CN108384064B - Bagasse-based nano antibacterial preservative film and preparation method thereof - Google Patents
Bagasse-based nano antibacterial preservative film and preparation method thereof Download PDFInfo
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Abstract
The invention provides a bagasse-based nano antibacterial preservative film and a preparation method thereof, and relates to the field of crop straw utilization. The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight: 60-80% of bagasse nano-cellulose, 10-30% of chitin nano-whisker, 1-5% of cinnamon essential oil, 3-10% of chitosan, 1-3% of glycerol and 1-3% of sorbitol fatty acid ester. The nano antibacterial preservative film prepared by the invention has better strength and air permeability, can uniformly moisten the surface of the film and form a water film so as to prevent external microorganisms from entering, and the added cinnamon essential oil and chitosan can inhibit the growth and reproduction of the microorganisms so as to prolong the preservation period of fruits.
Description
Technical Field
The invention relates to the field of biomass recycling, in particular to a bagasse-based nano antibacterial preservative film and a preparation method thereof.
Background
The fruit production has strong seasonality and regionality, and in order to meet the demand of consumers on fruits, the fresh-keeping technology of fruits needs to be improved, and the marketing period of fresh fruits is prolonged. However, fresh fruits still have higher physiological activity after being harvested, and especially fruits with higher moisture content are more prone to rot and deteriorate, so that the prolonging of the storage, transportation and preservation time becomes the key of the value preservation and appreciation of the fresh fruits.
The current commonly used fruit preservation technology mainly comprises means of low-temperature storage, modified atmosphere preservation, addition of chemical preservatives and the like. However, these techniques have limitations in practical applications. The cold chain technology is relatively immature at present, and the fruits are more easily rotten and deteriorated due to temperature fluctuation in the processes of storage, transportation and sale, so that the long-distance transportation is not facilitated; the modified atmosphere preservation requires a modified atmosphere box or a gas generating device, so that the requirements on equipment are high and the cost is high; the chemical preservative can form residues on the surfaces of fruits and vegetables, and has potential food safety problems. In recent years, a coating preservation technology has been favored.
The sugarcane industry is the main economic crop in Guangxi and also the pillar industry in Guangxi, and is the main economic source of farmers. Sugarcane is one of the main raw materials for sugar production. The residual bagasse after sugar pressing accounts for about 24-27% of the cane (the water content is about 50%), and 2-3 tons of bagasse can be produced for each ton of cane sugar. For a long time, large batches of bagasse are mainly burned or discarded by the sugar mills themselves as fuel, and the economic value of the utilization method is very low. The development and utilization of bagasse resources can not only improve the economic benefits of sugar mills, but also provide a large amount of resources for other industries, which has great significance for economic development and resource recycling in Guangxi province.
The Chinese patent with the application number of 201310359396.4 discloses a preparation method of bagasse cellulose nanofiber membrane, which realizes the recycling and effective cyclic utilization of wastes, is not only beneficial to reducing the pollution to the environment, but also beneficial to the high-value utilization of bagasse, but the prepared fiber membrane has poor effect of keeping fruits fresh and has no antibacterial effect. Therefore, the preservative film prepared from the bagasse has low cost and antibacterial and fresh-keeping effects, and has high market value.
Disclosure of Invention
One of the objectives of the present invention is to provide a bagasse-based nano-antibacterial preservative film, which has good strength and air permeability, and can wet the surface of the film uniformly and form a water film, thereby preventing external microorganisms from entering the film, wherein the added chitin nanowhiskers provide the preservative film with good strength and toughness, and the added cinnamon essential oil and chitosan can inhibit the growth and propagation of microorganisms, thereby prolonging the preservation period of fruits.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
60-80% of bagasse nano-cellulose, 10-30% of chitin nano-whisker, 1-5% of cinnamon essential oil, 3-10% of chitosan, 1-3% of glycerol and 1-3% of sorbitol fatty acid ester.
Preferably, the diameter of the chitin nanowhisker is 30-50 nm.
Preferably, the preparation method of the bagasse nanocellulose comprises the following steps: stirring bagasse and a NaOH aqueous solution with the mass fraction of 5% -30% and the temperature of 40-100 ℃ for reaction for 30-90 min, centrifuging, reacting in a NaClO solution for 30-60 min under the assistance of ultrasound for oxidation bleaching, wherein the available chlorine in the solution is more than 10g/L, after the reaction is finished, performing centrifugal water washing treatment, stirring and acidolysis for 30-150 min at the temperature of 60-90 ℃ by using a sulfuric acid solution with the mass fraction of 50% -70%, centrifuging, adjusting the pH value to 6-7, and performing ultrasound for 5-20 min to obtain the bagasse nanocellulose.
