AU2020103921A4 - Antibacterial compound fiber film, method for preparing the same and application thereof - Google Patents

Antibacterial compound fiber film, method for preparing the same and application thereof Download PDF

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AU2020103921A4
AU2020103921A4 AU2020103921A AU2020103921A AU2020103921A4 AU 2020103921 A4 AU2020103921 A4 AU 2020103921A4 AU 2020103921 A AU2020103921 A AU 2020103921A AU 2020103921 A AU2020103921 A AU 2020103921A AU 2020103921 A4 AU2020103921 A4 AU 2020103921A4
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antibacterial
parts
solution
fiber film
compound fiber
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AU2020103921A
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Jundong Chen
Lan CHENG
Xinxin HU
Yalan Jiang
Jingman Li
Yan Li
Yaowen LIU
Yihao WANG
Xinyi WU
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Sichuan Agricultural University
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Sichuan Agricultural University
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    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005Synthetic yarns or filaments
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/13Physical properties anti-allergenic or anti-bacterial
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2505/00Industrial
    • D10B2505/10Packaging, e.g. bags

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Medicinal Preparation (AREA)

Abstract

The application relates to the technical field of compound materials, and discloses an antibacterial compound fiber film, which comprises 2-3 parts of antibacterial microcapsule, 5-7 parts of cassava starch, 1-2 parts of glycerol, 6 parts of gelatin, and 5 100 parts of deionized water by weight; a method for preparing the antibacterial microcapsule comprises the following steps: Si: taking and mixing Cymbopogon citrates essential oil with ethyl acetate for dissolution to obtain mixed solution; S2: taking and mixing p-cyclodextrin with deionized water for dissolution to obtain oversaturated solution; S3: adding the mixed solution into the oversaturated solution, 10 and sequentially performing magnetic stirring, freeze thawing and suction filtration to obtain a precipitate; S4: drying the precipitate to constant weight to obtain the antibacterial microcapsule. In the application, the Cymbopogon citrates essential oil is prepared into the antibacterial microcapsule by adopting a p-cyclodextrin embedding method, then mixing is performed to obtain spinning solution by using the cassava 15 starch as a film forming matrix, the glycerol as a plasticizer and the gelatin as a enhancer, and then the antibacterial compound fiber film is prepared by adopting an electrospinning technology, which achieves the effects of bacteria inhibition, insect prevention, long-time acting, environmental friendliness and high safety.

Description

ANTIBACTERIAL COMPOUND FIBER FILM, METHOD FOR PREPARING THE SAME AND APPLICATION THEREOF
Technical Field
The application relates to the technical field of compound films, in particular to an
antibacterial compound fiber film, a method for preparing the same and application
thereof.
Background Art
In recent years, with the improvement of quality of life, people pay more and more
attention to food quality and food safety. With the professional development of
agricultural production, the long-distance transportation of fresh fruits and vegetables
is becoming more and more common. As fresh fruits and vegetables are fresh food
with high water content, they still have life characteristics after picked and can
continue to breathe, accompanied by processes such as metabolism, water evaporation
and ethylene production, which promote the further maturity of fruits and vegetables.
Therefore, the fresh keeping of fruits and vegetables is particularly important.
Preservative film is a kind of film to keep food fresh, mainly by preventing the
migration of substances such as dust, moisture, gas and solute to prevent the change in
aspects such as food flavor and texture, so as to ensure the quality of food and extend
the shelf life of food. At present, the commonly used preservative film in the prior art
is common polyethylene (PE) film, which can block dust and bacteria in the air.
However, bacteria adsorbed on the surfaces of fruits and vegetables will grow and
propagate in a short time, which will promote the migration of the bacteria and their
secretions, resulting in the deterioration of fruits and vegetables. Moreover, for fruits
and vegetables with mechanical damages, it is more likely to cause the breeding of
microbes and thus leads to the decay and deterioration of fruits and vegetables. In
addition, since this kind of preservative film is a chemically synthesized polymer material, there are certain hidden dangers. Therefore, environment-friendly and safe preservative films which are able to solve the problem of microbial contamination have become a research hotspot.
