CN108948437A - A kind of anti-oxidant tri compound film of biology base antibacterial, preparation method and its usage - Google Patents
A kind of anti-oxidant tri compound film of biology base antibacterial, preparation method and its usage Download PDFInfo
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- CN108948437A CN108948437A CN201810508517.XA CN201810508517A CN108948437A CN 108948437 A CN108948437 A CN 108948437A CN 201810508517 A CN201810508517 A CN 201810508517A CN 108948437 A CN108948437 A CN 108948437A
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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
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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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
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/14—Hemicellulose; Derivatives thereof
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Abstract
The present invention provides a kind of anti-oxidant tri compound films of biology base antibacterial, preparation method and its usage, hemicellulose, chitosan and polyacid are carried out esterification by this method, membrane material is prepared by the tape casting, then using hot press that the membrane material of preparation is hot-forming, further crosslinking curing is to prepare hemicellulose/chitosan/polyacid tri compound film.Composite membrane made from this method has excellent mechanical property, while having good anti-oxidant and antibacterial functions.This new bio base tri compound film has important application value in food function material, bio-medical material, Environmental Engineering Material field.
Description
Technical field
The invention belongs to biomembrane material technical field, it is related to a kind of anti-oxidant tri compound film of biology base antibacterial, preparation
Method and application thereof.
Background technique
Biomass source is extensive, rich reserves, renewable and degradable, at low cost compared with petrochemical industry class product
And to more environment-friendly.With the exhaustion of fossil energy and the deterioration of ecological environment, countries in the world will develop renewable life
The physical resources strategic choice important as country.The research and development of biomass-based macromolecule new material are repeatedly included in state by the Chinese government
The emphasis key scientific and technological projects of long-term scientific and technological development planning in family.As rich reserves in nature and reproducible day
Right macromolecule such as cellulose, lignin, chitin, starch, protein, polysaccharide and natural rubber etc. is advanced function material
Research and development provide resource abundant.Hemicellulose is the heteromeric polysaccharide of one kind for connecting cellulose and lignin, is widely present in
In the cell wall of plant fiber.Hemicellulose is non-crystalline structure, and intensity is lower, and the degree of polymerization is 80~200.According to main chain glycosyl
Structure, hemicellulose can be divided into xylan, poly- Galactose Glucose sugar mannose, araban galactolipin, polydextrose sweet dew
Sugar etc..Wherein, xylan is the main component of hemicellulose, accounts for the 35% of plant cell dry weight, is a kind of biomass abundant
Resource, be in nature in addition to cellulose the most abundant natural polymer of reserves.However, since its molecular weight is lower, heterogeneous
Property, polydispersity, branch degree is high and amorphous structure causes huge so that most of xylan is not used effectively in nature
The big wasting of resources.Nowadays becoming increasingly conspicuous with environment and energy problem, hemicellulose can be again as a kind of rich reserves
Raw biomass resource is gradually considered to have huge Exploitative potential and market value and is favored by the world.
Chitosan is a kind of substance processed from the different types crustacean such as shrimp crab, has multifunctional groups anti-
The characteristics of answering activity, biocompatibility, biodegradability, antibiotic property and antioxidant activity.The basic unit of chitosan is
Glucosamine contains amino, hydroxyl, acetylamino, oxygen bridge isoreactivity group on strand simultaneously, many derivatizations can occur
Reaction such as esterification, arylation and alkylation, Schiff reaction, graft copolymerization, make it in food function material, bio-medical
The fields such as material, cosmetics, agricultural, environmental protection all have wide practical use.However, its machinery of the chitosan of original form
Intensity is relatively low, and is soluble in weakly acidic solution, to limit the practical application of chitosan.Therefore, in conjunction with hemicellulose
With chitosan respectively molecular structure the characteristics of and advantage, pass through chemical modification technique and improve stabilization of the chitosan in acid medium
Property and mechanical strength, assign material antibacterial and antioxidant activity ability, preparation can be degradable biomass-based macromolecule material
Material, and new way can be opened up for the higher value application of biomass resource.
Summary of the invention
In face of the global energy crisis and problem of environmental pollution got worse, the biomass-based function that research and development can be degradable
Energy material has great importance.The product prepared using the biomass of natural reproducible as raw material is to human body and the nontoxic nothing of environment
Evil can effectively improve shortage of resources and maintain the ecological balance.The present invention passes through addition using chitosan, hemicellulose as raw material
Polyacid, which carries out esterification preparation, has stronger antibacterial, antioxidant activity, biodegradable and high mechanical strength food packet
Fill membrane material.