Preferably, the bagasse nanocellulose is subjected to acetylation treatment, and the specific treatment process is as follows: adding glacial acetic acid into the bagasse nanocellulose, standing for 1-2 h to fully moisten and expand the fibers, and performing ultrasonic treatment for 10-20 min; and then adding acetic anhydride and concentrated sulfuric acid, reacting for 1-2 h at 50-60 ℃, cooling to room temperature, adding absolute ethyl alcohol to obtain white flocculent precipitate, carrying out vacuum filtration on the white flocculent precipitate, washing with distilled water to be neutral, and freeze-drying the precipitate to obtain the acetylated bagasse nanocellulose.
The invention also aims to solve the problems and provide a preparation method of the bagasse-based nano antibacterial preservative film, which has the advantages of simple process, no pollution, easy industrial production and good market prospect.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a bagasse-based nano antibacterial preservative film comprises the following steps:
s1, preparing chitin nano whiskers:
weighing chitin, dispersing in 10mol/L hydrochloric acid at a bath ratio of 1: 8-12, reacting at 50-60 ℃ until the solution is completely transparent to obtain a mixed solution, pouring the mixed solution into 3-5 times of deionized water, centrifuging, and drying to obtain the chitin nanowhiskers.
S2, preparing bagasse nanocellulose:
stirring and reacting bagasse with 5-30 mass percent of NaOH aqueous solution at 40-100 ℃ for 30-90 min, and centrifuging; then adding the mixture into NaClO solution, carrying out ultrasonic auxiliary reaction for 30-60 min for oxidation bleaching, and carrying out centrifugation and water washing treatment after the reaction is finished; and finally, stirring and acidolyzing the mixture for 30 to 150 minutes at the temperature of between 60 and 90 ℃ by using a sulfuric acid solution with the mass fraction of 50 to 70 percent, adjusting the pH value to between 6 and 7 after centrifugation, and performing ultrasonic treatment for 5 to 20 minutes to obtain the bagasse nanocellulose.
S3, preparing a film forming solution:
mixing chitin nanowhiskers and bagasse nanocellulose, adding the mixture into deionized water, stirring for 10-20 min, then adding cinnamon essential oil, chitosan, sorbitol fatty acid ester and glycerol, ultrasonically dispersing for 10-30 min, and standing to obtain a film forming solution;
s4, molding:
and uniformly coating the film-forming solution on a glass plate by adopting a tape casting method, and then carrying out freeze drying to obtain the bagasse-based nano antibacterial preservative film.
Preferably, in step S1, the mixed solution is poured into 3 times of deionized water, centrifuged at 9000rpm for 10min, and then centrifuged repeatedly for 2-3 times.
Preferably, in step S2, the bagasse nanocellulose is acetylated, and the specific treatment process is as follows: adding glacial acetic acid into the bagasse nanocellulose, standing for 1-2 h to fully moisten and expand the fibers, and performing ultrasonic treatment for 10-20 min; and then adding acetic anhydride and concentrated sulfuric acid, reacting for 1-2 h at 50-60 ℃, cooling to room temperature, adding absolute ethyl alcohol to obtain white flocculent precipitate, carrying out vacuum filtration on the white flocculent precipitate, washing with distilled water to be neutral, and freeze-drying the precipitate to obtain the acetylated bagasse nanocellulose.
Preferably, in step S2, the available chlorine in the NaClO solution is greater than 10 g/L.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. the bagasse-based nano antibacterial preservative film prepared by the invention is based on bagasse nano cellulose, and the chitin nano whiskers capable of enhancing the tensile strength of the composite film, and the natural and non-toxic cinnamon essential oil and chitosan with antibacterial effects are added, so that the preservative film has good mechanical properties and fresh-keeping and sterilizing effects.
The nano-cellulose whiskers and the chitin nano-whiskers are uniform in size and nano-scale, and the ultralow-porosity composite fiber prepared by combining the nano-cellulose whiskers and the chitin nano-whiskers has high air permeability, high strength, toughness and thermal stability, and is green and environment-friendly because the nano-cellulose whiskers and the chitin nano-whiskers are renewable resources. The chitin whisker nanometer forms a net structure through the interaction of hydrogen bonds, so that the modulus is kept unchanged in a large temperature range, and the formed tangled chitin whisker seepage net structure can also block the movement of chains, thereby improving the toughness and stability of the preservative film.
