CN107365420A - A kind of bacteria cellulose/polyvinyl alcohol medical composite material and preparation method thereof - Google Patents
A kind of bacteria cellulose/polyvinyl alcohol medical composite material and preparation method thereof Download PDFInfo
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- CN107365420A CN107365420A CN201710314031.8A CN201710314031A CN107365420A CN 107365420 A CN107365420 A CN 107365420A CN 201710314031 A CN201710314031 A CN 201710314031A CN 107365420 A CN107365420 A CN 107365420A
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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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
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/02—Applications for biomedical use
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/02—Heterophasic composition
Abstract
The present invention relates to a kind of bacteria cellulose/polyvinyl alcohol bio-medical composition and preparation method thereof, key step is as follows：Polyvinyl alcohol is directly appended in acetobacter xylinum fermentation medium, make bacteria cellulose in its secretion and assembling process with polyvinyl alcohol In-situ reaction using the hydrogen bond action between polyvinyl alcohol and bacteria cellulose, gained composite membrane is purified, drying to bacteria cellulose/polyvinyl alcohol composite membrane（in‑situ BC/PVA）.Because bacteria cellulose has the intensity and modulus of superelevation, polyvinyl alcohol has higher transparency and biological stability, polyvinyl alcohol is introduced in bacteria cellulose can improve transparency, mechanical strength and the biological stability of material, lift it and be applied to the possibility of biological medicine Material Field as cornea,artificial.
Description
Technical field
The present invention relates to a kind of preparation of bio-medical material, particularly a kind of bacteria cellulose/polyvinyl alcohol is medical multiple
Condensation material and preparation method thereof.
Background technology
Bacteria cellulose（Bacterial Cellulose, abbreviation BC）, it is the natural fiber as caused by microbial metabolism
Element, its chemical constitution are no different with cellulose caused by plant and marine alga.Bacteria cellulose high mechanical strength, crystallinity are high, water holding
Property it is high, biocompatibility is good, biodegradable, without any impurity and possess superfine nano network of fibers.Have benefited from bacterium
The numerous excellent characteristics of cellulose, bacteria cellulose is in many field extensive uses, in terms of bio-medical material, bacterial fibers
Element can be used as medical dressing, artificial skin, artificial blood vessel, tissue engineering bracket, artificial cartilage etc., and have good application
Prospect.Though bacteria cellulose there are many excellent biological characteristicses, applied as artificial cornea material, still need to enter it
Some surfaces of row are modified, and its transparency and biological stability is further lifted.
Polyvinyl alcohol（Polyvinyl alcohol, abbreviation PVA）It is that the one kind for hydrolyzing to obtain by vinyl acetate is water-soluble high
Molecule, chemical property are stable, have good film forming, caking property and biological stability, can be widely applied to building, papermaking,
The industries such as weaving, chemical industry, daily use chemicals and biological medicine.Further, since polyvinyl alcohol has the splendid transparency, led in eye medical treatment
Domain, polyvinyl alcohol great potential is as cornea,artificial's materials'use, but its mechanical property is slightly inadequate.
Infusion process, in-situ method and casting method can be divided into by preparing the method for bacteria cellulose/polyvinyl alcohol composite.Pour
The method of building need to crush bacteria cellulose in advance, and process is complicated, and can destroy bacterial cellulose three-dimensional network structure；Current research
Achievement is concentrated mainly on infusion process.Jie hua wang etc.（Wang J, Gao C, Zhang Y, et al.
Preparation and in vitro characterization of BC/PVA hydrogel composite for
its potential use as artificial cornea biomaterial[J]. Materials Science &
Engineering C, 2010, 30(1):214-218.）The bacterial cellulose wet-coating prepared is immersed in polyvinyl alcohol water
In solution, content water and cornea is made close to bacteria cellulose/polyvinyl alcohol composite being recycled freeze thawing crosslinking, but
Need the step by complexity.It can make bacteria cellulose by being directly directly added into polyvinyl alcohol into acetobacter xylinum culture medium
It is in contact even closer, disperses more uniform with polyvinyl alcohol two.
