label prepared in the embodiment 1 has the characteristics of high form fidelity, good formability and clear printing structure, 3D printing fibers in the label after freeze-drying still keep a good hollow pipeline structure, and the cross section of the fibers is regular in shape, and can be seen in fig. 1.
The 3D printed nanocellulose-based fruit freshness monitoring and freshness retaining integrated label prepared in example 1 showed significant, perceptible color changes in different pH environments. The material has sensitive and visible pH response performance. The 3D printing nanocellulose-based fruit freshness monitoring and preservation integrated label prepared by the method can indicate the fruit spoilage process in real time through color change, has a food preservation function, and can be shown in table 1.
Example 2
A preparation method of a 3D printing nanocellulose-based fruit freshness monitoring and freshness keeping integrated label comprises the following steps:
(1) Under the condition of room temperature, adding 0.3g of sodium alginate powder and 0.1g of carrageenan powder into 8g of nano-cellulose solution with the concentration of 0.04g/mL, and uniformly mixing to obtain a mixed system of nano-cellulose, sodium alginate and carrageenan;
(2) Adding 5mg of anthocyanin into a mixed system of nano-cellulose, sodium alginate and carrageenan at room temperature, uniformly mixing, then filling into a 3D printing needle cylinder, carrying out centrifugal treatment to eliminate bubbles, wherein the speed of the centrifugal treatment is 3000rpm, and the time of the centrifugal treatment is 3min to obtain mixed printing ink;
(3) Adding 0.03g of chitosan into 10mL of pure water, uniformly stirring to uniformly disperse the chitosan in the water, then adding 0.07mL of lactic acid, uniformly mixing to completely dissolve the chitosan to obtain a chitosan lactic acid solution;
(4) Adding 3.0g of 1-methylcyclopropene powder into the chitosan lactic acid solution in the step (3), and uniformly mixing to obtain a chitosan/1-methylcyclopropene mixed solution;
(5) Taking the mixed printing ink in the step (2) as an outer layer material, taking the chitosan/1-methylcyclopropene mixed solution in the step (4) as an inner layer material, and carrying out coaxial 3D printing, wherein the pressure of the coaxial 3D printing is 0.2MPa, the printing speed of the inner layer is 2mL/h, and the printing speed of the outer layer is 3mm/s, so as to obtain a 3D printing product;
(6) Mixing 2.0g of calcium chloride and 1.0g of potassium chloride, adding 100mL of pure water, stirring and dissolving to obtain a calcium chloride/potassium chloride mixed solution;
(7) Uniformly spraying the calcium chloride/potassium chloride mixed solution obtained in the step (6) on the surface of the 3D printing product obtained in the step (5), wherein the mass-to-volume ratio of the 3D printing product (wet weight) to the calcium chloride solution is 0.7g/mL, carrying out curing treatment for 30s, and then carrying out freeze drying to obtain the 3D printing nano cellulose-based fruit freshness monitoring and freshness keeping integrated label.
The 3D printing nanocellulose based fruit freshness monitoring and fresh-keeping integration label of embodiment 2 preparation has the form fidelity height, and the formability is good, prints the clear characteristics of structure, and 3D prints the fibre in the freeze-drying back label and still keeps good hollow pipeline structure, and fibre cross sectional shape is regular, can refer to and show in fig. 1.
The 3D printed nanocellulose-based fruit freshness monitoring and freshness-retaining integrated label prepared in example 2 exhibited a noticeable, perceptible color change in different pH environments. The material has sensitive and visible pH response performance. The 3D printed nanocellulose-based fruit freshness monitoring and fresh-keeping integrated label prepared by the method can indicate the fruit spoilage process in real time through color change, has a food fresh-keeping function, and can be shown in Table 1.