The cinnamon essential oil has a strong bactericidal effect on microorganisms, also has various effects of resisting tumors, viruses and ulcers, relieving fever, relieving pain and spasm, killing insects and the like, has small irritation to a human body, is natural and fragrant, is safe and environment-friendly, and can maintain a good bactericidal effect for a long time. The cinnamon essential oil and the chitosan are compounded, so that the antibacterial effect can be obviously improved, and the defect of insufficient antibacterial property of the preservative film prepared from the chitosan is overcome.
The bagasse nanocellulose is extracted from the bagasse, so that the waste recycling and effective recycling are realized. The method is simple, has low cost and easy popularization, realizes the reclamation and effective cyclic utilization of wastes, is not only beneficial to reducing the pollution to the environment, but also beneficial to the high-value utilization of bagasse.
2. Although the chitin has the properties of wide source, degradability, biocompatibility, no toxicity, low antigenicity and the like, the chitin is insoluble in water and most of organic solvents and exists in a precipitation form, so that the application of the chitin is limited. The surface of the chitin nano whisker has a large amount of hydroxyl, N-acetyl and a small amount of amino, so that the surface of the chitin nano whisker can be chemically modified by controlling chemical reaction conditions, a new functional group or a new macromolecular chain is introduced, the property of the chitin is improved, and the enhancing effect, the antibacterial performance, the hydrophobicity, the dispersibility and the compatibility of the chitin are improved.
The glycerol enters between molecular chains of the composite membrane to open the molecular chains of the membrane, so that the structure of the membrane is loose, the hydrophilicity is increased, and the moisture permeability of the composite membrane is increased. The sorbitol fatty acid ester can improve the toughness of the preservative film.
3. According to the preparation method of the bagasse-based nano antibacterial preservative film, the bagasse nano cellulose and the chitin nano whisker have the performances of nano size, high strength, high specific surface area, high length-diameter ratio and the like, the fibers are pressurized and heated in the process of water evaporation, the nano cellulose is mutually repelled by the capillary phenomenon, and the form of the fibers is kept unchanged by hydrogen bonds formed among the nano cellulose, so that a high-strength material can be formed without using a cross-linking agent. Simple process, no pollution, easy industrial production and good market prospect.
4. The preparation method of the bagasse-based nano antibacterial preservative film has the advantages of simple process, no pollution, easy industrial production and good market prospect.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
75% of bagasse nano-cellulose, 10% of chitin nano-whisker, 3% of cinnamon essential oil, 8% of chitosan, 2% of glycerol and 2% of sorbitol fatty acid ester.
The diameter of the chitin nano whisker is 40 nm.
A preparation method of a bagasse-based nano antibacterial preservative film comprises the following steps:
s1, preparing chitin nano whiskers:
weighing chitin, dispersing in 10mol/L hydrochloric acid at a bath ratio of 1:10, reacting at 55 ℃ until the solution is completely transparent to obtain a mixed solution, pouring the mixed solution into 3 times of deionized water, centrifuging at 9000rpm for 10min, then repeatedly centrifuging for 2 times, and then drying to obtain the chitin nanowhiskers.
S2, preparing bagasse nanocellulose:
stirring and reacting bagasse with 10 mass percent of NaOH aqueous solution at the temperature of 60 ℃ for 60min, and centrifuging; then adding the solution into NaClO solution, carrying out ultrasonic auxiliary reaction for 45min to carry out oxidation bleaching, wherein the available chlorine in the NaClO solution is more than 10g/L, and carrying out centrifugation and water washing treatment after the reaction is finished; and finally, stirring and carrying out acidolysis for 60min at 80 ℃ by using a sulfuric acid solution with the mass fraction of 60%, regulating the pH value to 7 after centrifugation, and carrying out ultrasonic treatment for 15min to obtain the bagasse nanocellulose.
S3, preparing a film forming solution:
mixing chitin nanowhiskers and bagasse nanocellulose, adding into deionized water, stirring for 15min, adding cinnamon essential oil, chitosan, sorbitol fatty acid ester and glycerol, ultrasonically dispersing for 20min, and standing to obtain a film forming solution.
S4, molding:
and uniformly coating the film-forming solution on a glass plate by adopting a tape casting method, and then carrying out freeze drying to obtain the bagasse-based nano antibacterial preservative film.
Example 2
The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
70% of bagasse nano-cellulose, 15% of chitin nano-whisker, 3% of cinnamon essential oil, 8% of chitosan, 2% of glycerol and 2% of sorbitol fatty acid ester.
The diameter of the chitin nano whisker is 40 nm.
The preparation method is the same as example 1.
Example 3
The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
65% of bagasse nano-cellulose, 20% of chitin nano-whisker, 3% of cinnamon essential oil, 8% of chitosan, 2% of glycerol and 2% of sorbitol fatty acid ester.
