CN103938447A - Bacterial cellulose/fabric laminated composite material and preparation method thereof - Google Patents
Bacterial cellulose/fabric laminated composite material and preparation method thereof Download PDFInfo
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- CN103938447A CN103938447A CN201410165246.4A CN201410165246A CN103938447A CN 103938447 A CN103938447 A CN 103938447A CN 201410165246 A CN201410165246 A CN 201410165246A CN 103938447 A CN103938447 A CN 103938447A
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Abstract
The invention discloses a bacterial cellulose/fabric laminated composite material and a preparation method thereof. The preparation method comprises the following steps: (1) inoculating acetobacter xylinum into a fluid medium for enlarged cultivation; (2) appropriately cutting a fabric and treating with low-temperature oxygen plasmas or aqueous alkali, or through ultraviolet light surface grafting; and sterilizing and then drying the fabric; (3) arranging the medium containing floccules into a culture dish, spreading the treated fabric on bacterium solution, adding the medium containing floccules into the fabric, and arranging in a biochemical incubator until the laminated composite material is formed; and (4) soaking the composite material with deionized water at normal temperature, soaking the composite material with sodium hydroxide solution for two days, and soaking the composite material with deionized water until the composite material is neutral. The composite material is formed at a time, the appetency of the single fabric and the texture is improved, and the water retainability and the transdermal absorption ratio of the fabric are improved; meanwhile, the operation is convenient and simple and the using efficacy is greatly improved.
Description
Technical field
The present invention relates to a kind of composite, especially a kind of bacteria cellulose/fabric laminar composite and preparation method thereof.
Background technology
Bacteria cellulose refers to the cellulose being synthesized by microorganism.Compare with the cellulose of plant origin, bacteria cellulose has advantages of many uniquenesses: purity, degree of crystallinity are high, and mechanical strength is high, and good biocompatibility is permeable, permeability is excellent, protects fluidity good etc.Just because of these unique advantages of bacteria cellulose, make it at aspects such as food, papermaking, weaving and medical treatment, be subject to paying close attention to widely.In recent years, especially due to the good biocompatibility of bacteria cellulose, protect fluidity, water-permeable and air permeable and be widely used in medical field as dressing.
Fabric is the textiles made from natural fabric or synthetic fiber, is to be passed through to intersect by tiny soft and long thing the flat film piece thing that sintering or bonding form.The Application Areas of fabric is very wide, as each side such as clothing, decoration, automobile, military project and medical treatment.But merely using fabric when Medical dressing is used, because itself hydrophily is strong not, and there is shrink effect, and fabric itself is not ideal enough with the affinity of skin, and the application of fabric aspect dressing is restricted.
The ionized gas shape material that the positron-electron that atom after plasma is deprived of by portions of electronics and atom are ionized rear generation forms, is often regarded as a kind of object state arranged side by side with gas, liquid, solid, is the 4th state of material.Use Cement Composite Treated by Plasma fabric, fabric or fiber surface is first through plasma bombardment, its surface impurity is come off under the collision many times of plasma this " elastic sphere ", or the adhesion that makes impurity and fiber becomes loose or be vaporized, thereby greatly improve hydrophily and the hygroscopicity of fabric.
The surface light grafting of polymer, the glycerol polymerization that utilizes exactly ultraviolet light trigger monomer to carry out at polymer surfaces, radical polymerization mechanism is followed in reaction.The surface grafting polymerization (surface light connects skill) that ultraviolet light causes has two outstanding features: (1) ultraviolet light is poorer to the penetration power of material than high-energy radiation, therefore carry out on surface or sub-surface that glycerol polymerization can be strict is limited to material, bulk properties that can damaged material; (2) light source of ultra-violet radiation and equipment cost are low, are easy to continuous operation; (3) easy control of reaction system.Utilize ultraviolet surface graft technology can greatly improve hydrophily, antistatic behaviour, biocompatibility of fabric etc.
Alkali treatment is also a kind of mode of fabric being carried out to surface modification, and traditional fabric alkali treatment mode is that fabric is carried out to alkali treatment under the acting in conjunction of bleeding agent and promoter (being generally quaternary ammonium salt promoter).In general, fabric construction is tight, and hydrophily is not fine, but in the alkali lye of high concentration, particularly, under high temperature action, some in fabric becomes branch to be hydrolyzed, and at fabric face, forms rough vestige, fabric attenuated and have good hydrophily.
