CN107365420B - Bacterial cellulose/polyvinyl alcohol medical composite material and preparation method thereof - Google Patents

Bacterial cellulose/polyvinyl alcohol medical composite material and preparation method thereof Download PDF

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CN107365420B
CN107365420B CN201710314031.8A CN201710314031A CN107365420B CN 107365420 B CN107365420 B CN 107365420B CN 201710314031 A CN201710314031 A CN 201710314031A CN 107365420 B CN107365420 B CN 107365420B
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polyvinyl alcohol
bacterial cellulose
composite material
cellulose
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CN107365420A (en
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周晓东
杨眉
陈袁曦
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East China University of Science and Technology
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    • C12P19/00—Preparation of compounds containing saccharide radicals
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • 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
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Abstract

The invention relates to a bacterial cellulose/polyvinyl alcohol biomedical composite material and a preparation method thereof, and the preparation method mainly comprises the following steps: directly adding polyvinyl alcohol into an acetobacter xylinum fermentation culture medium, utilizing the hydrogen bond action between the polyvinyl alcohol and the bacterial cellulose to enable the bacterial cellulose to be compounded with the polyvinyl alcohol in situ in the secretion and assembly processes, purifying and drying the obtained composite membrane to obtain the bacterial cellulose/polyvinyl alcohol composite membrane (in-situ BC/PVA). Because the bacterial cellulose has ultrahigh strength and modulus, the polyvinyl alcohol has higher transparency and biological stability, and the introduction of the polyvinyl alcohol into the bacterial cellulose can improve the transparency, mechanical strength and biological stability of the material, and improve the possibility of applying the material as an artificial cornea in the field of biomedical materials.

