CN114409974A - Contains PEC, KGM and nano TiO2Antibacterial composite membrane and preparation method thereof - Google Patents

Contains PEC, KGM and nano TiO2Antibacterial composite membrane and preparation method thereof Download PDF

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CN114409974A
CN114409974A CN202111332950.0A CN202111332950A CN114409974A CN 114409974 A CN114409974 A CN 114409974A CN 202111332950 A CN202111332950 A CN 202111332950A CN 114409974 A CN114409974 A CN 114409974A
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kgm
pec
pectin
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composite membrane
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王楠
范丽萍
陈熠
崔伟怡
黄舒琦
李慧玲
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Jiaying University
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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
    • 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
    • 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
    • C08J2305/06—Pectin; Derivatives thereof
    • 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
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • 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
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/06—Pectin; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Abstract

The invention relates to the technical field of composite membranes, in particular to a composite membrane containing PEC, KGM and nano TiO2An antibacterial composite membrane containing PEC, KGM and TiO nanoparticles, and its preparing process2The antibacterial composite membrane is prepared from the following raw materials in percentage by weight: 0.6-1% of Pectin (PEC), 0.5-1.0% of Konjac Glucomannan (KGM), 0.5-0.7% of glycerol and nano TiO20.5-4.5%, and the balance of distilled water; the antibacterial composite membrane has excellent tensile property, high water vapor transmission rate and low oil transmission coefficient, can promote the water in the fresh meat to diffuse out, reduces the water content of the meat, and delays the decay of the meat; can also reduce flavor loss and block fatThe flavor of the fresh meat is maintained after the loss; the antibacterial composite membrane of the invention is added with nano TiO2Then, the mechanical property, the bacteriostatic activity, the barrier property and the like of the composite material are obviously improved; nano TiO 22Can inhibit the breeding of microorganisms on the surface of food, effectively make up the defects of the property of the PEC/KGM composite membrane, and strengthen the antibacterial action and the mechanical property of the PEC/KGM composite membrane.

Description

Contains PEC, KGM and nano TiO2Antibacterial composite membrane and preparation method thereof
Technical Field
The invention relates to the technical field of composite membranes, in particular to a composite membrane containing PEC, KGM and nano TiO2An antibacterial composite film and a preparation method thereof.
Background
Konjak Glucomannan (KGM) is a nonionic water-soluble high-molecular polysaccharide separated and extracted from natural plant konjak balls, has good thickening property, gelling property, cohesiveness and water absorption, and is widely applied to the food box food additive industry. Pectin (PEC) is a linear flexible macromolecule, the linear structure of the pectin can endow the membrane with the characteristics of flexibility and toughness, the pectin membrane has antibacterial property and degradability, and Konjac Glucomannan (KGM) and the Pectin (PEC) are blended to form an excellent thin film.
The KGM composite film forming is mainly used for fresh-keeping, film coating and fresh-keeping of fruits and vegetables, and is fresh on meat products. The cold fresh meat has the characteristics of rich nutrient substances and high water content, so that the cold fresh meat is extremely easy to decay in the shelf life. Researches find that the water content in fresh meat is higher, and when the water vapor transmission rate of the film is higher, the water in the fresh meat is promoted to be diffused out, the water content of the meat is reduced, and the deterioration of the meat is delayed; meanwhile, when the oil permeability coefficient of the film is lower, the loss of flavor substances and the loss of fat can be reduced, and the exchange of solutes can be regulated and controlled, so that the flavor of fresh meat is maintained.
The surface of the packaging film for packaging fruits, vegetables, meat and other nutrient-rich products at present is rich in nutrition, the conditions such as storage temperature, humidity and the like are also suitable for the growth of microorganisms, and the microorganisms stained on the surface of the packaging film are easy to migrate to the fruits, vegetables and meat, so that the fruits, vegetables and meat are accelerated to decay. Therefore, how to overcome the above technical problems and disadvantages is a problem to be solved.