While doing dressing use with pure bacteria cellulose, because it can absorb the liquid that wound oozes out, and there is good gas permeability, can greatly shorten wound healing time, but also can be used as the carrier of medicine, dress a wound, slow releasing pharmaceutical.But, because pure bacteria cellulose is comparatively soft, easily bonding, is difficult for being fitted in wound, and has limited its use as dressing.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of bacteria cellulose/fabric laminar composite and preparation method thereof, a kind of preparation method of bacteria cellulose/fabric laminar composite of once-forming is particularly provided, and fabric is processed to improve hydrophilic moisture retention through oxygen plasma, ultraviolet radiation graft, aqueous slkali, strengthen the physical bond between itself and bacteria cellulose, using and make up in prior art defect when bacteria cellulose and fabric are used as dressing respectively, thus the effect when improving the two and using as dressing.
A preparation method for bacteria cellulose/fabric laminar composite, comprises the steps:
(1) by acetobacter xylinum (Gluconacetobacter xylinus) access fluid nutrient medium, be placed in 150-200rpm, in the low temperature shaking table of 25-30 ℃, until there is floccule to produce in culture medium;
(2) fabric is cut into suitable size, with low-temperature oxygen plasma, ultraviolet surface graft or aqueous slkali, processes; Fabric is taken out and to be placed in container, after sterilizing, transfer them in the baking oven of 60-80 ℃ and dry;
(3) get above-mentioned flocculent culture medium and be placed in culture dish, processed good fabric is spread on bacterium liquid, more flocculent culture medium is added on fabric, be placed in the biochemical cultivation case of 25-30 ℃, until form laminar composite;
(4) under normal temperature, above-mentioned gained composite is soaked after 2-4 days with deionized water, use 0.1-0.3molL
-1sodium hydroxide solution soak two days, finally with deionized water, be dipped to again neutral.
The whole operating process of the above operates under aseptic condition.
The pore diameter range of described fabric is 5-200 micron, and porosity is 40%-90%, and thickness is 0.1-1.5mm, and weight per unit area is 10-300g/m
2.
Described fabric is jute, cotton, wood pulp, polyacrylic acid, nylon, polyethylene, polypropylene, polyester or viscose.
The power output 100-300W that described low-temperature oxygen plasma is processed, chamber pressure 1.0 * 10-1.0 * 10
2pa, the time is 4-7min.
Described fabric is processed and is comprised gas phase Graft Method and liquid-phase grafting method with ultraviolet radiation graft, gas phase grafting refers to fabric and treats that grafted monomers acrylic acid, light trigger benzophenone solution are placed in same closed container, pass into inert gas, heating makes the evaporation of light trigger benzophenone, benzophenone photosensitizer molecule in gaseous state produces initator free radical under UV-irradiation, capture the hydrogen atom of fabric face, produce surface free radical, trigger monomer molecule acrylic acid generation graft reaction (photosensitizer also can be coated in fabric face in advance); Liquid-phase grafting refers to fabric is directly placed in and treats that the solution that grafted monomers acrylic acid, photosensitizer benzophenone and auxiliary agent water are made into carries out UV-irradiation grafting.
Described aqueous slkali is the high-temperature water solution of alkali or the ethanolic solution of alkali.
Described fabric sterilization method is: high temperature and high pressure steam sterilizing, ethylene oxide sterilizing or absolute ethyl alcohol sterilizing.
In described fluid nutrient medium, add the nutritional labeling of high bioactivity, the nutritional labeling of described high bioactivity comprises carbohydrate, lipid, protein and peptide class etc.
The composition of described fluid nutrient medium is: in 1L Coconut Juice, contain dusty yeast 5-20g, peptone 5-15g, MgSO
40.1-1.0g, CaCl
20.1-0.6g, glucose 15-30g.
Bacteria cellulose/fabric laminar composite prepared by said method, through once-forming gained, by three-decker, formed, mid portion is fabric, the upper and lower two-layer bacteria cellulose that is respectively, bacteria cellulose better sticks to the upper and lower surface of fabric, and the microfiber of bacteria cellulose is penetrated in the middle of fabric.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention is compound with the fabric of processing through oxygen plasma, ultraviolet radiation graft, aqueous slkali etc. by bacteria cellulose, can greatly improve the affinity of single fabric and tissue on the one hand, improve guarantor's fluidity energy and the transdermal absorption factor of fabric, and the hydrophilic moisture retention of the fabric after oxygen plasma, ultraviolet radiation graft, aqueous slkali etc. are processed is better, can realize well compound with bacteria cellulose; Meanwhile, easy bonding, the shortcoming that is difficult for laminating when also having improved single bacteria cellulose and using as dressing, operates more easyly when bacteria cellulose is used as dressing, greatly improve the effect of its use.
