CN113234260A - Preparation method of guar gum base nano composite film - Google Patents
Preparation method of guar gum base nano composite film Download PDFInfo
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- CN113234260A CN113234260A CN202110625126.8A CN202110625126A CN113234260A CN 113234260 A CN113234260 A CN 113234260A CN 202110625126 A CN202110625126 A CN 202110625126A CN 113234260 A CN113234260 A CN 113234260A
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- guar gum
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- polyvinyl alcohol
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- ginseng root
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- 229920002907 Guar gum Polymers 0.000 title claims abstract description 192
- 239000000665 guar gum Substances 0.000 title claims abstract description 192
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- 235000010417 guar gum Nutrition 0.000 title claims abstract description 192
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 124
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 68
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 68
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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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
- C08J2429/00—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
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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Abstract
The invention provides a preparation method of a guar gum base nano composite film, which comprises the following steps: firstly, adding a polyvinyl alcohol aqueous solution with improved film forming performance into a guar gum aqueous solution, adding glycerol as a plasticizer and citric acid as a cross-linking agent, mixing and stirring to prepare a guar gum film forming solution, adding nano zinc oxide with improved antibacterial performance and a ginseng root extract with improved oxidation resistance, mixing and stirring, performing ultrasonic dispersion and vacuum defoaming, then casting the mixture in a glass vessel, and stripping the film after vacuum drying to obtain the guar gum base nano composite film with antibacterial and antioxidant functions. The guar gum base nano composite membrane prepared by the invention has excellent film forming property, oxidation resistance and bacteriostatic ability, and has good mechanical property and barrier property.
Description
Technical Field
The invention belongs to the technical field of nano composite films, and particularly relates to a preparation method of a guar gum base nano composite film.
Background
Guar gum is a natural polysaccharide gum extracted from the endosperm of guar seeds, can quickly form a high-viscosity solution in water, has good water solubility and thickening effect, and is widely applied to the fields of food, medicine, papermaking, printing and dyeing, petroleum industry and the like. However, guar gum has the disadvantages that the viscosity of the film forming solution is not easy to control, and the guar gum is easy to decompose by microorganisms and cannot be stored for a long time, so that the application of the guar gum in food packaging films is greatly limited. From the molecular structure of the guar gum, a macromolecule straight chain does not have a nonpolar group, but four hydroxyl groups on the branched galactose and the hydroxyl group of the mannose have hydrogen bond reaction activity, so that the guar gum can be chemically modified, the defects of a guar gum film forming solution are overcome, and the application of the guar gum in the field of food packaging is expanded.
The polyvinyl alcohol is a high molecular material which is biodegradable, nontoxic, high in hydrophilicity, good in biocompatibility, film-forming property and chemical stability. A large number of hydroxyl groups also exist in the molecular structure of the polyvinyl alcohol, so that an intermolecular hydrogen bond network system can be formed between the polyvinyl alcohol and guar gum, and a composite membrane with excellent mechanical properties is formed. The nano zinc oxide is used in food packing field, and can raise the mechanical performance and bacteriostasis performance of packing material. The ginseng root extract contains rich active ingredients, such as ginsenoside, panaxynol, panaxydol, alkaloid, oligosaccharide and other compounds, has excellent oxidation resistance, and can improve the oxidation resistance of the guar gum film by adding the ginseng root extract into the guar gum film-forming liquid.