Disclosure of Invention
The invention aims to overcome the defects described in the background technology, and provides a composite material containing PEC, KGM and nano TiO, which has high machine performance, high water vapor transmission rate, low oil transmission coefficient and antibacterial and bacteriostatic properties2An antibacterial composite film and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows: contains PEC, KGM and nano TiO2The antibacterial composite membrane is prepared from the following raw materials in percentage by weight: 0.6-1% of Pectin (PEC), 0.5-1.0% of Konjac Glucomannan (KGM), 0.5-0.7% of glycerol and nano TiO20.5-4.5% and the balance of distilled water.
Further, the material is prepared from the following raw materials in percentage by weight: 0.7-0.9% of Pectin (PEC), 0.6-0.9% of Konjac Glucomannan (KGM), 0.55-0.65% of glycerol and nano TiO21.5-3.5 percent, and the balance of distilled water.
Further, the material is prepared from the following raw materials in percentage by weight: pectin (PEC) 0.8%, Konjac Glucomannan (KGM) 0.75%, glycerol 0.6%, and nano TiO22.5 percent and the balance of distilled water.
Further, preparing a catalyst containing PEC, KGM and nano TiO2The preparation method of the antibacterial composite membrane comprises the following preparation steps:
(1) adding the distilled water in the amount of the components into a beaker, weighing the pectin in the amount of the components, and adding the pectin into the distilled water to prepare a pectin solution;
(2) adding the konjac glucomannan and the glycerol in the above amount into the pectin solution to form a PEC and KGM composite solution;
(3) adding the nano TiO into the PEC and KGM composite solution in the amount of the components2Stirring and uniformly mixing the mixture in an electric heating constant-temperature water tank at 60 ℃ by using a glass rod;
(4) stirring with a magnetic stirrer at 60 deg.C and 700r/min for 1.5h to form a uniform film-forming solution;
(5) placing the film-forming solution in an ultrasonic oscillator, and oscillating for 15min under the condition that the power is 100 w;
(6) spreading the oil absorption paper coated with glycerol in a culture dish, pouring the film-forming solution into the culture dish, wherein the thickness of the solution is 1.3-1.5cm, and drying in a forced air drying oven at 60 deg.C for 13-15 hr.
Further, when preparing the pectin solution in the step (1), the volume of distilled water is taken as a reference.
The invention contains PEC, KGM and nano TiO2The antibacterial composite membrane and the preparation method thereof have the beneficial effects that:
1. the invention contains PEC, KGM and nano TiO2The antibacterial composite film has excellent tensile property, high water vapor transmission rate and low oil transmission coefficient, is suitable for packaging fruits and vegetables and fresh meat, can promote the water in the fresh meat to diffuse out, reduces the water content of the meat, and delays the putrefaction of the meat; and the loss of flavor substances and the loss of fat can be reduced, and the exchange of solutes is regulated, so that the flavor of the fresh meat is maintained.
2. The invention contains PEC, KGM and nano TiO2The invention relates to an antibacterial composite membrane and a preparation method thereof, wherein nano TiO is added into the antibacterial composite membrane2Then, the mechanical property, the bacteriostatic activity, the barrier property and the like of the composite material are obviously improved; nano TiO 22Not only can inhibit the breeding of microorganisms on the surface of food, but also can keep good biocompatibility with human cells. The inorganic antibacterial agent can effectively make up the defects of PEC/KGM composite membrane performance, and can strengthen the antibacterial action and mechanical performance.