Description

Bacterial cellulose/polyvinyl alcohol medical composite material and preparation method thereof
Technical Field
The invention relates to preparation of a biomedical material, in particular to a bacterial cellulose/polyvinyl alcohol medical composite material and a preparation method thereof.
Background
Bacterial Cellulose (BC) is natural Cellulose produced by microbial metabolism, and the chemical structure of the Bacterial Cellulose is not different from that of Cellulose produced by plants and seaweeds. The bacterial cellulose has high mechanical strength, high crystallinity, high water holding capacity, good biocompatibility, biodegradability, no impurity and superfine nano fiber network. Due to the excellent characteristics of the bacterial cellulose, the bacterial cellulose is widely applied to many fields, and in the aspect of biomedical materials, the bacterial cellulose can be used as medical dressings, artificial skins, artificial blood vessels, tissue engineering scaffolds, artificial cartilages and the like, and has good application prospects. Although bacterial cellulose has many excellent biological characteristics, when the bacterial cellulose is used as an artificial cornea material, some surface modification needs to be carried out on the bacterial cellulose, so that the transparency and the biological stability of the bacterial cellulose are further improved.
Polyvinyl alcohol (PVA) is a water-soluble polymer obtained by hydrolyzing vinyl acetate, has stable chemical properties, good film-forming property, good cohesiveness and good biological stability, and can be widely applied to the industries of construction, papermaking, spinning, chemical industry, daily chemicals, biological medicine and the like. In addition, since polyvinyl alcohol has excellent transparency, polyvinyl alcohol has great potential to be used as an artificial cornea material in the field of eye medical treatment, but its mechanical properties are slightly insufficient.
The methods for preparing the bacterial cellulose/polyvinyl alcohol composite material can be divided into an impregnation method, an in-situ method and a pouring method. The pouring method needs to crush the bacterial cellulose in advance, has a complex process and can damage the three-dimensional net structure of the bacterial cellulose; the current research efforts are mainly focused on the dipping method. Jie hua Wang et al (Wang J, Gao C, Zhang Y, et al, Preparation and in vitro catalysis of BC/PVA hydrogel composite for substances as organic cornea biological material [ J ]. Materials Science & Engineering C, 2010, 30(1): 214. 218.) prepared bacterial cellulose wet film was immersed in polyvinyl alcohol aqueous solution, and subjected to cyclic freeze-thaw crosslinking to obtain a bacterial cellulose-containing water and cornea-approximating bacterial cellulose/polyvinyl alcohol composite material, but complicated steps were required. The polyvinyl alcohol is directly added into the acetobacter xylinum culture medium, so that the bacterial cellulose and the polyvinyl alcohol are in two-phase contact more closely and are dispersed more uniformly.
Disclosure of Invention
The invention aims to provide a simple and easy method for preparing a bacterial cellulose/polyvinyl alcohol composite material with high mechanical strength (particularly tensile strength and tearing strength in a wet state) and better light transmittance and biological stability, and relates to the field of preparation of biomedical composite materials.
The technical scheme of the invention is as follows:
a medical composite material comprises a bacterial cellulose membrane and polyvinyl alcohol. The preparation method of the bacterial cellulose/polyvinyl alcohol composite material provided by the invention comprises the following steps:
the method comprises the following steps: dissolving polyvinyl alcohol in hot water at 70-100 ℃, and preparing a acetobacter xylinum fermentation culture medium by using a polyvinyl alcohol aqueous solution instead of deionized water, wherein the culture medium consists of 7.0wt% of glucose, 1.5wt% of yeast extract, 1.0% (v/v) of absolute ethyl alcohol and 10-30g/L of polyvinyl alcohol, and the pH is = 6.8. Sterilizing at 121 deg.C for 20min, inoculating, culturing at 20-30 deg.C for 10 days to obtain wet film of bacterial cellulose/polyvinyl alcohol composite material,
step two: soaking the bacterial cellulose/polyvinyl alcohol composite membrane in 0.1M NaOH solution, washing with deionized water for multiple times until the surface of the cellulose is neutral,
step three: and dehydrating the purified bacterial cellulose/polyethylene composite material under a wet film at 30-80 ℃.
Compared with the prior art, the invention has the following characteristics and advantages:
(1) the polyvinyl alcohol is directly added into the bacterial cellulose culture medium, so that the bacterial cellulose fibrils and microfibers which are just secreted are directly contacted with the polyvinyl alcohol, two phases in the composite material are dispersed more uniformly, and the phase interface effect between the two phases of the composite material is enhanced;
(2) when the concentration of the polyvinyl alcohol is within the range of 10-30/L, the bacterial cellulose/polyvinyl alcohol composite material film prepared by the method has stronger tearing strength and tensile strength in a wet state and obviously improved light transmittance;
(3) the bacterial cellulose/polyvinyl alcohol composite material prepared by the invention has stronger biological stability.
(4) The fermentation temperature for preparing the bacterial fiber/polyvinyl alcohol composite material is lower, the yield of the composite material is higher, and the cost can be saved.
Drawings
FIG. 1 is a microstructure diagram of pure bacterial cellulose and a bacterial cellulose/polyvinyl alcohol composite when the PVA concentration is 20 g/L. FIG. 2, FIG. 3 and FIG. 4 are graphs comparing tensile strength, tear strength and light transmittance of pure bacterial cellulose and in-situ method bacterial cellulose/polyvinyl alcohol composite material in wet state at different concentrations, and the composite material light transmittance of 20g/L polyvinyl alcohol when placed in phosphate buffer solution at 37 ℃ for a period of time. FIG. 5 is a comparison of light transmittance before and after degradation in example 1.
As can be seen from FIG. 1 (b), when the concentration of the polyvinyl alcohol is 20g/L, the polyvinyl alcohol is uniformly coated on the bacterial cellulose silk ribbon to increase the diameter of the bacterial cellulose silk ribbon and fills the bacterial cellulose silk ribbon in the bacterial cellulose network structure, so that the material structure is compact, and a two-phase uniform composite material is formed. From FIG. 1 (c), when the concentration of polyvinyl alcohol is 50g/L, the bacterial cellulose silk ribbons become thin, and the silk ribbons are bonded with each other under the adhesion effect of polyvinyl alcohol to form a loose honeycomb structure, so that the uniformity of the material is reduced.
As can be seen from FIG. 2, when the concentration of polyvinyl alcohol is 20-30g/L, the transmittance of the bacterial cellulose/polyvinyl alcohol composite material is significantly improved, and particularly, when the concentration of polyvinyl alcohol is 20g/L, the obtained composite material has a high transmittance in the visible light region and a certain absorption in the ultraviolet light region.
It can be seen from FIG. 3 that the tensile strength of the bacterial cellulose/polyvinyl alcohol composite material in the wet state increases first and then decreases with the increase of the concentration of PVA in the culture medium, and reaches a maximum of 118.4. + -. 6.65MPa at a concentration of 20g/L of PVA.
It can be seen from FIG. 4 that the tear strength of the bacterial cellulose/polyvinyl alcohol composite material in the wet state increases first and then decreases as the concentration of PVA in the culture medium increases. A maximum of 116.95. + -. 10.41kN/m was reached at a PVA concentration of 20 g/L.
It can be seen from FIG. 5 that the light transmittance in the 200-800nm light wave range is slightly reduced after the degradation of example 1.
To examine the biological stability of the material, we soaked the in-situ BC/PVA2.0 composite material prepared in example 1 in phosphate buffered saline at 37 ℃ to simulate the change of the performance in body fluid. The tear strength of the in-situ BC/PVA2.0 composite was nearly unchanged after eight months of testing. And as can be seen from the above figure, the light transmittance of the material is only slightly reduced after 8 months of degradation, the light transmittance is reduced at the position with the wavelength of 425nm to the maximum, namely 3.94%, so that the biological stability of the light transmittance of the material is good.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be illustrative, not limiting, and the scope of the invention is not limited thereto.
Example 1
(1) Weighing 2g of polyvinyl alcohol, dissolving with deionized water at 80 ℃,
(2) then 7.0g of glucose and 1.5g of yeast extract are added into a beaker, after the mixture is fully stirred and dissolved, 1.0mL of absolute ethyl alcohol is added, the volume is determined to be 100mL, and the pH value of the solution is adjusted to be 6.8. Placing into a triangular flask, sealing, sterilizing at 121 deg.C for 20min, inoculating, and culturing at 20 deg.C for 10 days to obtain wet film of bacterial cellulose/polyvinyl alcohol composite material. Placing the composite membrane into 0.1M NaOH solution, standing at normal temperature for 24h, washing with a large amount of deionized water until the fiber surface is neutral,
(3) and (3) drying the composite material film obtained in the step (2) in an oven at the temperature of 30 ℃ to obtain the bacterial cellulose/polyvinyl alcohol medical composite dry film.
Through a light transmittance test, when the concentration of the polyvinyl alcohol is 20g/L, the bacterial cellulose/polyvinyl alcohol composite membrane has better transparency, and the light transmittance of the bacterial cellulose/polyvinyl alcohol composite membrane can reach 84.11 percent and is improved by 12.57 percent compared with that of pure bacterial cellulose; meanwhile, the tensile strength of the composite material in a wet state is 118.4 +/-6.65 MPa, and the tear strength is 116.95 +/-10.41 kN/m; the yield of the bacterial cellulose is increased by 22.12 percent and 7.80 percent respectively compared with that of the pure bacterial cellulose.
Example 2
3g of polyvinyl alcohol is weighed, dissolved in deionized water at 80 ℃, and then the bacterial cellulose/polyvinyl alcohol composite material is prepared according to the step (2) and the step (3) in the embodiment 1.
Example 3
(1) Weighing 2g of polyvinyl alcohol, dissolving with deionized water at 80 ℃,
(2) then 7.0g of glucose and 1.5g of yeast extract are added into a beaker, after the mixture is fully stirred and dissolved, 1.0mL of absolute ethyl alcohol is added, the volume is determined to be 100mL, and the pH value of the solution is adjusted to be 6.8. Placing into a triangular flask, sealing, sterilizing at 121 deg.C for 20min, inoculating, and culturing at 30 deg.C for 10 days to obtain wet film of bacterial cellulose/polyvinyl alcohol composite material. Putting the membrane into 0.1M NaOH solution, standing for 24h at normal temperature, washing with a large amount of deionized water until the fiber surface is neutral,
(3) and (3) drying the composite material film obtained in the step (2) in an oven at 40 ℃ to obtain the bacterial cellulose/polyvinyl alcohol medical composite dry film.
Example 4
3g of polyvinyl alcohol is weighed, dissolved in deionized water at 80 ℃, and then the bacterial cellulose/polyvinyl alcohol composite material is prepared according to the step (2) and the step (3) in the embodiment 3.