The diameter of the chitin nano whisker is 40 nm.
The preparation method is the same as example 1.
Example 4
The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
60% of bagasse nano-cellulose, 25% of chitin nano-whisker, 3% of cinnamon essential oil, 8% of chitosan, 2% of glycerol and 2% of sorbitol fatty acid ester.
The diameter of the chitin nano whisker is 40 nm.
The preparation method is the same as example 1.
Example 5
The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
60% of bagasse nano-cellulose, 28% of chitin nano-whisker, 3% of cinnamon essential oil, 5% of chitosan, 2% of glycerol and 2% of sorbitol fatty acid ester.
The diameter of the chitin nano whisker is 40 nm.
The preparation method is the same as example 1.
Example 6
The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
60% of bagasse nano-cellulose, 30% of chitin nano-whisker, 3% of cinnamon essential oil, 3% of chitosan, 2% of glycerol and 2% of sorbitol fatty acid ester.
The diameter of the chitin nano whisker is 40 nm.
The preparation method is the same as example 1.
Example 7
The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
60% of bagasse nano-cellulose, 25% of chitin nano-whisker, 3% of cinnamon essential oil, 8% of chitosan, 2% of glycerol and 2% of sorbitol fatty acid ester.
The diameter of the chitin nano whisker is 60 nm.
The preparation method is the same as example 1.
Comparative example 1
The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
85% of bagasse nano-cellulose, 3% of cinnamon essential oil, 8% of chitosan, 2% of glycerol and 2% of sorbitol fatty acid ester.
The preparation method is the same as example 1.
Comparative example 2
The bagasse-based nano antibacterial preservative film comprises the following components in percentage by weight:
63% of bagasse nano-cellulose, 25% of chitin nano-whisker, 8% of chitosan, 2% of glycerol and 2% of sorbitol fatty acid ester.
The diameter of the chitin nano whisker is 40 nm.
The preparation method is the same as example 1.
Comparative example 3
Common PE preservative film
The wrap films prepared in examples 1 to 7 and comparative examples 1 to 3 were tested for tensile strength, elongation at break, light transmittance, oxygen transmission rate and mass loss, and the results are shown in table 1 below.
TABLE 1 comparison of test results for examples 1-7 and comparative examples 1-3
As can be seen from the data of examples 1-7 and comparative example 3 combined with the data of Table 1, the preservative film prepared by the invention has greatly improved mechanical properties, greatly improved tensile strength and elongation at break, reduced oxygen transmission rate and better preservation effect compared with the common PE preservative film. The nano-cellulose whiskers and the chitin nano-whiskers are uniform in size and nano-scale, the composite fiber with ultralow porosity, which is prepared by combining the nano-cellulose whiskers and the chitin nano-whiskers, has high air permeability, high strength, toughness and thermal stability, and the sources of the nano-cellulose whiskers and the chitin nano-whiskers are renewable resources, so that the recycling and effective cyclic utilization of wastes are realized, the environmental pollution is favorably reduced, and the high-value utilization of bagasse is favorably realized.
As can be seen from the data of examples 1 to 6 and comparative example 1 in combination with the data of table 1, at the same time, as the content of the chitin nanowhiskers increases, the transverse rupture strength and the longitudinal rupture strength of the antibacterial film continuously increase, but reach 25%, at the equilibrium stage, and decrease at 28%. This is because: the chitin nano whisker has the advantages that the chitin nano whisker is well dispersed in a matrix and interacts with the matrix, the reinforcement effect has a threshold effect, and when the dosage exceeds a certain amount, the filler is easy to aggregate, so that the mechanical property is reduced, and the tensile strength and the elongation at break are increased firstly and then reduced along with the increase of the dosage of the chitin nano whisker. Therefore, the content of the chitin nanowhiskers needs to be strictly controlled, and when the content is 25%, the effect is better, and the cost is saved.
As can be seen from the data of example 4 and comparative example 2 in combination with the data of table 1, the cinnamon essential oil has a significant effect on the improvement of the preservative effect of the preservative film. Because the cinnamon essential oil has a strong bactericidal effect on microorganisms, can maintain a good bactericidal effect for a long time, and can obviously improve the antibacterial effect and overcome the defect of insufficient antibacterial property of the preservative film prepared from chitosan by compounding with chitosan.
The above description is directed to the details of the preferred and possible embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention. All changes and modifications that come within the spirit of the invention are desired to be protected.