Drawings
FIG. 1 shows a PEC, KGM, nano TiO-containing composition of the present invention2An experimental result chart of the influence of the pectin content in the antibacterial composite membrane on the tensile degree;
FIG. 2 shows a PEC, KGM, nano TiO-containing composition of the present invention2An experimental result chart of the influence of the pectin content in the antibacterial composite membrane on the water vapor transmission coefficient;
FIG. 3 shows a PEC, KGM, nano-TiO-containing composition of the present invention2An experimental result chart of the influence of the pectin content in the antibacterial composite membrane on the oil permeability coefficient;
FIG. 4 shows a PEC, KGM, nano-TiO-containing composition of the present invention2An experimental result chart of the influence of the konjac glucomannan content in the antibacterial composite film on the tensile degree;
FIG. 5 shows a PEC-, KGM-and TiO-containing nanoparticle of the present invention2An experimental result chart of the influence of the konjac glucomannan content in the antibacterial composite film on the water vapor transmission coefficient;
FIG. 6 shows a PEC-, KGM-and TiO-containing nanoparticle of the present invention2An experimental result chart of the influence of the konjac glucomannan content in the antibacterial composite film on the oil penetration coefficient;
FIG. 7 shows a process for preparing a polymer containing PEC, KGM and TiO nanoparticles according to the present invention2An experimental result chart of the influence of the glycerol content in the antibacterial composite membrane on the tensile degree;
FIG. 8 shows a process for preparing a polymer containing PEC, KGM and nano-TiO according to the present invention2An experimental result chart of the influence of the glycerol content in the antibacterial composite membrane on the water vapor transmission coefficient;
FIG. 9 shows a PEC-, KGM-and TiO-containing nanoparticle of the present invention2An experimental result chart of the influence of the content of glycerol in the antibacterial composite membrane on the oil permeability coefficient;
FIG. 10 shows a PEC-, KGM-and TiO-containing nanoparticle of the present invention2TiO is added into the antibacterial composite film2Experimental result graphs of the effect of content on tensile strength;
FIG. 11 shows a PEC-, KGM-and TiO-containing nanoparticle of the present invention2TiO is added into the antibacterial composite film2An experimental result chart of the influence of the content on the water permeation quality;
FIG. 12 shows a PEC-, KGM-and TiO-containing nanoparticle of the present invention2TiO is added into the antibacterial composite film2An experimental result chart of the influence of the content on the oil permeability coefficient;
FIG. 13 shows a composition of the present invention comprising PEC, KGM, and TiO nanoparticles2No TiO is added in the antibacterial composite film2Experimental effect graph of the membrane of (1);
FIG. 14 shows a PEC-, KGM-and TiO-containing nanoparticle of the present invention2TiO is added into the antibacterial composite film2Experimental effect graph of the membrane of (1);
Detailed Description
Test items:
1. degree of tension
Cutting the film into strips of 100mm multiplied by 7mm, fixing the strips on a tensile tester, setting an initial clamp to be 80mm, and setting the tensile rate to be 1 mm/s; the tensile strength is calculated according to equation (1):
Figure RE-GDA0003477760720000041
in the formula: TS is tensile strength, MPa; f is the maximum tensile force borne by the film when the film is broken, and N is the maximum tensile force borne by the film when the film is broken; s is the cross-sectional area of the film, m2。
2. Measurement of Water vapor Transmission coefficient
Drying anhydrous calcium chloride in a 105 ℃ oven to constant weight, weighing 5g of the anhydrous calcium chloride, putting the anhydrous calcium chloride into a small conical flask, sealing the small conical flask by using a film, weighing and counting the anhydrous calcium chloride, putting the weighed anhydrous calcium chloride into a dryer with the bottom added with 1000mL of distilled water, taking out the anhydrous calcium chloride at a certain interval after balancing for 2 hours, weighing the anhydrous calcium chloride until the difference between the mass increment of the anhydrous calcium chloride and the mass increment of the anhydrous calcium chloride is not more than 5% of the initial weight, and ending the test. Calculating the water vapor transmission coefficient according to the formula (2)
Figure RE-GDA0003477760720000042
In the formula: WVP is the water vapor transmission coefficient, g.cm/cm2s.Pa; m is the water permeable mass, g; d is the film thickness, cm; s is the area of the film in cm2(ii) a T is time, s; p is the water vapor pressure difference Pa.
3. Determination of oil permeability coefficient
Putting 5mL camellia oil into a test tube, sealing the test tube with a film, inversely putting the test tube on filter paper, standing for 2 days, and weighing the change of the mass of the filter paper. And (4) calculating the oil permeability coefficient according to the formula (4).
Figure RE-GDA0003477760720000043
In the formula: PO is oil permeability coefficient, g.mm/m2D; delta W is the mass change of the filter paper, g; d is the thickness of the film, mm; s is the film area, T is the time, d.