At present, many reports of polysaccharide gum-inorganic nanoparticle composite materials exist, the research focuses on the aspect of adding nano silver and the like to improve the antibacterial performance of a polysaccharide adhesive film, or adding natural active polyphenol compounds to improve the oxidation resistance of the polysaccharide adhesive film, and no report exists for researching the antibacterial performance and the oxidation resistance of a guar gum-ginseng root extract-nano zinc oxide based composite film.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a guar gum base nano composite membrane aiming at the defects of the prior art, and the guar gum base nano composite membrane prepared by the method has excellent film forming property, oxidation resistance and bacteriostatic ability, and has good mechanical property and barrier property.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a guar gum base nano composite film is characterized by comprising the following steps:
s1, preparing guar gum film forming liquid: adding distilled water a into guar gum, and magnetically stirring for 30min under the water bath condition at the temperature of 65 ℃ to obtain a guar gum water solution; adding distilled water b into polyvinyl alcohol, magnetically stirring for 2 hours under the water bath condition at the temperature of 80 ℃ to obtain a polyvinyl alcohol aqueous solution, mixing the guar gum aqueous solution and the polyvinyl alcohol aqueous solution with the improved film-forming property, magnetically stirring for 1 hour under the water bath condition at the temperature of 80 ℃ to obtain a guar gum polyvinyl alcohol mixed solution, then adding glycerol as a plasticizer and citric acid as a cross-linking agent into the guar gum polyvinyl alcohol mixed solution, and magnetically stirring for 2 hours under the water bath condition at the temperature of 50 ℃ to obtain a guar gum film-forming solution;
the dosage ratio of the guar gum to the distilled water a is 1g:100 mL; the dosage ratio of the polyvinyl alcohol to the distilled water b is 1g:100 mL;
guar gum, polyvinyl alcohol, glycerol and citric acid used in the guar gum film forming solution all contain hydroxyl, and intermolecular hydrogen bonds can improve the film forming property of the guar gum and improve the strength of a film;
s2, preparing a ginseng root extract solution: grinding ginseng roots, sieving the ground ginseng roots by a 60-mesh sieve to obtain ginseng root powder, soaking the ginseng root powder in an ethanol solution with the mass fraction of 90% for extraction for 2 hours to obtain an extracting solution a, then soaking the residual residue a in an ethanol solution with the mass fraction of 70% for extraction for 2 hours to obtain an extracting solution b, then soaking the residual residue b in an ethanol solution with the mass fraction of 50% for extraction for 2 hours to obtain an extracting solution c, combining the extracting solution a, the extracting solution b and the extracting solution c to obtain a mixed extracting solution, performing ultrasonic dispersion for 30 minutes, centrifuging for 3 times at the rotation speed of 10000r/min, centrifuging for 10 minutes each time, filtering supernatant, and performing rotary evaporation concentration to obtain a ginseng root extract solution;
and S3, adding the nano zinc oxide with the antibacterial performance improved and the ginseng root extract solution with the oxidation resistance improved obtained in the S2 into the guar gum film forming solution obtained in the S1 to obtain guar gum base nano composite liquid, magnetically stirring for 2 hours, then ultrasonically dispersing for 30 minutes, casting in a glass dish after vacuum defoamation, drying in a vacuum drying oven at the temperature of 45 ℃ for 24 hours, and then uncovering the film to obtain the guar gum base nano composite film.
Preferably, the alcoholysis degree of the polyvinyl alcohol in S1 is 88%.
Preferably, the mass ratio of the guar gum aqueous solution to the polyvinyl alcohol aqueous solution in the guar gum polyvinyl alcohol mixed solution in S1 is (7-9): (1-3); the mass ratio of the guar gum polyvinyl alcohol mixed solution to the glycerol to the citric acid in the guar gum film-forming solution is 1:0.3: 0.2.
Preferably, the mass concentration of the ginseng root extract solution in S2 is 0.01 g/mL.
Preferably, the particle size of the nano zinc oxide in S3 is 20 nm-40 nm.
Preferably, the ultrasonic power of the ultrasonic dispersion in S2 and S3 is 600W, and the ultrasonic frequency is 40 kHz.
Preferably, the mass of the ginseng root extract solution in the S3 is 20-40% of the sum of the mass of the guar gum and the polyvinyl alcohol in the guar gum film-forming solution; the mass of the nano zinc oxide is 5% of the total mass of the guar gum and the polyvinyl alcohol in the guar gum film-forming liquid.
Preferably, the guar-based nanocomposite membrane of S3 has an average thickness of 50 to 70 μm.