Example 3
A preparation method of a 3D printed nanocellulose-based fruit freshness monitoring and freshness keeping integrated label comprises the following steps:
(1) Under the condition of room temperature, adding 0.2g of sodium alginate powder and 0.2g of carrageenan powder into 20g of nano-cellulose solution with the concentration of 0.05g/mL, and uniformly mixing to obtain a mixed system of nano-cellulose, sodium alginate and carrageenan;
(2) Adding 10mg of anthocyanin into a mixed system of nano-cellulose, sodium alginate and carrageenan at room temperature, uniformly mixing, then pouring into a 3D printing needle cylinder, and carrying out centrifugal treatment to eliminate bubbles, wherein the speed of the centrifugal treatment is 4000rpm, and the time of the centrifugal treatment is 5min to obtain mixed printing ink;
(3) Adding 0.05g of chitosan into 10mL of pure water, uniformly stirring to uniformly disperse the chitosan in the water, then adding 0.10mL of lactic acid, uniformly mixing to completely dissolve the chitosan to obtain a chitosan lactic acid solution;
(4) Adding 2.5g of 1-methylcyclopropene powder into the chitosan lactic acid solution obtained in the step (3), and uniformly mixing to obtain a chitosan/1-methylcyclopropene mixed solution;
(5) Taking the mixed printing ink in the step (2) as an outer layer material, taking the chitosan/1-methylcyclopropene mixed solution in the step (4) as an inner layer material, and carrying out coaxial 3D printing, wherein the pressure of the coaxial 3D printing is 0.3MPa, the printing speed of the inner layer is 3mL/h, and the printing speed of the outer layer is 4mm/s, so as to obtain a 3D printing product;
(6) Mixing 2.0g of calcium chloride and 2.0g of potassium chloride, adding 100mL of pure water, stirring and dissolving to obtain a calcium chloride/potassium chloride mixed solution;
(7) Uniformly spraying the calcium chloride/potassium chloride mixed solution obtained in the step (6) on the surface of the 3D printing product obtained in the step (5), wherein the mass-to-volume ratio of the 3D printing product (wet weight) to the calcium chloride solution is 1.0g/mL, carrying out curing treatment for 20s, and then carrying out freeze drying to obtain the 3D printing nano cellulose-based fruit freshness monitoring and freshness keeping integrated label.
The 3D printing nanocellulose-based fruit freshness monitoring and freshness keeping integrated label obtained by the preparation of the embodiment 3 has the characteristics of high form fidelity, good formability and clear printing structure. As shown in fig. 1, the 3D printed fibers in the label after freeze-drying still maintain a good hollow tube structure, and the cross-sectional shape of the fibers is regular.
The following table 1 is a data table of color values of the 3D printed nanocellulose-based fruit freshness monitoring and freshness retaining integrated label obtained in example 3 in solutions with different pH values. L, a, b in table 1 are actually measured color value parameters, Δ E represents the difference from the original color, and when Δ E >3.5, the color change is noticeable to the naked eye. The data in table 1 below were obtained by monitoring the ripening and spoilage processes of litchi using the 3D printed nanocellulose based fruit freshness monitoring and freshness integrated label of example 3.
As shown in table 1, the 3D printed nanocellulose-based freshness monitoring and freshness-retaining integrated label exhibited a noticeable, perceptible color change in different pH environments. The material has sensitively visualized pH response performance. The 3D printing nanocellulose-based fruit freshness monitoring and preservation integrated label prepared by the method can indicate the fruit spoilage process in real time through color change, and has a food preservation function. In practical application, the 3D printing nanocellulose-based fruit freshness monitoring and freshness keeping integrated label for intelligent fruit packaging sensitively indicates the ripening and spoilage processes of litchi through visual color change, and effectively prolongs the shelf life of the litchi by 6 days.