Test examples
And (3) respectively detecting the influence of the addition amount of pectin, the addition amount of konjac glucomannan and the addition amount of glycerol on the performance of the film by adopting a single-factor test, wherein the performance research is tensile degree detection, water vapor transmission coefficient determination and oil penetration coefficient determination.
Test example 1
Effect of pectin addition on film Performance
Proportioning 1: the mass fractions of glycerol, konjac glucomannan and pectin are respectively 0.5%, 0.75% and 0.2%.
And (2) proportioning: the mass fraction of glycerol is 0.5%, the mass fraction of konjac glucomannan is 0.75%, and the mass fraction of pectin is 0.4%.
Proportioning 3: the mass fraction of glycerol is 0.5%, the mass fraction of konjac glucomannan is 0.75%, and the mass fraction of pectin is 0.6%.
And (4) proportioning: the mass fraction of glycerol is 0.5%, the mass fraction of konjac glucomannan is 0.75%, and the mass fraction of pectin is 0.8%.
And (2) proportioning 5: the mass fraction of glycerol is 0.5%, the mass fraction of konjac glucomannan is 0.75%, and the mass fraction of pectin is 1%.
The preparation methods of the formula 1 to the formula 5 are as follows:
(1) adding the distilled water in the amount of the components into a beaker, weighing the pectin in the amount of the components, and adding the pectin into the distilled water to prepare a pectin solution;
(2) adding the konjac glucomannan and the glycerol in the above amount into the pectin solution to form a PEC and KGM composite solution; stirring and uniformly mixing the mixture in an electric heating constant-temperature water tank at 60 ℃ by using a glass rod;
(3) stirring with a magnetic stirrer at 60 deg.C and 700r/min for 1.5h to form a uniform film-forming solution;
(4) placing the film-forming solution in an ultrasonic oscillator, and oscillating for 15min under the condition that the power is 100 w;
(5) spreading the oil absorption paper coated with glycerol in a culture dish, pouring the film-forming solution into the culture dish, wherein the thickness of the solution is 1.3-1.5cm, and drying in a forced air drying oven at 60 deg.C for 13-15 hr.
The detection results are shown in fig. 1, 2 and 3:
from the data shown in fig. 1, 2 and 3, when the pectin content is 0.6-1.0%, the tensile strength is 40-110G, the water vapor transmission quality is 0.1-0.5G, the water vapor transmission coefficient is proportional to the water vapor transmission quality, and the oil transmission coefficient is 100-700, it can be seen that when the pectin content is 0.8%, the tensile strength is higher, the water vapor transmission quality is the largest, the water vapor transmission coefficient is the largest, and the oil transmission coefficient is the smallest, and the composite membrane has the best performance.
Test example 2
Effect of addition amount of Konjac glucomannan on film performance
Proportioning 6: the mass fraction of glycerol is 0.5%, the mass fraction of pectin is 0.6%, and the mass fraction of konjac glucomannan is 0.25%.
Proportioning 7: the mass fraction of glycerol is 0.5%, the mass fraction of pectin is 0.6%, and the mass fraction of konjac glucomannan is 0.5%.
Proportioning 8: the mass fraction of glycerol is 0.5%, the mass fraction of pectin is 0.6%, and the mass fraction of konjac glucomannan is 0.75%.
Proportioning 9: the mass fraction of glycerol is 0.5%, the mass fraction of pectin is 0.6%, and the mass fraction of konjac glucomannan is 1%.
The mixture ratio is 10: the mass fraction of glycerol is 0.5%, the mass fraction of pectin is 0.6%, and the mass fraction of konjac glucomannan is 1.25%.
The preparation method is the same as formula 1 and is not described herein again.
The detection results are shown in fig. 4, 5 and 6.