Compared with the prior art, the invention has the following advantages:
according to the invention, the guar gum is not subjected to complex modification operations such as oxidation, esterification, etherification and enzymatic degradation, complex and expensive equipment is not needed, the preparation process flow is simple, the reaction condition is mild, the guar gum is used as a film forming matrix, the polyvinyl alcohol is added to improve the film forming property, meanwhile, the high-activity component of the ginseng root extract solution is added to improve the oxidation resistance of the guar gum base nano composite film, and the nano zinc oxide is added to endow the guar gum base nano composite film with good bacteriostatic ability. The interaction of the raw materials in the guar gum base nano composite membrane can improve the mechanical property and the barrier property of the guar gum base nano composite membrane, and can disperse the nano zinc oxide in a mixed system to avoid aggregation to influence the antibacterial effect. The successful implementation of the preparation method is beneficial to expanding the application field of the guar gum base nano composite membrane as a food packaging material.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
Fig. 1 is a graph showing the inhibitory effect of the guar-based nanocomposite fluid obtained in step S3 of the present invention on escherichia coli (e.coli) and staphylococcus aureus (s.au).
Fig. 2 is a scanning electron microscope cross-section of the guar-based nanocomposite film prepared in example 1 of the present invention.
Detailed Description
Example 1
The preparation method of the guar gum based nano composite membrane is characterized by comprising the following steps:
s1, preparing guar gum film forming liquid: adding distilled water a into guar gum, and magnetically stirring for 30min at a speed of 600r/min under a water bath condition at a temperature of 65 ℃ to obtain a guar gum water solution; adding distilled water b into polyvinyl alcohol, magnetically stirring for 2 hours at a speed of 600r/min under a water bath condition at the temperature of 80 ℃ to obtain a polyvinyl alcohol aqueous solution, mixing the guar gum aqueous solution and the polyvinyl alcohol aqueous solution, magnetically stirring for 1 hour at a speed of 600r/min under a water bath condition at the temperature of 80 ℃ to obtain a guar gum and polyvinyl alcohol mixed solution, then adding glycerol and citric acid into the guar gum and polyvinyl alcohol mixed solution, and magnetically stirring for 2 hours at a speed of 600r/min under a water bath condition at the temperature of 50 ℃ to obtain a guar gum film forming solution; the dosage ratio of the guar gum to the distilled water a is 1g:100 mL; the dosage ratio of the polyvinyl alcohol to the distilled water b is 1g:100 mL; the mass ratio of the guar gum aqueous solution to the polyvinyl alcohol aqueous solution in the guar gum polyvinyl alcohol mixed solution is 9: 1; the mass ratio of the guar gum polyvinyl alcohol mixed solution to the glycerol to the citric acid in the guar gum film-forming solution is 1:0.3: 0.2;
s2, preparing a ginseng root extract solution: grinding ginseng roots, sieving the ground ginseng roots by a 60-mesh sieve to obtain ginseng root powder, soaking the ginseng root powder in an ethanol solution with the mass fraction of 90% for extraction for 2 hours to obtain an extracting solution a, then soaking the residual residue a in an ethanol solution with the mass fraction of 70% for extraction for 2 hours to obtain an extracting solution b, then soaking the residual residue b in an ethanol solution with the mass fraction of 50% for extraction for 2 hours to obtain an extracting solution c, combining the extracting solution a, the extracting solution b and the extracting solution c to obtain a mixed extracting solution, ultrasonically dispersing for 30 minutes at the ultrasonic frequency of 40kHz and the ultrasonic power of 600W, then centrifuging at the rotating speed of 10000r/min for 3 times and 10 minutes each time, filtering supernatant, and then performing rotary evaporation and concentration to obtain a ginseng root extract solution with the mass concentration of 0.01 g/mL;
s3, adding nano zinc oxide with the granularity of 20-40 nm and the ginseng root extract solution obtained in S2 into the guar gum film forming solution obtained in S1 to obtain guar gum base nano composite solution, magnetically stirring at the speed of 600r/min for 2 hours, ultrasonically dispersing at the ultrasonic power of 600W and the ultrasonic frequency of 40kHz for 30 minutes, defoaming in vacuum, casting in a glass dish, drying in a vacuum drying oven with the temperature of 45 ℃ and the vacuum degree of-0.9 MPa for 24 hours, and uncovering the membrane to obtain the guar gum base nano composite membrane; the mass of the ginseng root extract solution is 20% of the sum of the mass of guar gum and polyvinyl alcohol in the guar gum film-forming solution; the mass of the nano zinc oxide is 5% of the total mass of the guar gum and the polyvinyl alcohol in the guar gum film-forming liquid.