A kind of preparation method of the anti-oxidant tri compound film of biology base antibacterial, which comprises the following steps:
(1) chitosan is dissolved in volume fraction is that it is poly- to prepare the shell that mass concentration is 2~5% in 1~3% acetic acid solution
Sugared acetic acid solution, then be added mass concentration be 4~10% hemicellulose aqueous solutions and at room temperature magnetic agitation 20~
60min, then it is (2~5) that mass ratio, which is added, into mixed liquor: 1 polyacid-Sodium Thiosulfate mixture continues to stir at room temperature
Mix 20~30min, using sodium acetate adjust solution pH be 3~5,60~180min of water-bath back flow reaction under the conditions of 100 DEG C,
Casting film-forming obtains chitosan/hemicellulose/polyacid composite membrane after reaction；
(2) using hot press by chitosan/hemicellulose/polyacid composite membrane of preparation at 80~160 DEG C, 50~
Hot-forming 30~60min under the conditions of 80MPa, further crosslinking curing obtain the target product with antibacterial anti-oxidation function
Hemicellulose/chitosan/polyacid tri compound film.
Further, the chitosan viscosity average molecular weigh is 20~1,000,000, and deacetylation is 85~95%.
Further, the hemicellulose is water-soluble Arabic sugar -4-O- methyl glucose uronic acid xylan.
Further, the polyacid is itaconic acid, malonic acid, maleic acid, malic acid, succinic acid or citric acid.
Further, both the chitosan, hemicellulose quality and polyacid-Sodium Thiosulfate mixture mass ratio
For (1~3): 1.
The anti-oxidant tri compound film of biology base antibacterial of the method preparation, which is characterized in that by chitosan, hemicellulose
Chitosan, hemicellulose, the polyacid co-polymer membrane that element, polyacid are esterified under the action of sodium sulfite catalyst.
The anti-oxidant tri compound film of biology base antibacterial is used as antibacterial, oxidation-resistant film.
Compared with prior art, the present invention having the advantage that
(1) it is membrane material matrix, from a wealth of sources, cheap, production cost that the present invention, which selects hemicellulose, chitosan,
It is low, in material biomass material account for 75% or more, it can be achieved that commercial scale resource utilization requirement.
(2) present invention solves the technical problem of biomass material blending, modification by copolymerization poor compatibility, makes full use of half fiber
The characteristics of dimension element and chitosan molecule structure, the compatibility of biomass-based material is improved by esterification, improves material
Mechanical strength and stability.
(3) composite membrane prepared by the present invention have antibacterial, antioxidant activity and can completely environment degradable characteristic, both may be used
It realizes making full use of for agricultural wastes, and can realize economic growth, be the higher value application and expansion work of biomass resource
Industry product scope opens up new way.
Detailed description of the invention
Fig. 1 is the mechanical property of Examples 1 to 6 tri compound film.
Fig. 2 is the antibiotic property of Examples 1 to 6 tri compound film.
Fig. 3 is the antioxidant activity of Examples 1 to 6 tri compound film.
Specific embodiment
Present invention will be further explained with reference to the attached drawings and specific examples, but protection scope of the present invention is simultaneously
It is without being limited thereto.
Embodiment 1
It is in 1% acetic acid solution that 4g chitosan, which is dissolved in 100mL volume fraction, and magnetic agitation is poly- to shell at room temperature
Sugar is completely dissolved, and 50mL mass concentration is then added and is 8% hemicellulose aqueous solution and continues to stir 30min, then to mixed liquor
It is middle that itaconic acid-Sodium Thiosulfate that 3g mass ratio is 2:1 is added, continue to stir 30min at room temperature, adjusts solution using sodium acetate
PH be 4, the water-bath back flow reaction 60min under the conditions of 100 DEG C, after reaction casting film-forming obtain chitosan/hemicellulose/
Itaconic acid composite membrane.Using hot press by chitosan/hemicellulose/itaconic acid composite membrane of preparation at 80 DEG C, under the conditions of 60MPa
Hot-forming 45min, further crosslinking curing are to obtain target product to gather with hemicellulose/shell of antibacterial anti-oxidation function
Sugar/itaconic acid tri compound film.
Embodiment 2
It is in 2% acetic acid solution that 4g chitosan, which is dissolved in 100mL volume fraction, and magnetic agitation is poly- to shell at room temperature
Sugar is completely dissolved, and 50mL mass concentration is then added and is 8% hemicellulose aqueous solution and continues to stir 30min, then to mixed liquor
It is middle that malonic acid-Sodium Thiosulfate that 3g mass ratio is 2:1 is added, continue to stir 40min at room temperature, adjusts solution using sodium acetate
PH be 4.5, the water-bath back flow reaction 60min under the conditions of 100 DEG C, casting film-forming obtains chitosan/hemicellulose after reaction
Element/malonic acid composite membrane.Using hot press by chitosan/hemicellulose/malonic acid composite membrane of preparation at 90 DEG C, 60MPa item
Hot-forming 30min under part, further crosslinking curing are the hemicellulose/shell for obtaining target product and having antibacterial anti-oxidation function
Glycan/malonic acid tri compound film.