(2) the present invention is successfully combined with each other bacteria cellulose and fabric, and once-forming is convenient and swift.The compound rear obvious biocompatibility that improves fabric, protect fluidity energy, ventilative water permeability and transdermal absorption factor, and the bacteria cellulose after compound can better be fitted in wound, so as dress a wound, slow releasing pharmaceutical.Range of application when in a word, the successful preparation of bacteria cellulose/fabric laminar composite has expanded further the two and uses as dressing.
(3) bacteria cellulose/fabric laminar composite of the present invention is 12.00-19.50g/g according to the conventional in the world test surface of a wound by the hygroscopicity scope that the hygroscopic method of dressing records its Unit Weight, and in blank group, the hygroscopicity of the Unit Weight of fabric is 5.20-9.22g/g.The hygroscopicity of composite of the present invention is good.
(4) bacteria cellulose/fabric laminar composite of the present invention is in diffusivity experimental test, and the altitude range that after 5min, liquid climbs on this material is 60.0-90.0mm, and the altitude range climbing on blank fabric is only 5.0-20.0mm.The diffusivity of composite of the present invention is good.
Accompanying drawing explanation
Fig. 1 is the Electronic Speculum figure of the bacterial fibers vegetarian noodles of embodiment 1 bacteria cellulose/fabric laminar composite;
Fig. 2 is the Electronic Speculum figure of embodiment 1 bacteria cellulose/fabric laminar composite section; Wherein b is the partial enlarged drawing of a;
Fig. 3 is fabric photo under the microscope in embodiment 1, and a is 4 times of enlarged drawings, and b is 40 times of enlarged drawings.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention, but the present invention is not limited in following embodiment.
Embodiment 1
(1) bacterial classification amplification, gets in a ring acetobacter xylinum access fluid nutrient medium, is placed in 150rpm, in the low temperature shaking table of 30 ℃, until there is floccule to produce in culture medium;
(2) polypropylene fabric is cut into the circle that diameter is 15cm, then at power output 300W, chamber pressure 1.0 * 10
2under the condition of Pa, by low-temperature oxygen plasma, process 7min.Fabric is taken out and to be placed in container, adopt in the baking oven that transfers them to 60 ℃ after 121 ℃ of high temperature 0.1MPa autoclavings and dry;
(3) the above-mentioned culture medium of getting 10mL is placed in the culture dish that diameter is 15cm, processed good polypropylene fabric is spread on bacterium liquid, again 5mL culture medium is added on fabric, be placed in the biochemical cultivation case of 25 ℃, until formation laminar composite, the aperture of polypropylene fabric is 5 microns, and porosity is 40%, thickness is 0.3mm, and weight per unit area is 300g/m
2;
(4) under normal temperature, above-mentioned gained composite is used to 0.1molL with deionized water immersion after 2 days
-1sodium hydroxide solution soak two days, finally with deionized water, be dipped to again neutral.
Wherein Liquid Culture based component is in 1L Coconut Juice, to contain dusty yeast 20g, peptone 5g, MgSO
41.0g, CaCl
20.1g, glucose 15g.
Gained bacteria cellulose/fabric laminar composite is carried out to SEM observation, find that bacteria cellulose better sticks to the upper and lower surface of fabric, and the microfiber of bacteria cellulose has been penetrated in the middle of fabric, can be referring to Fig. 1 Fig. 2.In above-described embodiment, the microstructure of fabric used can be referring to Fig. 3.
Gained bacteria cellulose/fabric laminar composite is carried out respectively to hygroscopicity and diffusion test, and the hygroscopicity that records its Unit Weight is 12.00g/g, and the height that after 5min, liquid climbs on material is 60.00mm.In 80 people's experiment, have 78 people feel bacteria cellulose and the compound rear use of fabric more convenient.