Starch is considered as one of the most promising biodegradable packaging materials. A starch film made after gelatinization, coagulation and drying has the advantages of good tensile properties and high transparency. A number of studies have shown that the antibacterial properties of starch films can be improved by adopting a compounding method.
Chinese patent literature CN201810424640.3 (application date: 20180507), titled "Environmentally-friendly Preservative Film Capable of Enhancing Banana Freshness Retaining Effect and Preparation Method of Environmentally-Friendly Preservative Film", has disclosed a preservative film, which includes the following raw materials in parts by weight: 36-40 parts of ABS resin, 32-36 parts of modified potato starch, 8-14 parts of pre-gel starch, 4-8 parts of antibacterial enhancers, 1-3 parts of compound plant essential oil, 6-10 parts of methacrylate-methacrylic acid copolymer, and 18-24 parts of propylene glycol diacetate.
By using the ABS resin and the modified potato starch as the main base material, modifying by using organic acid and adding mica powder and compound plant essential oil, the effect of improving the viscosity and antibacterial properties of starch is achieved. However, since the essential oil is directly added into the film forming matrix in this compounding method and the essential oil has the features of insolubility in water, poor compatibility with polar packaging materials, strong volatility and oxidizability, and high sensitivity to temperature and light, resulting in low stability, such that a long-term antibacterial effect cannot be achieved by packaging films.
Therefore, we urgently need a kind of preservative film which can inhibit bacteria, prevent insects and act for a long time, and is environment-friendly and safe.
Summary
The first purpose of the application is to overcome the defects of the prior art and
provide an antibacterial compound fiber film, which at least can achieve the effects of
bacteria inhibition, insect prevention, long-time acting, environmental friendliness and
high safety.
The purpose is achieved by adopting the following technical solution: an antibacterial
compound fiber film includes 2-3 parts of antibacterial microcapsule, 5-7 parts of
cassava starch, 1-2 parts of glycerol, 6 parts of gelatin, and 100 parts of deionized
water by weight.
As a further optimized solution, the antibacterial compound fiber film includes 3 parts
of antibacterial microcapsule, 7 parts of cassava starch, 2 parts of glycerol, 6 parts of
gelatin, and 100 parts of deionized water by weight.
As a further optimized solution, the weight of the glycerol is 2g and the weight of the
gelatin is 6g.
As a further optimized solution, a method for preparing the antibacterial microcapsule
includes the following steps:
Si: taking and mixing Cymbopogon citrates essential oil with ethyl acetate for
dissolution to obtain mixed solution;
S2: taking and mixing p-cyclodextrin with deionized water for dissolution to obtain
oversaturated solution;
S3: adding the mixed solution into the oversaturated solution, and sequentially
performing magnetic stirring, freeze thawing and suction filtration to obtain a
precipitate;
S4: heating and drying the precipitate to constant weight to obtain the antibacterial
microcapsule.
Through the above technical solution, by adding the Cymbopogon citrates essential
oil, citral and citronellal components therein can be used to destroy the cell
membranes and cell walls of microbes, thus changing the selective permeability of the cell membranes of microbes, inhibiting the breeding and growth of microbes and causing microbes to die.
As a further optimized solution, the volume ratio of Cymbopogon citrates essential oil to ethyl acetate is 1:4-6; and/or, the volume ratio of the supersaturated solution to the mixed solution is 8-10:1.
Through the above technical solution, by limiting the volume ratio of Cymbopogon citrates essential oil to ethyl acetate and the volume ratio of the supersaturated solution to the mixed solution, the effect of improving the embedding rate is achieved.
As a further optimized solution, in S3, the temperature of magnetic stirring is 60-80°C, and the time is 120min; and/or, the temperature of freeze thawing is -18°C, and the time is 4h.
As a further optimized solution, in S4, the temperature of heating and drying is 50°C.
The second purpose of the application is to provide a method for preparing the antibacterial compound fiber film.
The purpose is achieved by adopting the following technical solution: a method for preparing the antibacterial compound fiber film includes the following steps:
S5: weighing the antibacterial microcapsule, the cassava starch, the glycerol, the gelatin and the deionized water according to proportions;
S6: dissolving the cassava starch in the deionized water for gelatinization to obtain gelatinized starch solution;
S7: taking and uniformly mixing the glycerol, the gelatin and the gelatinized starch solution, performing cooling, and adding the antibacterial microcapsule to obtain spinning solution;
S8: performing electrospinning by using the spinning solution to obtain the antibacterial compound fiber film.