Example 2
The preparation method of the guar gum based nano composite membrane is characterized by comprising the following steps:
s1, preparing guar gum film forming liquid: adding distilled water a into guar gum, and magnetically stirring for 30min at a speed of 600r/min under a water bath condition at a temperature of 65 ℃ to obtain a guar gum water solution; adding distilled water b into polyvinyl alcohol, magnetically stirring for 2 hours at a speed of 600r/min under a water bath condition at the temperature of 80 ℃ to obtain a polyvinyl alcohol aqueous solution, mixing the guar gum aqueous solution and the polyvinyl alcohol aqueous solution, magnetically stirring for 1 hour at a speed of 600r/min under a water bath condition at the temperature of 80 ℃ to obtain a guar gum and polyvinyl alcohol mixed solution, then adding glycerol and citric acid into the guar gum and polyvinyl alcohol mixed solution, and magnetically stirring for 2 hours at a speed of 600r/min under a water bath condition at the temperature of 50 ℃ to obtain a guar gum film forming solution; the dosage ratio of the guar gum to the distilled water a is 1g:100 mL; the dosage ratio of the polyvinyl alcohol to the distilled water b is 1g:100 mL; the mass ratio of the guar gum aqueous solution to the polyvinyl alcohol aqueous solution in the guar gum polyvinyl alcohol mixed solution is 8: 2; the mass ratio of the guar gum polyvinyl alcohol mixed solution to the glycerol to the citric acid in the guar gum film-forming solution is 1:0.3: 0.2;
s2, preparing a ginseng root extract solution: grinding ginseng roots, sieving the ground ginseng roots by a 60-mesh sieve to obtain ginseng root powder, soaking the ginseng root powder in an ethanol solution with the mass fraction of 90% for extraction for 2 hours to obtain an extracting solution a, then soaking the residual residue a in an ethanol solution with the mass fraction of 70% for extraction for 2 hours to obtain an extracting solution b, then soaking the residual residue b in an ethanol solution with the mass fraction of 50% for extraction for 2 hours to obtain an extracting solution c, combining the extracting solution a, the extracting solution b and the extracting solution c to obtain a mixed extracting solution, ultrasonically dispersing for 30 minutes at the ultrasonic frequency of 40kHz and the ultrasonic power of 600W, then centrifuging at the rotating speed of 10000r/min for 3 times and 10 minutes each time, filtering supernatant, and then performing rotary evaporation and concentration to obtain a ginseng root extract solution with the mass concentration of 0.01 g/mL;
s3, adding nano zinc oxide with the granularity of 20-40 nm and the ginseng root extract solution obtained in S2 into the guar gum film forming solution obtained in S1 to obtain guar gum base nano composite solution, magnetically stirring at the speed of 600r/min for 2 hours, ultrasonically dispersing at the ultrasonic power of 600W and the ultrasonic frequency of 40kHz for 30 minutes, carrying out vacuum defoamation under the vacuum degree of-0.9 MPa, casting in a glass dish, drying in a vacuum drying oven at the temperature of 45 ℃ for 24 hours, and then uncovering the membrane to obtain the guar gum base nano composite membrane; the mass of the ginseng root extract solution is 30% of the sum of the mass of guar gum and polyvinyl alcohol in the guar gum film-forming solution; the mass of the nano zinc oxide is 5% of the total mass of the guar gum and the polyvinyl alcohol in the guar gum film-forming liquid.