The content of the invention
The invention aims to provide a kind of easy-to-use to prepare mechanical strength（Especially pulled down in moisture state
Stretch intensity and tearing strength）High and light transmission and the preferable bacteria cellulose/polyvinyl alcohol composite of biological stability
Method, be related to a kind of bio-medical composition preparation field.
Technical scheme is as follows：
A kind of medical composite material, including bacteria cellulose film, polyvinyl alcohol.Bacteria cellulose provided by the invention/poly-
Vinyl alcohol composite material and preparation method thereof comprises the following steps：
Step 1：With 70-100 °C of hot water dissolving's polyvinyl alcohol, deionized water is replaced to prepare wooden vinegar with polyvinyl alcohol water solution
Bacillus fermentation culture medium, the culture medium composition made is 7.0wt% glucose, 1.5wt% yeast extracts, 1.0% (v/v) absolute ethyl alcohol,
10-30g/L polyvinyl alcohol, pH=6.8.121 DEG C of high-temperature sterilization 20min, after inoculation, incubated 10 days at 20-30 DEG C, obtain
Bacteria cellulose/polyvinyl alcohol composite wet film,
Step 2：Bacteria cellulose/polyvinyl alcohol composite membrane is soaked with 0.1M NaOH solutions, then is cleaned repeatedly with deionized water
It is in neutrality to cellulose surface,
Step 3：It will be dehydrated under bacteria cellulose after purification processes/composite polyethylene material wet film under 30-80 °C.
Compared with existing technologies, the invention has the characteristics that and advantage：
(1) polyvinyl alcohol is directly appended to that the bacteria cellulose fibril just secreted out of can be made in culture medium of bacterial cellulose
Dimension, microfibre directly contact with polyvinyl alcohol, make the two-phase in composite scattered more equal, enhancing composite two is alternate
Phase interface effect；
(2) when the concentration of polyvinyl alcohol is in 10-30/L concentration ranges, the bacterial fibers that are prepared by the above method
Tearing strength of the element/polyvinyl alcohol composite material film under moisture state, tensile strength are relatively strong and translucency significantly improves；
(3) bacteria cellulose/polyvinyl alcohol composite produced by the present invention has stronger biological stability.
(4) fermentation temperature of bacterial fibers/polyvinyl alcohol composite material is relatively low in the preparation present invention, and composite yield is higher,
It is cost-saved.
Brief description of the drawings
Fig. 1 be pure bacteria cellulose and when PVA concentration is 20g/L bacteria cellulose/polyvinyl alcohol composite it is micro-
See structure chart.Fig. 2, Fig. 3 and Fig. 4 are in-situ method bacteria cellulose/polyvinyl alcohol under pure bacteria cellulose and various concentrations respectively
Composite when composite moisture state Tensile strength, tearing strength, light transmission and polyvinyl alcohol concentration are 20g/L
Translucency places the comparison diagram of a period of time under 37 °C in phosphate buffer.Fig. 5 is that embodiment 1 is degraded front and rear light transmittance
Contrast.
From Fig. 1（b）In as can be seen that when polyvinyl alcohol concentration is 20g/L, polyvinyl alcohol is coated uniformly on bacterial fibers
Increase its diameter on plain silk ribbon and fill up in bacteria cellulose network structure, make material structure fine and close, it is homogeneous to form two-phase
Composite.From Fig. 1（c）When polyvinyl alcohol concentration is 50g/L, bacteria cellulose silk ribbon attenuates, in polyvinyl alcohol between silk ribbon
Adhesive effect under mutually cohere to form loose alveolate texture, material homogeneity reduce.
As can be seen from Figure 2 when polyvinyl alcohol concentration is in 20-30g/L, bacteria cellulose/polyvinyl alcohol composite
Light transmittance is obviously improved, and composite obtained by especially when polyvinyl alcohol concentration is in 20g/L is higher in visible region light transmittance
And there is certain absorption in ultraviolet region.