As a further optimized solution, in S6, the temperature of gelatinization is 100°C, and the time is 30min.
As a further optimized solution, the specification of a syringe for the electrospinning
is 1Oml.
As a further optimized solution, in S8, the conditions for electrospinning are as
follows: electric field intensity: 18kv/cm, distance: 15cm, speed: 0.2ml/h, time: 12h.
The third purpose of the application is to provide application of the antibacterial
compound fiber film to fresh keeping of fruits and vegetables.
It is worth noting that, in the application, by using the p-cyclodextrin embedding
method to prepare the antibacterial microcapsule from the Cymbopogon citrates
essential oil, and changing the liquid essential oil antibacterial agent into powder that
can flow freely, the bacteria can be inhibited and the insects can be prevented;
moreover, since the Cymbopogon citrates essential oil is encapsulated in the
p-cyclodextrin such fine particles are formed, the surrounding p-cyclodextrin acts as a protective film to resist the influence of external light and temperature on the essential
oil, thus the volatility of the essential oil is reduced, the stability of the essential oil is
improved, and a slow-release effect is achieved. Further, the stability can be improved
and the slow-release effect can be achieved. Finally, by using the cassava starch as a
film forming matrix, the glycerol as a plasticizer and the gelatin as an enhancer,
mixing with the antibacterial microcapsule is performed to obtain the spinning
solution, and finally the antibacterial compound fiber film is prepared by adopting an
electrospinning technology, such that the release speed of the Cymbopogon citrates
essential oil can be further slowed down and the slow-release effect is enhanced. In
addition, all raw materials are selected from natural substances, which are safe and
non-toxic.
The application has the following beneficial effects:
1. In the method for preparing the antibacterial compound fiber film provided by the
application, the Cymbopogon citrates essential oil is prepared into the antibacterial
microcapsule by adopting a p-cyclodextrin embedding method, then mixing is performed to obtain spinning solution by using the cassava starch as a film forming matrix, the glycerol as a plasticizer and the gelatin as an enhancer, and then the antibacterial compound fiber film is prepared by adopting an electrospinning technology, which achieves the effects of bacteria inhibition, insect prevention, long-time acting, environmental friendliness and high safety.
2. The antibacterial compound fiber film provided by the application can effectively
inhibit Escherichia coli and Staphylococcus aureus, and has a wide antibacterial
spectrum.
Description of the Embodiments
The technical solution of the application will be further described below in detail.
However, the scope of protection of the application is not limited to what described
below.
Example 1
A method for preparing an antibacterial compound fiber film included the following
steps:
1) Preparation of antibacterial microcapsule
Al: mixing Cymbopogon citrates essential oil with ethyl acetate for dissolution
according to 1:4 (v:v) to obtain mixed solution;
A2: mixing p-cyclodextrin with deionized water for dissolution to obtain oversaturated solution;
A3: mixing the mixed solution with the oversaturated solution according 1:10 (v:v),
performing magnetic stirring for 120min at 60°C, then performing freeze thawing for
4h at -18°C, and performing suction filtration to obtain a precipitate;
A4: heating and drying the precipitate to constant weight at 50°C to obtain an
antibacterial microcapsule.
2) Preparation of antibacterial compound fiber film:
BI: weighing 3g of antibacterial microcapsule, 7g of cassava starch, 2g of glycerol
and 6g of gelatin, and taking 100ml of deionized water;
B2: mixing the cassava starch with the deionized water, performing stirring for 20min,
performing heating to 100C, and performing gelatinization for 30min to obtain
gelatinized starch solution;
B3: adding 2g of glycerol and 6g of gelatin into the gelatinized starch solution,
performing stirring for 15min, performing cooling to 40C, adding the antibacterial
microcapsule, and performing uniform stirring to obtain spinning solution;
B4: filling the spinning solution into a 10ml syringe, keeping an included angle
between the syringe and a horizontal line to be 18, using an aluminum foil as a
negative pole collector of nanofibers, using a conducting wire as a positive pole, and
connecting the conducting wire to a metal needle of the syringe; controlling electric
field intensity to be 18kv/cm, distance to be 15cm and speed to be 0.2mh, enabling
the spinning solution to be sprayed from the needle tip of the syringe under the joint
effect of gravity and electric field to form nanofibers, and gradually collecting the
nanofibers on the negative pole collector to obtain an antibacterial compound fiber
film after 12h.