TABLE 1
Example 4
A preparation method of a 3D printed nanocellulose-based fruit freshness monitoring and freshness keeping integrated label comprises the following steps:
(1) Under the condition of room temperature, adding 0.1g of sodium alginate powder and 0.2g of carrageenan powder into 20g of nano-cellulose solution with the concentration of 0.07g/mL, and uniformly mixing to obtain a mixed system of nano-cellulose, sodium alginate and carrageenan;
(2) Adding 5mg of anthocyanin into a mixed system of nano-cellulose, sodium alginate and carrageenan at room temperature, uniformly mixing, then filling into a 3D printing needle cylinder, carrying out centrifugal treatment to eliminate bubbles, wherein the speed of the centrifugal treatment is 6000rpm, and the time of the centrifugal treatment is 3min to obtain mixed printing ink;
(3) Adding 0.08g of chitosan into 10mL of pure water, uniformly stirring to uniformly disperse the chitosan in the water, then adding 0.15mL of lactic acid, uniformly mixing to completely dissolve the chitosan to obtain a chitosan-lactic acid solution;
(4) Adding 1.5g of 1-methylcyclopropene powder into the chitosan lactic acid solution obtained in the step (3), and uniformly mixing to obtain a chitosan/1-methylcyclopropene mixed solution;
(5) Taking the mixed printing ink in the step (2) as an outer layer material, taking the chitosan/1-methylcyclopropene mixed solution in the step (4) as an inner layer material, and carrying out coaxial 3D printing, wherein the pressure of the coaxial 3D printing is 0.4MPa, the inner layer printing speed is 4mL/h, and the outer layer printing speed is 6mm/s, so as to obtain a 3D printing product;
(6) Mixing 1.0g of calcium chloride and 3.0g of potassium chloride, adding 100mL of pure water, stirring and dissolving to obtain a calcium chloride/potassium chloride mixed solution;
(7) Uniformly spraying the calcium chloride/potassium chloride mixed solution obtained in the step (6) on the surface of the 3D printing product obtained in the step (5), wherein the mass-to-volume ratio of the 3D printing product (wet weight) to the calcium chloride solution is 1.2g/mL, carrying out curing treatment for 10s, and then carrying out freeze drying to obtain the 3D printing nano cellulose-based fruit freshness monitoring and freshness keeping integrated label.
The 3D printing nanocellulose based fruit freshness monitoring and fresh keeping integrated label prepared in the embodiment 4 has the characteristics of high form fidelity, good formability and clear printing structure, 3D printing fibers in the label after freeze-drying still keep a good hollow pipeline structure, and the cross section of the fibers is regular in shape, and can be seen in fig. 1.
The 3D printed nanocellulose-based fruit freshness monitoring and freshness retaining integrated label prepared in example 4 showed significant, perceptible color changes in different pH environments. The material has sensitively visualized pH response performance. The 3D printed nanocellulose-based fruit freshness monitoring and fresh-keeping integrated label prepared by the method can indicate the fruit spoilage process in real time through color change, has a food fresh-keeping function, and can be shown in Table 1.
Example 5
A preparation method of a 3D printed nanocellulose-based fruit freshness monitoring and freshness keeping integrated label comprises the following steps:
(1) Under the condition of room temperature, adding 0.1g of sodium alginate powder and 0.5g of carrageenan powder into 60g of nano-cellulose solution with the concentration of 0.10g/mL, and uniformly mixing to obtain a mixed system of nano-cellulose, sodium alginate and carrageenan;
(2) Adding 12mg of anthocyanin into a mixed system of nano-cellulose, sodium alginate and carrageenan at room temperature, uniformly mixing, then pouring into a 3D printing needle cylinder, and carrying out centrifugal treatment to eliminate bubbles, wherein the speed of the centrifugal treatment is 8000rpm, and the time of the centrifugal treatment is 1min to obtain mixed printing ink;
(3) Adding 0.10g of chitosan into 10mL of pure water, uniformly stirring to uniformly disperse the chitosan in the water, then adding 0.20mL of lactic acid, uniformly mixing to completely dissolve the chitosan to obtain a chitosan-lactic acid solution;
(4) Adding 0.5g of 1-methylcyclopropene powder into the chitosan lactic acid solution in the step (3), and uniformly mixing to obtain a chitosan/1-methylcyclopropene mixed solution;
(5) Taking the mixed printing ink obtained in the step (2) as an outer layer material, taking the chitosan/1-methylcyclopropene mixed solution obtained in the step (4) as an inner layer material, and carrying out coaxial 3D printing at the pressure of 0.5MPa, the inner layer printing speed of 5mL/h and the outer layer printing speed of 10mm/s to obtain a 3D printing product;
(6) Mixing 1.0g of calcium chloride and 5.0g of potassium chloride, adding 100mL of pure water, stirring and dissolving to obtain a calcium chloride/potassium chloride mixed solution;
(7) Uniformly spraying the calcium chloride/potassium chloride mixed solution obtained in the step (6) on the surface of the 3D printing product obtained in the step (5), wherein the mass-to-volume ratio of the 3D printing product (wet weight) to the calcium chloride solution is 1.5g/mL, carrying out curing treatment for 5s, and then carrying out freeze drying to obtain the 3D printing nano cellulose-based fruit freshness monitoring and freshness keeping integrated label.