As can be seen from fig. 4, 5 and 6, when the konjac glucomannan content is 0.5% -1.0%, the tensile strength is 90-110G, the water vapor transmission quality is 0.25-0.5G, the water vapor transmission coefficient is proportional to the water vapor transmission quality, and the oil transmission coefficient is 200-0, and from the above data, when the konjac glucomannan content is 0.75%, the tensile strength is the largest, the water vapor transmission quality is the largest, the water vapor transmission coefficient is the largest, and the oil transmission coefficient is the smallest, and the performance of the composite film is the best.
Test example 3
Effect of Glycerol addition on film Performance
Proportioning 11: the mass fraction of pectin is 0.6%, the mass fraction of konjac glucomannan is 0.75%, and the mass fraction of glycerol is 0.3%.
Proportioning 12: the mass fraction of pectin is 0.6%, the mass fraction of konjac glucomannan is 0.75%, and the mass fraction of glycerol is 0.4%.
Proportioning 13: the mass fraction of pectin is 0.6%, the mass fraction of konjac glucomannan is 0.75%, and the mass fraction of glycerol is 0.5%.
Proportioning 14: the mass fraction of pectin is 0.6%, the mass fraction of konjac glucomannan is 0.75%, and the mass fraction of glycerol is 0.6%.
Proportioning 15: the mass fraction of pectin is 0.6%, the mass fraction of konjac glucomannan is 0.75%, and the mass fraction of glycerol is 0.7%.
The preparation method is the same as formula 1 and is not described herein again.
The detection results are shown in fig. 7, 8 and 9.
As can be seen from fig. 7, 8 and 9, when the glycerin content is 0.5% to 0.7%, the tensile strength is 30 to 50G, the water vapor transmission mass is 0.08 to 0.3G, the water vapor transmission coefficient is proportional to the water vapor transmission mass, and the oil transmission coefficient is 190 to 160, it can be seen from the above data that when the glycerin content is 0.6%, the tensile strength is high, the water vapor transmission mass is high, the water vapor transmission coefficient is high, and the oil transmission coefficient is low, and the performance of the composite membrane is the best.
In summary, based on the single-factor test, we find that, when the pectin content is 0.6% -1.0%, the tensile strength is higher, the water vapor permeability coefficient is lower, and the oil permeability coefficient is higher; the konjac glucomannan content is 0.5-1.0%, and the konjac glucomannan has higher tensile strength, lower water vapor transmission coefficient and higher oil transmission coefficient; the glycerol content is as follows: 0.5-0.7%, high tensile strength, low water vapor permeability coefficient and high oil permeability coefficient; especially, when the mass fraction of the glycerol is 0.6 percent, the mass fraction of the konjac glucomannan is 0.75 percent, and the mass fraction of the pectin is 0.8 percent, all the performances can reach better physicochemical performances.
Experimental example 2
And (3) detecting the influence of the addition of the titanium dioxide on various performances of the film by adopting a single-factor test. The measurement items are the tensile strength measurement, the water vapor permeability measurement, and the oil permeability measurement.
The nano titanium dioxide decomposes bacteria under the photocatalysis to achieve the antibacterial effect. The electronic structure of the nano titanium dioxide is characterized by being full of TiO2And a vacant conduction band, in a system of water and air, the nano titanium dioxide is irradiated by sunlight, especially ultraviolet rays, when the electron energy reaches or exceeds the band gap energy. Electrons can be excited from a valence band to a conduction band, corresponding holes are generated in the valence band, namely electron and hole pairs are generated, under the action of an electric field, the electrons and the holes are separated and migrate to different positions on the surface of particles to generate a series of reactions, and the reactions are adsorbed and dissolved in TiO2Oxygen-trapped electron formation of O at the surface2The superoxide anion radical formed reacts with most organic species. Simultaneously can react with organic matters in bacteria to generate CO2And H2O; and eventually cause the bacteria to break down.
The nano titanium dioxide has the antibacterial characteristics that: is safe and nontoxic to human bodies and has no irritation to skin; the antibacterial ability is strong, and the antibacterial range is wide; no odor, strange odor and small smell; the product is water-fast and has long storage period; the thermal stability is good, and the color is not changed, decomposed, volatilized and deteriorated at high temperature; the instantaneity is good, the nano titanium dioxide antibacterial agent can exert the effect only within 1 hour, and the effect of other antibacterial agents is about 24 hours; the nano titanium dioxide is an antibacterial agent for permanently maintaining the antibacterial effect; has good safety, can be used as food additive, etc., and has no adverse effect when in contact with skin.