Claims (6)
1. The bagasse-based nano antibacterial preservative film is characterized by comprising the following components in percentage by weight:
60% of bagasse nano-cellulose, 25% of chitin nano-whisker, 1% -5% of cinnamon essential oil, 8% of chitosan, 1% -3% of glycerol and 1% -3% of sorbitol fatty acid ester;
the preparation method of the bagasse nanocellulose comprises the following steps: stirring bagasse and a NaOH aqueous solution with the mass fraction of 5% -30% and the temperature of 40-100 ℃ for reaction for 30-90 min, centrifuging, reacting in a NaClO solution for 30-60 min under the assistance of ultrasound for oxidation bleaching, wherein the available chlorine in the solution is more than 10g/L, after the reaction is finished, performing centrifugal water washing treatment, stirring and acidolysis for 30-150 min at the temperature of 60-90 ℃ by using a sulfuric acid solution with the mass fraction of 50% -70%, centrifuging, adjusting the pH value to 6-7, and performing ultrasound for 5-20 min to obtain bagasse nanocellulose;
performing acetylation treatment on the bagasse nanocellulose, wherein the specific treatment process comprises the following steps: adding glacial acetic acid into the bagasse nanocellulose, standing for 1-2 h to fully moisten and expand the fibers, and performing ultrasonic treatment for 10-20 min; and then adding acetic anhydride and concentrated sulfuric acid, reacting for 1-2 h at 50-60 ℃, cooling to room temperature, adding absolute ethyl alcohol to obtain white flocculent precipitate, carrying out vacuum filtration on the white flocculent precipitate, washing with distilled water to be neutral, and freeze-drying the precipitate to obtain the acetylated bagasse nanocellulose.
2. The bagasse-based nano antibacterial preservative film according to claim 1, wherein the diameter of the chitin nanowhiskers is 30 to 50 nm.
3. The preparation method of the bagasse-based nano-antibacterial preservative film according to any one of claims 1-2, characterized by comprising the steps of:
s1, preparing chitin nano whiskers:
weighing chitin, dispersing in 10mol/L hydrochloric acid at a bath ratio of 1: 8-12, reacting at 50-60 ℃ until the solution is completely transparent to obtain a mixed solution, pouring the mixed solution into 3-5 times of deionized water, centrifuging, and drying to obtain chitin nanowhiskers;
s2, preparing bagasse nanocellulose:
stirring and reacting bagasse with 5-30 wt% of NaOH aqueous solution at 40-100 ℃ for 30-90 min, and centrifuging; then adding the mixture into NaClO solution, carrying out ultrasonic auxiliary reaction for 30-60 min for oxidation bleaching, and carrying out centrifugation and water washing treatment after the reaction is finished; finally, stirring and acidolyzing the mixture for 30 to 150 minutes at the temperature of between 60 and 90 ℃ by using a sulfuric acid solution with the mass fraction of 50 to 70 percent, adjusting the pH value to between 6 and 7 after centrifugation, and performing ultrasonic treatment for 5 to 20 minutes to obtain bagasse nanocellulose;
s3, preparing a film forming solution:
mixing chitin nanowhiskers and bagasse nanocellulose, adding the mixture into deionized water, stirring for 10-20 min, then adding cinnamon essential oil, chitosan, sorbitol fatty acid ester and glycerol, ultrasonically dispersing for 10-30 min, and standing to obtain a film forming solution;
s4, molding:
and uniformly coating the film-forming solution on a glass plate by adopting a tape casting method, and then carrying out freeze drying to obtain the bagasse-based nano antibacterial preservative film.
4. The preparation method of the bagasse-based nano-antibacterial preservative film according to claim 3, wherein in step S1, the mixed solution is poured into 3 times of deionized water, centrifuged at 9000rpm for 10min, and then centrifuged repeatedly for 2-3 times.
5. The preparation method of the bagasse-based nano-antibacterial preservative film according to claim 3, wherein in step S2, the bagasse nanocellulose is acetylated, and the specific treatment process is as follows: adding glacial acetic acid into the bagasse nanocellulose, standing for 1-2 h to fully moisten and expand the fibers, and performing ultrasonic treatment for 10-20 min; and then adding acetic anhydride and concentrated sulfuric acid, reacting for 1-2 h at 50-60 ℃, cooling to room temperature, adding absolute ethyl alcohol to obtain white flocculent precipitate, carrying out vacuum filtration on the white flocculent precipitate, washing with distilled water to be neutral, and freeze-drying the precipitate to obtain the acetylated bagasse nanocellulose.
6. The method for preparing the bagasse-based nano antibacterial preservative film according to claim 3, wherein in step S2, the available chlorine in the NaClO solution is more than 10 g/L.
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