Example 2
A method for preparing an antibacterial compound fiber film included the following
steps:
1) Preparation of antibacterial microcapsule
Al: mixing Cymbopogon citrates essential oil with ethyl acetate for dissolution
according to 1:4 (v:v) to obtain mixed solution;
A2: mixing p-cyclodextrin with deionized water for dissolution to obtain oversaturated solution;
A3: mixing the mixed solution with the oversaturated solution according 1:10 (v:v),
performing magnetic stirring for 120min at 60C, then performing freeze thawing for
4h at -18°C, and performing suction filtration to obtain a precipitate;
A4: heating and drying the precipitate to constant weight at 50°C to obtain an
antibacterial microcapsule.
2) Preparation of antibacterial compound fiber film:
B1: weighing 2g of antibacterial microcapsule, 7g of cassava starch, 2g of glycerol
and 6g of gelatin, and taking 100ml of deionized water;
B2: mixing the cassava starch with the deionized water, performing stirring for 20min,
performing heating to 100C, and performing gelatinization for 30min to obtain
gelatinized starch solution;
B3: adding the glycerol and the gelatin into the gelatinized starch solution, performing
stirring for 15min, performing cooling to 40C, adding the antibacterial microcapsule,
and performing uniform stirring to obtain spinning solution;
B4: filling the spinning solution into a 10ml syringe, keeping an included angle
between the syringe and a horizontal line to be 18, using an aluminum foil as a
negative pole collector of nanofibers, using a conducting wire as a positive pole, and
connecting the conducting wire to a metal needle of the syringe; controlling electric
field intensity to be 18kv/cm, distance to be 15cm and speed to be 0.2mh, enabling
the spinning solution to be sprayed from the needle tip of the syringe under the joint
effect of gravity and electric field to form nanofibers, and gradually collecting the
nanofibers on the negative pole collector to obtain an antibacterial compound fiber
film after 12h.
Example 3
A method for preparing an antibacterial compound fiber film included the following
steps:
1) Preparation of antibacterial microcapsule
Al: mixing Cymbopogon citrates essential oil with ethyl acetate for dissolution according to 1:4 (v:v) to obtain mixed solution;
A2: mixing p-cyclodextrin with deionized water for dissolution to obtain oversaturated solution;
A3: mixing the mixed solution with the oversaturated solution according 1:10 (v:v), performing magnetic stirring for 120min at 60C, then performing freeze thawing for
4h at -18°C, and performing suction filtration to obtain a precipitate;
A4: heating and drying the precipitate to constant weight at 50C to obtain an
antibacterial microcapsule.
2) Preparation of antibacterial compound fiber film:
BI: weighing 2g of antibacterial microcapsule, 5g of cassava starch, 2g of glycerol
and 6g of gelatin, and taking 100ml of deionized water;
B2: mixing the cassava starch with the deionized water, performing stirring for 20min,
performing heating to 100C, and performing gelatinization for 30min to obtain
gelatinized starch solution;
B3: adding the glycerol and the gelatin into the gelatinized starch solution, performing
stirring for 15min, performing cooling to 40C, adding the antibacterial microcapsule,
and performing uniform stirring to obtain spinning solution;
B4: filling the spinning solution into a 10ml syringe, keeping an included angle
between the syringe and a horizontal line to be 18, using an aluminum foil as a
negative pole collector of nanofibers, using a conducting wire as a positive pole, and
connecting the conducting wire to a metal needle of the syringe; controlling electric
field intensity to be 18kv/cm, distance to be 15cm and speed to be 0.2mh, enabling
the spinning solution to be sprayed from the needle tip of the syringe under the joint
effect of gravity and electric field to form nanofibers, and gradually collecting the
nanofibers on the negative pole collector to obtain an antibacterial compound fiber
film after 12h.