Embodiment 3
It is in 3% acetic acid solution that 4g chitosan, which is dissolved in 100mL volume fraction, and magnetic agitation is poly- to shell at room temperature
Sugar is completely dissolved, and 50mL mass concentration is then added and is 8% hemicellulose aqueous solution and continues to stir 30min, then to mixed liquor
It is middle that maleic acid-Sodium Thiosulfate that 3g mass ratio is 2:1 is added, continue to stir 40min at room temperature, adjusts solution using sodium acetate
PH be 5.0, the water-bath back flow reaction 80min under the conditions of 100 DEG C, casting film-forming obtains chitosan/hemicellulose after reaction
Element/maleic acid composite membrane.Using hot press by chitosan/hemicellulose/maleic acid composite membrane of preparation at 80 DEG C, 70MPa item
Hot-forming 50min under part, further crosslinking curing are the hemicellulose/shell for obtaining target product and having antibacterial anti-oxidation function
Glycan/maleic acid tri compound film.
Embodiment 4
It is in 1% acetic acid solution that 4g chitosan, which is dissolved in 100mL volume fraction, and magnetic agitation is poly- to shell at room temperature
Sugar is completely dissolved, and 50mL mass concentration is then added and is 8% hemicellulose aqueous solution and continues to stir 30min, then to mixed liquor
It is middle that malic acid-Sodium Thiosulfate that 3g mass ratio is 2:1 is added, continue to stir 40min at room temperature, adjusts solution using sodium acetate
PH be 5.5, the water-bath back flow reaction 100min under the conditions of 100 DEG C, casting film-forming obtains chitosan/hemicellulose after reaction
Element/malic acid composite membrane.Using hot press by chitosan/hemicellulose/malic acid composite membrane of preparation at 100 DEG C, 60MPa item
Hot-forming 60min under part, further crosslinking curing are the hemicellulose/shell for obtaining target product and having antibacterial anti-oxidation function
Glycan/malic acid tri compound film.
Embodiment 5
It is in 2% acetic acid solution that 4g chitosan, which is dissolved in 100mL volume fraction, and magnetic agitation is poly- to shell at room temperature
Sugar is completely dissolved, and 50mL mass concentration is then added and is 8% hemicellulose aqueous solution and continues to stir 30min, then to mixed liquor
It is middle that succinic acid-Sodium Thiosulfate that 3g mass ratio is 2:1 is added, continue to stir 40min at room temperature, adjusts solution using sodium acetate
PH be 6.0, the water-bath back flow reaction 60min under the conditions of 100 DEG C, casting film-forming obtains chitosan/hemicellulose after reaction
Element/succinic acid composite membrane.Using hot press by chitosan/hemicellulose/succinic acid composite membrane of preparation at 100 DEG C, 70MPa item
Hot-forming 45min under part, further crosslinking curing are the hemicellulose/shell for obtaining target product and having antibacterial anti-oxidation function
Glycan/succinic acid tri compound film.
Embodiment 6
It is in 3% acetic acid solution that 4g chitosan, which is dissolved in 100mL volume fraction, and magnetic agitation is poly- to shell at room temperature
Sugar is completely dissolved, and 50mL mass concentration is then added and is 8% hemicellulose aqueous solution and continues to stir 30min, then to mixed liquor
It is middle that citric acid-Sodium Thiosulfate that 3g mass ratio is 2:1 is added, continue to stir 40min at room temperature, adjusts solution using sodium acetate
PH be 6.0, the water-bath back flow reaction 60min under the conditions of 100 DEG C, casting film-forming obtains chitosan/hemicellulose after reaction
Element/citric acid composite membrane.Using hot press by chitosan/hemicellulose/citric acid composite membrane of preparation at 100 DEG C, 80MPa item
Hot-forming 60min under part, further crosslinking curing are the hemicellulose/shell for obtaining target product and having antibacterial anti-oxidation function
Glycan/citric acid tri compound film.
The preparation method of the anti-oxidant tri compound film of biology base antibacterial of the present invention is to be with chitosan, hemicellulose
Raw material carries out esterification by addition polyacid and obtains the terpolymer film of chitosan, hemicellulose, polyacid.Fig. 1,
Fig. 2, Fig. 3 respectively illustrate mechanical property, antibiotic property, the antioxidant activity of tri compound film prepared by embodiment 1-6, embodiment
Tri compound film elasticity modulus prepared by 1-6 is 250-700MPa, reaches 74- to the antibacterial ability of staphylococcus aureus
86%, the clearance rate to DPPH free radical is 65-82%.Show that the tri compound film has preferable mechanical performance, obvious
Biocidal property and good inoxidizability.It can be widely applied for packaging material for food, bio-medical material, Environmental Engineering Material
Antibacterial, oxidation-resistant film in field.