Example 3
The preparation method of the guar gum based nano composite membrane is characterized by comprising the following steps:
s1, preparing guar gum film forming liquid: adding distilled water a into guar gum, and magnetically stirring for 30min at a speed of 600r/min under a water bath condition at a temperature of 65 ℃ to obtain a guar gum water solution; adding distilled water b into polyvinyl alcohol, magnetically stirring for 2 hours at a speed of 600r/min under a water bath condition at the temperature of 80 ℃ to obtain a polyvinyl alcohol aqueous solution, mixing the guar gum aqueous solution and the polyvinyl alcohol aqueous solution, magnetically stirring for 1 hour at a speed of 600r/min under a water bath condition at the temperature of 80 ℃ to obtain a guar gum and polyvinyl alcohol mixed solution, then adding glycerol and citric acid into the guar gum and polyvinyl alcohol mixed solution, and magnetically stirring for 2 hours at a speed of 600r/min under a water bath condition at the temperature of 50 ℃ to obtain a guar gum film forming solution; the dosage ratio of the guar gum to the distilled water a is 1g:100 mL; the dosage ratio of the polyvinyl alcohol to the distilled water b is 1g:100 mL; the mass ratio of the guar gum aqueous solution to the polyvinyl alcohol aqueous solution in the guar gum polyvinyl alcohol mixed solution is 7: 3; the mass ratio of the guar gum polyvinyl alcohol mixed solution to the glycerol to the citric acid in the guar gum film-forming solution is 1:0.3: 0.2;
s2, preparing a ginseng root extract solution: grinding ginseng roots, sieving the ground ginseng roots by a 60-mesh sieve to obtain ginseng root powder, soaking the ginseng root powder in an ethanol solution with the mass fraction of 90% for extraction for 2 hours to obtain an extracting solution a, then soaking the residual residue a in an ethanol solution with the mass fraction of 70% for extraction for 2 hours to obtain an extracting solution b, then soaking the residual residue b in an ethanol solution with the mass fraction of 50% for extraction for 2 hours to obtain an extracting solution c, combining the extracting solution a, the extracting solution b and the extracting solution c to obtain a mixed extracting solution, ultrasonically dispersing for 30 minutes at the ultrasonic frequency of 40kHz and the ultrasonic power of 600W, then centrifuging at the rotating speed of 10000r/min for 3 times and 10 minutes each time, filtering supernatant, and then performing rotary evaporation and concentration to obtain a ginseng root extract solution with the mass concentration of 0.01 g/mL;
s3, adding nano zinc oxide with the granularity of 20-40 nm and the ginseng root extract solution obtained in S2 into the guar gum film forming solution obtained in S1 to obtain guar gum base nano composite solution, magnetically stirring at the speed of 600r/min for 2 hours, ultrasonically dispersing at the ultrasonic power of 600W and the ultrasonic frequency of 40kHz for 30 minutes, carrying out vacuum defoamation under the vacuum degree of-0.9 MPa, casting in a glass dish, drying in a vacuum drying oven at the temperature of 45 ℃ for 24 hours, and then uncovering the membrane to obtain the guar gum base nano composite membrane; the mass of the ginseng root extract solution is 40% of the sum of the mass of guar gum and polyvinyl alcohol in the guar gum film-forming solution; the mass of the nano zinc oxide is 5% of the total mass of the guar gum and the polyvinyl alcohol in the guar gum film-forming liquid.
Comparative example 1
The comparative example is a preparation method of guar gum film (GG), which comprises the following steps:
s1, preparing guar gum water solution: adding distilled water a into guar gum, and magnetically stirring for 30min at a speed of 600r/min under a water bath condition at a temperature of 65 ℃ to obtain a guar gum water solution; the dosage ratio of the guar gum to the distilled water a is 1g:100 mL;
and S2, performing vacuum defoamation on the guar gum aqueous solution obtained in the S1 under the condition that the vacuum degree is-0.9 MPa, casting the guar gum aqueous solution in a glass dish, drying the guar gum aqueous solution in a vacuum drying oven at the temperature of 45 ℃ for 24 hours, and then uncovering the guar gum membrane to obtain a guar gum membrane, which is marked as GG.
Comparative example 2
The comparative example is a preparation method of guar gum film (GG-1), and the method comprises the following steps:
s1, preparing guar gum film forming liquid: same as S1 of example 1;
and S2, ultrasonically dispersing the guar gum film forming solution obtained in the S1 for 30min at the ultrasonic frequency of 40kHz and the ultrasonic power of 600W, then casting the guar gum film forming solution into a glass dish after vacuum defoamation under the vacuum degree of-0.9 MPa, drying the guar gum film forming solution in a vacuum drying oven at the temperature of 45 ℃ for 24h, and then uncovering the guar gum film to obtain the guar gum film which is marked as GG-1.
Comparative example 3
The comparative example is a preparation method of guar gum film (GG-2), and the method comprises the following steps:
s1, preparing guar gum film forming liquid: same as S1 of example 2;
and S2, ultrasonically dispersing the guar gum film forming solution obtained in the S1 for 30min at the ultrasonic frequency of 40kHz and the ultrasonic power of 600W, then casting the guar gum film forming solution into a glass dish after vacuum defoamation under the vacuum degree of-0.9 MPa, drying the guar gum film forming solution in a vacuum drying oven at the temperature of 45 ℃ for 24h, and then uncovering the guar gum film to obtain the guar gum film which is marked as GG-2.