As can be seen from Figure 3 under moisture state the tensile strength of bacteria cellulose/polyvinyl alcohol composite with PVA
In the medium the rising of concentration and first rise and decline afterwards, 118.4 ± 6.65MPa of maximum is reached when PVA concentration is 20g/L.
As can be seen from Figure 4 under moisture state the tearing strength of bacteria cellulose/polyvinyl alcohol composite with PVA
The rising of concentration first rises in the medium declines afterwards.Reach 116.95 ± 10.41kN/m of maximum when PVA concentration is 20g/L
。
As can be seen from Figure 5 after embodiment 1 is degraded light transmittance in the range of 200-800nm light waves slightly under
Drop.
To investigate the biological stability of material, it is compound that we will pass through in-situ BC/PVA2.0 made from case study on implementation 1
Material is immersed in phosphate buffered saline solution under 37 °C, simulates the change of its performance in body fluid.Tested by eight months
Afterwards, the tearing strength of in-situ BC/PVA2.0 composites is almost unchanged.And as can be seen that being dropped at 8 months in from the graph
Its light transmittance only slightly reduces after solution, and wavelength is to be reduced at 425nm at most, is 3.94%, it may be said that the biology of material transmissivity
Have good stability.
Embodiment
The present invention is further described with reference to specific embodiment, following examples are descriptive, are not
Limited, but protection domain is not limited thereto.
Embodiment 1
(1) 2g polyvinyl alcohol is weighed, deionized water dissolving is used under 80 °C,
(2) add 7.0g glucose and 1.5g yeast extracts are put into beaker, after being sufficiently stirred dissolving, it is anhydrous to add 1.0mL
Ethanol, it is settled to 100mL, regulation pH value of solution to 6.8.It is fitted into conical flask, 121 DEG C of high-temperature sterilization 20min after sealing, is inoculated with
Afterwards, incubated 10 days under 20 °C, bacteria cellulose/polyvinyl alcohol composite wet film is obtained.Composite membrane is put into 0.1M
In NaOH solution, normal temperature stands 24h, is in neutrality with a large amount of deionized water rinsings to fiber surface,
(3) it will be dried at 30 DEG C of composite material film obtained by step (2) in baking oven, it is medical to obtain bacteria cellulose/polyvinyl alcohol
Compound dry film.
Tested through translucency, when polyvinyl alcohol concentration is 20g/L, bacteria cellulose/polyvinyl alcohol composite membrane has preferable
Transparency, its light transmittance is up to 84.11%, than pure bacteria cellulose lifting 12.57%；Drawing under composite moisture state simultaneously
It is 118.4 ± 6.65MPa to stretch intensity, and tearing strength is 116.95 ± 10.41kN/m；Purer bacteria cellulose lifting respectively
22.12%, 7.80%.
Embodiment 2
3g polyvinyl alcohol is weighed, deionized water dissolving is used under 80 °C, then make with step (2) in case study on implementation 1 and step (3)
Detailed fungin/polyvinyl alcohol composite material.
Embodiment 3
(1) 2g polyvinyl alcohol is weighed, deionized water dissolving is used under 80 °C,
(2) add 7.0g glucose and 1.5g yeast extracts are put into beaker, after being sufficiently stirred dissolving, it is anhydrous to add 1.0mL
Ethanol, it is settled to 100mL, regulation pH value of solution to 6.8.It is fitted into conical flask, 121 DEG C of high-temperature sterilization 20min after sealing, is inoculated with
Afterwards, incubated 10 days under 30 °C, bacteria cellulose/polyvinyl alcohol composite wet film is obtained.It is molten that film is put into 0.1M NaOH
In liquid, normal temperature stands 24h, is in neutrality with a large amount of deionized water rinsings to fiber surface,
(3) it will be dried at 40 DEG C of composite material film obtained by step (2) in baking oven, obtain bacteria cellulose/polyvinyl alcohol doctor
With compound dry film.