Embodiment 2
(1) bacterial classification amplification, gets in a ring acetobacter xylinum access fluid nutrient medium, is placed in 170rpm, in the low temperature shaking table of 30 ℃, until there is floccule to produce in culture medium;
(2) megila is cut into the square that the length of side is 10cm, then uses gas phase ultraviolet radiation graft technical finesse fabric.Fabric is taken out and to be placed in container, adopt in the baking oven that transfers them to 60 ℃ after ethylene oxide sterilizing and dry;
(3) the above-mentioned culture medium of getting 16mL is placed in culture dish, processed good megila is spread on bacterium liquid, again 4mL culture medium is added on fabric, be placed in the biochemical cultivation case of 26 ℃, until formation laminar composite, the aperture of megila is 40 microns, and porosity is 60%, thickness is 0.1mm, and weight per unit area is 110g/m
2;
(4) under normal temperature, above-mentioned gained composite is used to 0.1molL with deionized water immersion after 3 days
-1sodium hydroxide solution soak two days, finally with deionized water, be dipped to again neutral.
Wherein Liquid Culture based component is in 1L Coconut Juice, to contain dusty yeast 18g, peptone 10g, MgSO
40.8g, CaCl
20.4g, glucose 20g.
Wherein fabric is that photosensitizer dibenzoyl peroxide is coated in to megila surface by the processing mode of gas phase ultraviolet radiation graft technology, after being placed in closed container heating, utilize ultraviolet light acrylamide triggered at megila surface generation graft reaction, UV-irradiation time 30min.
Gained bacteria cellulose/fabric laminar composite is carried out respectively to hygroscopicity and diffusion test, and the hygroscopicity that records its Unit Weight is 13.00g/g, and the height that after 5min, liquid climbs on material is 63.00mm.
Embodiment 3
(1) under aseptic condition, getting 5g glutathione adds in the fluid nutrient medium having prepared;
(2) bacterial classification amplification, gets in a ring acetobacter xylinum access aforesaid liquid culture medium, is placed in 200rpm, in the low temperature shaking table of 25 ℃, until there is floccule to produce in culture medium;
(3) nylon fabrics cutting being grown into 10cm wide is the rectangle of 8cm, then with 80 ℃ of high-temperature water solution of potassium hydroxide, carries out surface treatment 12h, finally with deionized water, processes to neutral.Fabric is taken out and to be placed in container, adopt in the baking oven that transfers them to 60 ℃ after absolute ethyl alcohol sterilizing and dry;
(4) the above-mentioned culture medium of getting 20mL is placed in culture dish, processed good nylon fabrics is spread on bacterium liquid, again 5mL culture medium is added on fabric, be placed in the biochemical cultivation case of 28 ℃, until formation laminar composite, the aperture of nylon fabrics is 200 microns, and porosity is 90%, thickness is 1.5mm, and weight per unit area is 10g/m
2;
(5) under normal temperature, above-mentioned gained composite is used to 0.1molL with deionized water immersion after 3 days
-1soaking with sodium hydroxide two days, finally with deionized water, be dipped to again neutral.
Wherein Liquid Culture based component is in 1L Coconut Juice, to contain dusty yeast 12g, peptone 10g, MgSO
41.0g, CaCl
20.5g, glucose 18g.
Gained bacteria cellulose/fabric laminar composite is carried out respectively to hygroscopicity and diffusion test, and the hygroscopicity that records its Unit Weight is 15.00g/g, and the height that after 5min, liquid climbs on material is 72.50mm.
Embodiment 4
(1) under aseptic condition, getting 10g collagen adds in the fluid nutrient medium having prepared;
(2) bacterial classification amplification, gets in a ring acetobacter xylinum access aforesaid liquid culture medium, is placed in 180rpm, in the low temperature shaking table of 29 ℃, until there is floccule to produce in culture medium;
(3) cutting of polyacrylic acid fabric is grown into 13cm wide for the rectangle of 7cm, then by low-temperature oxygen plasma, process 4min.Fabric is taken out and to be placed in container, adopt in the baking oven that transfers them to 60 ℃ after high temperature and high pressure steam sterilizing and dry;
(4) the above-mentioned culture medium of getting 24mL is placed in the culture dish that diameter is 15cm, processed good polyacrylic acid fabric is spread on bacterium liquid, again 6mL culture medium is added on fabric, be placed in the biochemical cultivation case of 27 ℃, until formation laminar composite, the aperture of polyacrylic acid fabric is 140 microns, and porosity is 65%, thickness is 0.5mm, and weight per unit area is 200g/m
2;
(5) under normal temperature, above-mentioned gained composite is used to 0.1molL with deionized water immersion after 3 days
-1soaking with sodium hydroxide two days, finally with deionized water, be dipped to again neutral.