Comparative example 4
The comparative example is a preparation method of guar gum film (GG-3), and the method comprises the following steps:
s1, preparing guar gum film forming liquid: same as S1 of example 3;
and S2, ultrasonically dispersing the guar gum film forming solution obtained in the S1 for 30min at the ultrasonic frequency of 40kHz and the ultrasonic power of 600W, then casting the guar gum film forming solution into a glass dish after vacuum defoamation under the vacuum degree of-0.9 MPa, drying the guar gum film forming solution in a vacuum drying oven at the temperature of 45 ℃ for 24h, and then uncovering the guar gum film to obtain the guar gum film, wherein the guar gum film is marked as GG-3.
The film properties of examples 1 to 3 and comparative examples 1 to 4 were tested, and the index test of each example (comparative example) was repeated 5 times, and the results are shown in Table 1.
The test method of each index comprises the following steps:
(1) tensile strength test method is as follows: the dimensions of each film sample are 15X 90mm, the initial clamping distance of a tensile testing machine is 50mm, the tensile speed is 300mm/min, and the calculation formula is as follows:
TS＝P/(B×T)
in the formula:
TS-is tensile strength (MPa);
p- -is the maximum load (N);
b-is the sample film width (mm);
t-is the thickness (mm) of the sample film.
(2) The moisture permeability coefficient test method is as follows: the size of each film sample is 6cm in diameter, the film samples are sealed on the surface of a moisture permeable cup by hot melt adhesive, and 20g of anhydrous calcium chloride serving as a drying agent is placed in the moisture permeable cup. And putting the moisture permeable cup in a solution containing saturated sodium chloride, taking out the cup at regular intervals, weighing, and calculating to obtain the moisture permeability coefficient. The calculation formula is as follows:
WVP＝(△m×B)/(△t×S×P)
in the formula:
WVP- -is the water vapor transmission coefficient (g.m)-1·s·Pa-1)；
Δ m/. DELTA.t- -is the water vapor transmission (g/s) per unit time;
b-is the average thickness (mm) of the sample film;
s- -is the effective area (m) of the sample film2)；
P-is the osmotic pressure (Pa) of a NaCl saturated solution.
(3) The DPPH free radical clearance rate is determined as follows: 50mg of each membrane sample was immersed in 10mL of a 95% ethanol solution by mass and shaken at 25 ℃ for 24 hours. Subsequently, 1mL of the membrane extract was added to 100. mu.M of a 50mg/L solution of DPPH in ethanol, and the mixture was left to react at room temperature for 15min with exclusion of light. Finally, the absorbance was measured at a wavelength of 517nm, and 1mL of ethanol was used as a blank. The calculation formula is as follows:
I＝[(Abs0-Abslifting device)/Abs0]×100
In the formula:
i- -is DPPH radical clearance (%) of the sample membrane;
Abs0and AbsLifting deviceRespectively the absorbance values of the solvent used as a blank and the sample membrane extract after reaction.
TABLE 1 film Properties of examples 1-3 and comparative examples 1-4
Note: in the table, "━" indicates that no measurement was performed.
In the tensile strength test, as can be seen from the data in comparative examples 1 to 4, the tensile strength value of the guar gum film is gradually increased after the polyvinyl alcohol, the glycerol and the citric acid are added, wherein the tensile strength of comparative example 4 is improved by nearly 28.32% compared with that of comparative example 1, because the four substances all contain hydroxyl groups on the molecular structure, intermolecular hydrogen bonds can be formed between the four substances, and the mechanical strength of the material is improved. As can be seen from the data in comparative examples 2-4 and examples 1-3, the tensile strength of the guar-based nanocomposite membrane (example 1) after adding the ginseng root extract solution in an amount of 20% by mass of the sum of the amounts of guar gum and polyvinyl alcohol in the guar-based membrane-forming solution was improved by 36.23% compared to the nanocomposite membrane (comparative example 2) without adding the ginseng root extract solution, and after adding the ginseng root extract solution in an amount of 30% (example 2) and 40% (example 3) by mass of the sum of the amounts of guar gum and polyvinyl alcohol in the guar-based membrane-forming solution, the tensile strength of the guar-based nanocomposite membranes increased by 14.23% (relative to comparative example 3) and 4.5% (relative to comparative example 4), respectively, at lower values, this is due to the fact that the solvent content of the composite system is increased and the tight bonds between the molecules are dispersed. And the guar based nanocomposite membrane of example 1 showed the best mechanical properties.