Embodiment 4
3g polyvinyl alcohol is weighed, deionized water dissolving is used under 80 °C, then make with step (2) in case study on implementation 3 and step (3)
Detailed fungin/polyvinyl alcohol composite material.
Claims (6)
1. a kind of bacteria cellulose/polyvinyl alcohol bio-medical composition, it is characterised in that trained by being fermented to acetobacter xylinum
Support and the polyvinyl alcohol of dissolving added in base, make the polyvinyl alcohol in culture medium during bacteria cellulose is secreted and assembles with
Its In-situ reaction, obtains bacteria cellulose/polyvinyl alcohol composite, and described bacteria cellulose is by production bacteria cellulose bacterium
The native cellulose of strain secretion, its molecular structure are consistent with plant cellulose and marine alga；The described polyvinyl alcohol degree of polymerization is
1750 ± 50, alcoholysis degree 98%.
2. a kind of method for preparing bacteria cellulose/polyvinyl alcohol composite according to claim 1, its feature exist
In, comprise the following steps, (1) prepares the acetobacter xylinum fermentation medium containing PVA macromoleculars, incubated 10 days after inoculation,
Obtain bacteria cellulose/polyvinyl alcohol composite wet film, purified, (2) again by the bacteria cellulose Jing Guo step (2)/
Polyvinyl alcohol composite material wet film takes out, and is dehydrated in an oven.
3. a kind of method for preparing bacteria cellulose/polyvinyl alcohol medical composite material according to claim 2, it is special
Sign is that culture medium composition is 7.0wt% glucose, 1.5wt% yeast extracts, 1.0% (v/v) anhydrous second in the step (1)
Alcohol, 10-30g/L polyvinyl alcohol, pH=6.8.
4. a kind of method for preparing bacteria cellulose/polyvinyl alcohol medical composite material according to claim 2, it is special
Sign is that method of purification is to be soaked in 0.1M NaOH solutions in the step (1), then fine to bacterium with deionized water rinsing
Element/composite membrane of polyvinyl alcohol surface is tieed up in neutrality.
5. a kind of method for preparing bacteria cellulose/polyvinyl alcohol medical composite material according to claim 2, its feature
It is, incubated temperature is 20-30 DEG C in the step (1).
6. a kind of method for preparing bacteria cellulose/polyvinyl alcohol medical composite material according to claim 2, its feature
It is, oven temperature is 30-80 DEG C in the step (3).
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| CN201710314031.8A CN107365420B (en) | 2017-05-05 | 2017-05-05 | Bacterial cellulose/polyvinyl alcohol medical composite material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115725119A (en) * | 2022-12-01 | 2023-03-03 | 国纳之星(上海)纳米科技发展有限公司 | Preparation method of bacterial cellulose/polyvinyl alcohol biomedical composite material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961784A (en) * | 2012-11-29 | 2013-03-13 | 华南理工大学 | BC (Bacterial Cellulose)/PVA (Polyvinyl Alcohol) composite material, as well as preparation method and application thereof |
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2017
- 2017-05-05 CN CN201710314031.8A patent/CN107365420B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961784A (en) * | 2012-11-29 | 2013-03-13 | 华南理工大学 | BC (Bacterial Cellulose)/PVA (Polyvinyl Alcohol) composite material, as well as preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| GEA S,BILOTTI E,REYNOLDS CT,SOYKEABKEAW N,PEIJS T.: "Bacterial cellulose–poly(vinyl alcohol) nanocomposites prepared by an in-situ process", 《MATERIALS LETTERS》 * |
| S. GEA, F.G. TORRES, O.P. TRONSCOSO, C.T. REYNOLDS, F. VILASECCA: "Biocomposites based on bacterial cellulose and apple and radish pulp", 《INTERNATIONAL POLYMER PROCESSING》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115725119A (en) * | 2022-12-01 | 2023-03-03 | 国纳之星(上海)纳米科技发展有限公司 | Preparation method of bacterial cellulose/polyvinyl alcohol biomedical composite material |
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