According to the existing research, the method comprises the following steps: the nanometer titanium dioxide does not influence the proliferation and apoptosis activity of normal cells; moreover, the influence of the nano titanium dioxide on the main organ structure and the oxidative stress level of the animal body has a certain relation with the administration mode, the grain diameter and the crystal form. The results of cell experiments and animal experiments are integrated, and the nano titanium dioxide has good biocompatibility within a certain time and concentration range.
The specific formula is as follows:
formula 1: the mass fraction of glycerol is 0.6%, the mass fraction of konjac glucomannan is 0.75%, the mass fraction of pectin is 0.8%, and the mass fraction of titanium dioxide is 0.5%.
And (2) formula: the mass fraction of glycerol is 0.6%, the mass fraction of konjac glucomannan is 0.75%, the mass fraction of pectin is 0.8%, and the mass fraction of titanium dioxide is 1.5%.
And (3) formula: the mass fraction of glycerol is 0.6%, the mass fraction of konjac glucomannan is 0.75%, the mass fraction of pectin is 0.8%, and the mass fraction of titanium dioxide is 2.5%.
And (4) formula: the mass fraction of glycerol is 0.6%, the mass fraction of konjac glucomannan is 0.75%, the mass fraction of pectin is 0.8%, and the mass fraction of titanium dioxide is 3.5%.
And (5) formula: the mass fraction of glycerol is 0.6%, the mass fraction of konjac glucomannan is 0.75%, the mass fraction of pectin is 0.8%, and the mass fraction of titanium dioxide is 4.5%.
The preparation methods of formulations 1 to 5 are as follows:
1. adding distilled water in the amount of the components into a beaker, then weighing pectin with the mass fraction of 0.8 percent, adding the pectin into the distilled water, and preparing a pectin solution;
2. adding konjac glucomannan with the mass fraction of 0.75% and glycerol with the mass fraction of 0.6% into the pectin solution to form a PEC and KGM composite solution;
3. adding the nano TiO into the PEC and KGM composite solution in the amount of the components2Stirring and uniformly mixing the mixture in an electric heating constant-temperature water tank at 60 ℃ by using a glass rod;
4. stirring with a magnetic stirrer at 60 deg.C and 700r/min for 1.5h to form a uniform film-forming solution;
5. placing the film-forming solution in an ultrasonic oscillator, and oscillating for 15min under the condition that the power is 100 w;
6. spreading the oil absorption paper coated with glycerol in a culture dish, pouring the film-forming solution into the culture dish, wherein the thickness of the solution is 1.3-1.5cm, and drying in a forced air drying oven at 60 deg.C for 13-15 hr.
The detection results are shown in fig. 10, 11 and 12.
As can be seen from a combination of FIGS. 10, 11 and 12, when TiO is used2The content is 1.5-3.5%, the tensile strength is 70-170G, the water vapor transmission quality is 0.4-0.55G, the water vapor transmission coefficient is in direct proportion to the water vapor transmission quality, and the oil transmission coefficient is 35-80.
Comparing the data with the data in FIGS. 1-9, it was found that TiO was added2The tensile property and the water vapor transmission quality of the composite membrane are greatly improved, and the fluctuation range of the oil permeability coefficient is small and is not more than 100. When the above data are combined, the TiO compound is used2When the content is 0.25%, the tensile strength is high, the water vapor transmission quality is high, the water vapor transmission coefficient is high, and the oil transmission coefficient is low, so that the performance of the composite membrane is best.
Experimental example 3
And (3) detecting the determination of the antibacterial performance of the film by using a single-factor test.
Detection method
Firstly, in the experiment, escherichia coli is used as a test strain, a certain amount of composite membrane is crushed into fragments and added into an escherichia coli suspension, a colony group experiment is carried out after 24 hours of culture, and the number of colony groups is counted.