In the moisture permeability coefficient test, as can be seen from the data in comparative examples 1 to 4, after the polyvinyl alcohol, the glycerol and the citric acid are added, the moisture permeability coefficient of each guar film is gradually reduced due to the hydrophilicity of the hydroxyl groups, but the reduction is not large, and the moisture permeability coefficient of comparative example 4 is reduced by only 6% compared with that of comparative example 1. After the ginseng root extract is added, the moisture permeability coefficient of the guar-based nanocomposite film of each example is significantly lower than that of the guar film of the comparative example, and the guar-based nanocomposite film of example 1 shows the lowest moisture permeability coefficient.
In the free radical clearance test, after the ginseng root extract solution is added to each guar gum film, the free radical clearance is obviously improved, and the free radical clearance of the example 3 is improved by nearly 21.5 percent compared with that of the example 1. The guar based nanocomposite membranes of example 3 showed the best oxidation resistance.
According to the invention, after the polyvinyl alcohol, the glycerol and the citric acid are added into the guar gum, hydrogen bonds formed among molecules are beneficial to improving the mechanical strength and the barrier property of the membrane, the ginseng root extract solution can improve the free radical scavenging capacity of the guar gum base nano composite membrane, and the oxidation resistance of the guar gum base nano composite membrane is improved.
Secondly, the present invention determines the bacteriostatic ability of the guar gum based nanocomposite liquid prepared in step S3 of examples 1-3 by the bacteriostatic circle method.
Taking Escherichia coli and Staphylococcus aureus as experimental strains, pouring 20mL of nutrient agar on the culture medium, cooling, and mixing with 106CFU/mL bacterial suspension is evenly coated on the bacterial suspension. Then, the filter paper round piece cut into the diameter of 15mm is soaked in each guar gum base nano composite liquid for fully wetting for 10min, and is taken out and placed at the center of the culture medium. And taking out the culture medium after culturing for 24 hours in an incubator at 37 ℃, and accurately measuring the diameter of the inhibition zone. The bacteriostatic effect is shown in figure 1, and it can be seen from the figure that the bacteriostatic circle of the filter paper sheet soaked with each guar gum base nano-composite liquid is particularly obvious. It is also shown that in examples 1-3, the guar gum based nanocomposite fluid obtained after adding nano zinc oxide in step S3 shows significant inhibitory effects on both escherichia coli (e.coli) and staphylococcus aureus (s.au). (1-3 in the figure are guar-based nanocomposite liquids prepared in examples 1-3 in sequence)
A cross-sectional scanning electron microscope image of the guar gum based nano composite membrane prepared in example 1 is shown in fig. 2, the nano zinc oxide in the prepared guar gum based nano composite membrane does not have the phenomenon of large particle agglomeration, the dispersion is relatively uniform, and the bacteriostatic ability of the guar gum based nano composite membrane is well improved.
According to the invention, the guar gum is not subjected to complex modification operations such as oxidation, esterification, etherification and enzymatic degradation, complex and expensive equipment is not needed, the preparation process flow is simple, the reaction condition is mild, the guar gum is used as a film forming matrix, the polyvinyl alcohol is added to improve the film forming property, meanwhile, the high-activity component of the ginseng root extract solution is added to improve the oxidation resistance of the guar gum base nano composite film, and the nano zinc oxide is added to endow the guar gum base nano composite film with good bacteriostatic ability. The interaction of the raw materials in the guar gum base nano composite membrane can improve the mechanical property and the barrier property of the guar gum base nano composite membrane, and can disperse the nano zinc oxide in a mixed system to avoid aggregation to influence the antibacterial effect. The successful implementation of the preparation method is beneficial to expanding the application field of the guar gum base nano composite membrane as a food packaging material.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (8)
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