Claims (6)

1. A bacterial cellulose/polyvinyl alcohol biomedical composite material is characterized in that dissolved polyvinyl alcohol is added into a fermentation culture medium of acetobacter xylinum, so that the polyvinyl alcohol in the culture medium is compounded with the bacterial cellulose in situ in the secretion and assembly processes of the bacterial cellulose to obtain the bacterial cellulose/polyvinyl alcohol composite material, wherein the bacterial cellulose is natural cellulose secreted by a bacterial cellulose producing strain, and the molecular structure of the bacterial cellulose is consistent with that of plant cellulose and seaweed;
the polymerization degree of the polyvinyl alcohol is 1750 +/-50, and the alcoholysis degree is 98%;
the culture medium comprises 7.0wt% of glucose, 1.5wt% of yeast extract, 1.0% of absolute ethyl alcohol in volume fraction and 10-30g/L of polyvinyl alcohol.
2. The method for preparing a bacterial cellulose/polyvinyl alcohol composite material according to claim 1, comprising the steps of (1) preparing an acetobacter xylinum fermentation medium containing polyvinyl alcohol macromolecules, inoculating, culturing at a constant temperature for 10 days to obtain a bacterial cellulose/polyvinyl alcohol composite material wet film, purifying, and (2) taking out the bacterial cellulose/polyvinyl alcohol composite material wet film subjected to the step (1), and dehydrating in an oven.
3. The method for preparing the bacterial cellulose/polyvinyl alcohol medical composite material as claimed in claim 2, wherein the composition of the culture medium in the step (1) is 7.0wt% of glucose, 1.5wt% of yeast extract, 1.0% of absolute ethyl alcohol by volume fraction, 10-30g/L of polyvinyl alcohol, and the pH value is 6.8.
4. The method for preparing the bacterial cellulose/polyvinyl alcohol medical composite material according to claim 2, wherein the purification method in the step (1) is to soak the composite material in 0.1M NaOH solution and wash the composite material with deionized water until the surface of the composite film is neutral.
5. The method for preparing the bacterial cellulose/polyvinyl alcohol medical composite material as claimed in claim 2, wherein the constant temperature culture temperature in the step (1) is 20-30 ℃.
6. The method for preparing the bacterial cellulose/polyvinyl alcohol medical composite material as claimed in claim 2, wherein the oven temperature in the step (3) is 30-80 ℃.
CN201710314031.8A 2017-05-05 2017-05-05 Bacterial cellulose/polyvinyl alcohol medical composite material and preparation method thereof Expired - Fee Related CN107365420B (en)

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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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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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Biocomposites based on bacterial cellulose and apple and radish pulp;S. Gea, F.G. Torres, O.P. Tronscoso, C.T. Reynolds, F. Vilasecca;《International Polymer Processing》;20071130;第497-501页 *

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