Secondly, preparing LB culture medium by taking escherichia coli as a test strain in the experiment, and smearing TiO-containing bacteria liquid2The membrane is punched into a sheet with the diameter of two centimeters by a puncher, the sheet is placed in a culture dish coated with bacterial liquid, and the culture dish is placed in an incubator for 24 hours and then observed.
The results are shown in Table 1:
table 1: detection result of titanium dioxide addition amount to antibacterial performance measurement of film
Figure RE-GDA0003477760720000081
Figure RE-GDA0003477760720000091
The experimental effects are shown in fig. 13 and 14:
as can be seen from the experiments, TiO was added at different concentrations2The antibacterial film has stronger inhibition effect on different pathogenic bacteria, along with TiO2The inhibition effect of the content increase on different pathogenic bacteria is continuously strengthened, and no pathogenic bacteria grow in the place of the antibacterial membrane cover.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The use of the terms "a" or "an" and the like in the description and in the claims of this application do not necessarily denote a limitation of quantity. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items. The terms "connected" or "coupled" and the like are not restricted to physical or mechanical connections, but may include electrical connections, whether direct or indirect.
Exemplary embodiments of the present invention have been described in detail with reference to the preferred embodiments, however, it will be understood by those skilled in the art that various changes and modifications may be made to the specific embodiments described above, and various combinations of the technical features and structures proposed by the present invention may be made without departing from the concept of the present invention.

Claims (5)

1. Contains PEC, KGM and nano TiO2Antibiotic complex film, its characterized in that: the material is prepared from the following raw materials in percentage by weight: 0.6-1% of Pectin (PEC), 0.5-1.0% of Konjac Glucomannan (KGM), 0.5-0.7% of glycerol and nano TiO20.5-4.5% and the balance of distilled water.
2. The PEC, KGM, nano-TiO-containing material of claim 12Antibiotic complex film, its characterized in that: the material is prepared from the following raw materials in percentage by weight: 0.7-0.9% of Pectin (PEC), 0.6-0.9% of Konjac Glucomannan (KGM), 0.55-0.65% of glycerol and nano TiO21.5-3.5 percent, and the balance of distilled water.
3. The PEC, KGM, nano-TiO-containing composition of claim 22The antibacterial composite membrane and the preparation method thereof are characterized in that: the material is prepared from the following raw materials in percentage by weight: pectin (PEC) 0.8%, Konjac Glucomannan (KGM) 0.75%, glycerol 0.6%, and nano TiO22.5 percent and the balance of distilled water.
4. Preparation of a PEC-, KGM-or TiO-containing nanoparticle according to any of claims 1 to 32The preparation method of the antibacterial composite membrane is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
(1) adding the distilled water in the amount of the components into a beaker, weighing the pectin in the amount of the components, and adding the pectin into the distilled water to prepare a pectin solution;
(2) adding the konjac glucomannan and the glycerol in the above amount into the pectin solution to form a PEC and KGM composite solution;
(3) adding the nano TiO into the PEC and KGM composite solution in the amount of the components2Stirring and uniformly mixing the mixture in an electric heating constant-temperature water tank at 60 ℃ by using a glass rod;
(4) stirring with a magnetic stirrer at 60 deg.C and 700r/min for 1.5h to form a uniform film-forming solution;
(5) placing the film-forming solution in an ultrasonic oscillator, and oscillating for 15min under the condition that the power is 100 w;
(6) spreading the oil absorption paper coated with glycerol in a culture dish, pouring the film-forming solution into the culture dish, wherein the thickness of the solution is 1.3-1.5cm, and drying in a forced air drying oven at 60 deg.C for 13-15 hr.
5. The PEC, KGM, nano-TiO-containing material of claim 42Antibacterial composite film and preparation method thereofThe method is characterized in that: and (2) when the pectin solution is prepared in the step (1), taking the volume of distilled water as a reference.
CN202111332950.0A 2021-11-11 2021-11-11 Contains PEC, KGM and nano TiO2Antibacterial composite membrane and preparation method thereof Pending CN114409974A (en)

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