Example 4
A method for preparing an antibacterial compound fiber film included the following steps:
1) Preparation of antibacterial microcapsule
Al: mixing Cymbopogon citrates essential oil with ethyl acetate for dissolution according to 1:4 (v:v) to obtain mixed solution;
A2: mixing p-cyclodextrin with deionized water for dissolution to obtain oversaturatedsolution;
A3: mixing the mixed solution with the oversaturated solution according 1:10 (v:v), performing magnetic stirring for 120min at 60C, then performing freeze thawing for 4h at -18°C, and performing suction filtration to obtain a precipitate;
A4: heating and drying the precipitate to constant weight at 50C to obtain an antibacterial microcapsule.
2) Preparation of antibacterial compound fiber film:
B1: weighing 2g of antibacterial microcapsule, 7g of cassava starch, 1g of glycerol and 6g of gelatin, and taking 100ml of deionized water;
B2: mixing the cassava starch with the deionized water, performing stirring for 20min, performing heating to 100C, and performing gelatinization for 30min to obtain gelatinized starch solution;
B3: adding the glycerol and the gelatin into the gelatinized starch solution, performing stirring for 15min, performing cooling to 40C, adding the antibacterial microcapsule, and performing uniform stirring to obtain spinning solution;
B4: filling the spinning solution into a 10ml syringe, keeping an included angle between the syringe and a horizontal line to be 18, using an aluminum foil as a negative pole collector of nanofibers, using a conducting wire as a positive pole, and connecting the conducting wire to a metal needle of the syringe; controlling electric field intensity to be 18kv/cm, distance to be 15cm and speed to be 0.2mh, enabling the spinning solution to be sprayed from the needle tip of the syringe under the joint effect of gravity and electric field to form nanofibers, and gradually collecting the nanofibers on the negative pole collector to obtain an antibacterial compound fiber film after 12h.
Example 5
A method for preparing an antibacterial compound fiber film included the following
steps:
1) Preparation of antibacterial microcapsule
Al: mixing Cymbopogon citrates essential oil with ethyl acetate for dissolution
according to 1:4 (v:v) to obtain mixed solution;
A2: mixing p-cyclodextrin with deionized water for dissolution to obtain oversaturatedsolution;
A3: mixing the mixed solution with the oversaturated solution according 1:10 (v:v),
performing magnetic stirring for 120min at 60C, then performing freeze thawing for
4h at -18°C, and performing suction filtration to obtain a precipitate;
A4: heating and drying the precipitate to constant weight at 50C to obtain an
antibacterial microcapsule.
2) Preparation of antibacterial compound fiber film:
BI: weighing 3g of antibacterial microcapsule, 7g of cassava starch, Ig of glycerol
and 6g of gelatin, and taking 100ml of deionized water;
B2: mixing the cassava starch with the deionized water, performing stirring for 20min,
performing heating to 100C, and performing gelatinization for 30min to obtain
gelatinized starch solution;
B3: adding the glycerol and the gelatin into the gelatinized starch solution, performing
stirring for 15min, performing cooling to 40C, adding the antibacterial microcapsule,
and performing uniform stirring to obtain spinning solution;
B4: filling the spinning solution into a 10ml syringe, keeping an included angle
between the syringe and a horizontal line to be 18, using an aluminum foil as a
negative pole collector of nanofibers, using a conducting wire as a positive pole, and
connecting the conducting wire to a metal needle of the syringe; controlling electric
field intensity to be 18kv/cm, distance to be 15cm and speed to be 0.2mh, enabling
the spinning solution to be sprayed from the needle tip of the syringe under the joint
effect of gravity and electric field to form nanofibers, and gradually collecting the
nanofibers on the negative pole collector to obtain an antibacterial compound fiber
film after 12h.
Comparative example 1
The method in example 1 of the application was adopted for making a comparison
with comparative example 1. In comparative example 1, Cymbopogon citrates
essential oil was not added; other conditions such as the use amounts and steps were
the same as that in example 1 of the application (compared with example 1, in
comparative example 1, Cymbopogon citrates essential oil was not added, for the
purpose of proving that the effect of the compound fiber film of the application was
better).