The 3D printing nanocellulose based fruit freshness monitoring and fresh-keeping integration label of embodiment 5 preparation has the form fidelity height, and the formability is good, prints the clear characteristics of structure, and 3D prints the fibre in the freeze-drying back label and still keeps good hollow pipeline structure, and fibre cross-sectional shape is regular, can refer to and show in fig. 1.
The 3D printed nanocellulose-based fruit freshness monitoring and freshness-retaining integrated label prepared in example 5 exhibited a noticeable, perceptible color change in different pH environments. The material has sensitively visualized pH response performance. The 3D printed nanocellulose-based fruit freshness monitoring and fresh-keeping integrated label prepared by the method can indicate the fruit spoilage process in real time through color change, has a food fresh-keeping function, and can be shown in Table 1.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (6)
1. A preparation method of a 3D printing freshness monitoring and freshness keeping integrated label is characterized by comprising the following steps:
(1) Adding sodium alginate and carrageenan into the nano-cellulose solution, and uniformly mixing to obtain a mixed system;
(2) Adding anthocyanin into the mixed system in the step (1), uniformly mixing, and carrying out centrifugal treatment to eliminate bubbles to obtain mixed printing ink;
(3) Adding chitosan into water, uniformly mixing to obtain a chitosan solution, then adding lactic acid, and uniformly mixing to obtain a chitosan lactic acid solution;
(4) Adding 1-methylcyclopropene powder into the chitosan lactic acid solution obtained in the step (3), and uniformly mixing to obtain a chitosan/1-methylcyclopropene mixed solution;
(5) Performing coaxial 3D printing by using the mixed printing ink in the step (2) as an outer-layer printing material and the chitosan/1-methylcyclopropene mixed solution in the step (4) as an inner-layer printing material to obtain a 3D printing product;
(6) Dissolving calcium chloride and potassium chloride in water to obtain a calcium chloride/potassium chloride curing agent;
(7) Spraying the calcium chloride/potassium chloride curing agent in the step (6) on the surface of the 3D printing product in the step (5), curing, and freeze-drying to obtain the 3D printing freshness monitoring and freshness keeping integrated label;
the concentration of the nano-cellulose solution in the step (1) is 0.03-0.10g/mL; the mass ratio of the sodium alginate to the carrageenan is 1.2-1; the mass ratio of the total mass of the sodium alginate and the carrageenan to the mass of the nano cellulose solution is 1;
the mass ratio of the anthocyanin to the mixed system in the step (2) is 1; the speed of the centrifugal treatment is 2000-8000rpm, and the time of the centrifugal treatment is 1-10min;
the concentration of the chitosan solution in the step (3) is 1-10g/L; the volume of the lactic acid is 0.5-2.0% of the volume of the chitosan solution;
in the step (4), the mass ratio of the 1-methylcyclopropene to the chitosan lactic acid solution is (1).
2. The method for preparing the 3D printed integrated label with freshness monitoring and freshness keeping function according to claim 1, wherein the printing pressure of the coaxial 3D printing in the step (5) is 0.1-0.5MPa; the printing speed of the outer layer is 1-10mm/s; the printing speed of the inner layer is 1-5mL/h.
3. The method for preparing the 3D-printed integrated label for freshness monitoring and freshness keeping according to claim 1, wherein the mass ratio of the calcium chloride to the potassium chloride in the step (6) is 1; in the calcium chloride/potassium chloride curing agent, the concentrations of calcium chloride and potassium chloride are both 0.01-0.10g/mL.
4. The method for preparing the 3D printed integrated label with freshness monitoring and freshness keeping function according to claim 1, wherein the mass volume ratio of the 3D printed product to the calcium chloride/potassium chloride solution in the step (7) is 0.5-1.5:1g/mL; the time of the curing treatment is 5-50s.
5. A3D printed integrated freshness monitoring and freshness label made by the manufacturing method of any one of claims 1-4.
6. Use of the 3D printed freshness monitoring and freshness integral label of claim 5 in fruit freshness monitoring and fruit freshness preservation.
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