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (7)
1. a kind of preparation method of the anti-oxidant tri compound film of biology base antibacterial, which comprises the following steps:
(1) chitosan is dissolved in volume fraction is to prepare the chitosan second that mass concentration is 2~5% in 1~3% acetic acid solution
Acid solution, then be added mass concentration be 4~10% hemicellulose aqueous solutions and at room temperature magnetic agitation 20~
60min, then it is (2~5) that mass ratio, which is added, into mixed liquor: 1 polyacid-Sodium Thiosulfate mixture continues to stir at room temperature
Mix 20~30min, using sodium acetate adjust solution pH be 3~5,60~180min of water-bath back flow reaction under the conditions of 100 DEG C,
Casting film-forming obtains chitosan/hemicellulose/polyacid composite membrane after reaction；
(2) using hot press by chitosan/hemicellulose/polyacid composite membrane of preparation at 80~160 DEG C, 50~80MPa item
Hot-forming 30~60min under part, further crosslinking curing obtain the target product hemicellulose with antibacterial anti-oxidation function
Element/chitosan/polyacid tri compound film.
2. preparation side's method described in accordance with the claim 1, it is characterised in that: the chitosan viscosity average molecular weigh is 20~100
Ten thousand, deacetylation is 85~95%.
3. preparation side's method described in accordance with the claim 1, it is characterised in that: the hemicellulose is water-soluble Arabic sugar-
4-O- methyl glucose uronic acid xylan.
4. preparation side's method described in accordance with the claim 1, it is characterised in that: the polyacid is itaconic acid, malonic acid, Malaysia
Acid, malic acid, succinic acid or citric acid.
5. preparation side's method described in accordance with the claim 1, it is characterised in that: both the chitosan, hemicellulose quality with
Polyacid-Sodium Thiosulfate mixture mass ratio is (1~3): 1.
6. a kind of anti-oxidant tri compound film of biology base antibacterial of the preparation of any one of -5 the methods according to claim 1,
Be characterized in that, by be esterified under the action of chitosan, hemicellulose, polyacid are in sodium sulfite catalyst chitosan,
Hemicellulose, polyacid co-polymer membrane.
7. the anti-oxidant tri compound film of biology base antibacterial described in claim 6 is used as antibacterial, oxidation-resistant film.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111264615A (en) * | 2020-03-16 | 2020-06-12 | 四川天星智能包装股份有限公司 | Bacteriostasis method for vegetable and fruit processing |
| CN111320771A (en) * | 2020-04-03 | 2020-06-23 | 蚌埠学院 | Preparation method of chitosan/montmorillonite hybrid microspheres and application of chitosan/montmorillonite hybrid microspheres in sustained release of methacycline hydrochloride |
| CN112280067A (en) * | 2019-07-24 | 2021-01-29 | 南京理工大学 | Preparation method of edible antibacterial film |
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| US8975387B1 (en) * | 2010-03-22 | 2015-03-10 | North Carolina State University | Modified carbohydrate-chitosan compounds, methods of making the same and methods of using the same |
| CN109081930A (en) * | 2018-07-09 | 2018-12-25 | 北京林业大学 | A kind of functional edible film and preparation method thereof based on hemicellulose and chitosan |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US8975387B1 (en) * | 2010-03-22 | 2015-03-10 | North Carolina State University | Modified carbohydrate-chitosan compounds, methods of making the same and methods of using the same |
| CN109081930A (en) * | 2018-07-09 | 2018-12-25 | 北京林业大学 | A kind of functional edible film and preparation method thereof based on hemicellulose and chitosan |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112280067A (en) * | 2019-07-24 | 2021-01-29 | 南京理工大学 | Preparation method of edible antibacterial film |
| CN112280067B (en) * | 2019-07-24 | 2022-06-10 | 南京理工大学 | Preparation method of edible antibacterial film |
| CN111264615A (en) * | 2020-03-16 | 2020-06-12 | 四川天星智能包装股份有限公司 | Bacteriostasis method for vegetable and fruit processing |
| CN111320771A (en) * | 2020-04-03 | 2020-06-23 | 蚌埠学院 | Preparation method of chitosan/montmorillonite hybrid microspheres and application of chitosan/montmorillonite hybrid microspheres in sustained release of methacycline hydrochloride |
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