Comparative example 2
The method in example 1 of the application was adopted for making a comparison
with comparative example 2. The method in comparative example 2 was as follows:
step 1) was not included; in B2 of step 2), glycerol, gelatin and Cymbopogon citrates
essential oil were added into the gelatinized starch solution, and uniform stirring was
performed to obtain mixed solution; in B4 of step 2), tape casting was performed to
the mixed solution on a glass plate, and drying was performed to obtain a preservative
film; other conditions such as the use amounts and steps were the same as that in
example 1 of the application (compared with example 1, in comparative example 2,
Cymbopogon citrates essential oil was not prepared into the antibacterial
microcapsule and the electrospinning technology was not adopted, for the purpose of proving that the effect of the compound fiber film of the application was better).
Comparative example 3
The method in example 1 of the application was adopted for making a comparison
with comparative example 3. The method in comparative example 3 was as follows:
step 1) was not included; in B2 of step 2), glycerol, gelatin and Cymbopogon citrates
essential oil were added into the gelatinized starch solution, and uniform stirring was
performed to obtain spinning solution; other conditions such as the use amounts and
steps were the same as that in example 1 of the application (compared with example 1,
in comparative example 3, Cymbopogon citrates essential oil was not prepared into
the antibacterial microcapsule, for the purpose of proving that the effect of the
compound fiber film of the application was better).
Comparative example 4
The method in example 1 of the application was adopted for making a comparison
with comparative example 4. The method in comparative example 4 was as follows:
in B4 of step 2), tape casting was performed to the mixed solution obtained in B3 on a
glass plate to obtain a preservative film; other conditions such as the use amounts and
steps were the same as that in example 1 of the application (compared with example 1,
in comparative example 4, the electrospinning technology was not adopted, for the
purpose of proving that the effect of the compound fiber film of the application was
better).
Test effects
In order to verify the effect of the antibacterial compound fiber film of the application,
the thickness, tensile strength, elongation at break, water vapor permeability and
antibacterial property of the films obtained in examples 1-4 were tested. The results
were as shown in the following table:
Thickn Tensile Elongation Water vapor Diameter of zone Category ess strength at break permeability of inhibition (cm)
(mm) (MPa) (%) (g-mmm2-d~1-kPa-)
Example 1 0.087 3.01 26.54 9.21 3.14
Example 2 0.079 3.36 35.74 8.79 2.59
Example 3 0.074 3.13 41.17 7.35 2.61
Example 4 0.082 3.57 38.67 5.04 2.28
Example 5 0.085 3.43 19.86 7.12 3.02
Comparative 0.078 2.89 24.76 6.85 1.60 example
Comparative 0.071 2.57 30.43 6.12 1.98 example2
Comparative 0.072 2.73 32.87 6.37 2.22 example3
Comparative 0.075 2.06 38.47 6.90 2.08 example
From the above table, it can be seen that:
1) With the increase of the amount of glycerol, the tensile strength of the film
decreases, and the elongation at break and the water vapor permeability increase.
Glycerol, as an alcohol substance, contains three hydrophilic groups. Therefore, the
film also obtains hydrophilicity, which makes it easier to absorb water from the
environment, resulting in the moisture resistance decreases; at the same time, the
interaction between molecules is weakened, resulting in that the density of the film
decreases, the structure becomes worse and the tensile strength decreases.
2) Cassava starch contains a large number of hydrophilic groups, and the
intermolecular acting force increases with the evaporation of water in the film
forming process. Therefore, within a certain range, with the increase of the content of
the starch, the tensile strength increases, and the water vapor permeability decreases.
3) In examples 1-5, the zone of inhibition formed by the film added with 3g of
antibacterial microcapsule is significantly larger than that formed by the film added with 2g of antibacterial microcapsule. Therefore, it can be seen that the Cymbopogon citrates essential oil has a bacteriostatic effect, and the antibacterial effect increases with the increase of the content of the Cymbopogon citrates essential oil within a certain range. From the zones of inhibition in example 1 and comparative examples
1-4, it can be seen that the bacteriostatic effect is improved by adopting the
Cymbopogon citrates essential oil in combination with the electrospinning
technology.
2. In order to verify the slow-release effect of the antibacterial compound fiber film of
the application, the release rate of the essential oil of the film obtained in example 1
and comparative examples 1-4 were tested. The results were as shown in the
following table:
Comparative Comparative Comparative Category Example 1 example 2 example 3 example 4
Id 12% 13% 12% 12%
3d 19% 18% 17% 18%
6d 21% 26% 26% 22%
9d 22% 34% 25% 23%
12d 23% 41% 28% 25%
15d 21% 48% 26% 24%
18d 21% 53% 27% 24%
From the above table, it can be seen that:
1) When comparative example 3 is compared with comparative example 4, the release
rate in comparative example 3 is slightly lower than that in comparative example 4.
Therefore, it can be seen that, if only one of the technologies is used, microcapsule
encapsulation can better improve the slow-release function of the essential oil.
2) Before the sixth day, the release rate of the essential oil in each example or
comparative example is basically the same; after the sixth day, the release rate in
comparative example 2 continues to rise, while the rising rate in the other three methods is basically the same. It shows that both microcapsule and electrospinning technology can achieve the slow-release function, presented as that the release speed of the essential oil is faster at the beginning and the release speed is slower later.
What are described above are just preferred implementation modes of the application.
It should be understood that the application is not limited to the modes disclosed
herein, and should not be regarded as excluding other embodiments, but may be used
for various other combinations, modifications and environments, and may be
modified through the above-mentioned teaching or technology or knowledge in the
related art within the scope of the concept described herein. However, any
modifications and changes made by those skilled in the art without departing from the
spirit and scope of the application shall fall within the scope of protection defined by
the attached claims of the application.

Claims (5)

1. An antibacterial compound fiber film, wherein the antibacterial compound fiber film comprises 2-3 parts of antibacterial microcapsule, 5-7 parts of cassava starch, 1-2 parts of glycerol, 6 parts of gelatin, and 100 parts of deionized water by weight.
2. The antibacterial compound fiber film according to claim 1, wherein the antibacterial compound fiber film comprises 3 parts of antibacterial microcapsule, 7 parts of cassava starch, 2 parts of glycerol, 6 parts of gelatin, and 100 parts of deionized water by weight.
3. The antibacterial compound fiber film according to claim 1, wherein a method for preparing the antibacterial microcapsule comprises the following steps:
Sl: taking and mixing Cymbopogon citrates essential oil with ethyl acetate for dissolution to obtain mixed solution;
S2: taking and mixing p-cyclodextrin with deionized water for dissolution to obtain oversaturated solution;
S3: adding the mixed solution into the oversaturated solution, and sequentially performing magnetic stirring, freeze thawing and suction filtration to obtain a precipitate;
S4: heating and drying the precipitate to constant weight to obtain the antibacterial microcapsule;
wherein the volume ratio of Cymbopogon citrates essential oil to ethyl acetate is 1:4-6; and/or, the volume ratio of the supersaturated solution to the mixed solution is 8-10:1;
wherein in S3, the temperature of magnetic stirring is 60-80°C, and the time is 120min; and/or, the temperature of freeze thawing is -18°C, and the time is 4h;
wherein in S4, the temperature of heating and drying is 50°C.
4. A method for preparing the antibacterial compound fiber film according to any one of claims 1-3, wherein the method comprises the following steps:
S5: weighing the antibacterial microcapsule, the cassava starch, the glycerol, the
gelatin and the deionized water according to proportions;
S6: dissolving the cassava starch in the deionized water for gelatinization to obtain
gelatinized starch solution;
S7: taking and uniformly mixing the glycerol, the gelatin and the gelatinized starch
solution, performing cooling, and adding the antibacterial microcapsule to obtain
spinning solution;
S8: performing electrospinning by using the spinning solution to obtain the
antibacterial compound fiber film;
wherein in S6, the temperature of gelatinization is 100C, and the time is 30min;
wherein in S8, the conditions for electrospinning are as follows: electric field intensity:
18kv/cm, distance: 15cm, speed: 0.2ml/h, time: 12h.
5. Application of the antibacterial compound fiber film according to any one of
claims 1-3 to fresh keeping of fruits and vegetables.
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