Wherein Liquid Culture based component is in 1L Coconut Juice, to contain dusty yeast 5g, peptone 15g, MgSO
40.1g, CaCl
20.6g, glucose 30g.
Gained bacteria cellulose/fabric laminar composite is carried out respectively to hygroscopicity and diffusion test, and the hygroscopicity that records its Unit Weight is 17.00g/g, and the height that after 5min, liquid climbs on material is 81.00mm.
Embodiment 5
(1) bacterial classification amplification, gets in a ring acetobacter xylinum access fluid nutrient medium, is placed in 160rpm, in the low temperature shaking table of 29 ℃, until there is floccule to produce in culture medium;
(2), by the square of polyethylene fabric cutting growth 15cm, then use liquid phase ultraviolet radiation graft technical finesse fabric.Fabric is taken out and to be placed in container, adopt in the baking oven that transfers them to 60 ℃ after ethylene oxide sterilizing and dry;
(3) the above-mentioned culture medium of getting 30mL is placed in the culture dish that diameter is 15cm, processed good polyethylene fabric is spread on bacterium liquid, again 6mL culture medium is added on fabric, be placed in the biochemical cultivation case of 30 ℃, until formation laminar composite, the aperture of polyethylene fabric is 140 microns, and porosity is 55%, thickness is 0.6mm, and weight per unit area is 220g/m
2;
(4) under normal temperature, above-mentioned gained composite is soaked to the soaking with sodium hydroxide two days use afterwards 0.1molL-1 for 4 days with deionized water, finally with deionized water, be dipped to again neutral.
Wherein Liquid Culture based component is in 1L Coconut Juice, to contain dusty yeast 20g, peptone 5g, MgSO
40.5g, CaCl
20.3g, glucose 18g.
Wherein fabric is to using benzophenone as photosensitizer by the processing mode of liquid phase ultraviolet radiation graft technology, utilizes ultraviolet light to cause acrylic acid, on polyethylene fabric surface, liquid-phase grafting reaction occurs.
Gained bacteria cellulose/fabric laminar composite is carried out respectively to hygroscopicity and diffusion test, and the hygroscopicity that records its Unit Weight is 18.00g/g, and the height that after 5min, liquid climbs on material is 87.86mm.
Embodiment 6
(1) bacterial classification amplification, gets in a ring acetobacter xylinum access fluid nutrient medium, is placed in 190rpm, in the low temperature shaking table of 26 ℃, until there is floccule to produce in culture medium;
(2) polyester textile is cut into the circle that diameter is 15cm, then with the ethanolic solution of NaOH, processes fabric, finally with deionized water, process to neutral.Fabric is taken out and to be placed in container, adopt in the baking oven that transfers them to 60 ℃ after absolute ethyl alcohol sterilizing and dry.
(3) the above-mentioned culture medium of getting 30mL is placed in the culture dish that diameter is 15cm, processed good polyester textile is spread on bacterium liquid, again 10mL culture medium is added on fabric, be placed in the biochemical cultivation case of 29 ℃, until formation laminar composite, the aperture of polyester textile is 170 microns, and porosity is 70%, thickness is 0.8mm, and weight per unit area is 160g/m
2;
(4) under normal temperature, above-mentioned gained composite is used to 0.1molL with deionized water immersion after 4 days
-1soaking with sodium hydroxide two days, finally with deionized water, be dipped to again neutral.
Wherein Liquid Culture based component is in 1L Coconut Juice, to contain dusty yeast 18g, peptone 8g, MgSO
41.0g, CaCl
20.1g, glucose 20g.
Gained bacteria cellulose/fabric laminar composite is carried out respectively to hygroscopicity and diffusion test, and the hygroscopicity that records its Unit Weight is 19.50g/g, and the height that after 5min, liquid climbs on material is 90.00mm.
Claims (10)
1. a preparation method for bacteria cellulose/fabric laminar composite, is characterized in that, comprises the steps:
(1) by acetobacter xylinum (Gluconacetobacter xylinus) access fluid nutrient medium, be placed in 150-200rpm, in the low temperature shaking table of 25-30 ℃, until there is floccule to produce in culture medium;
(2) fabric is cut into suitable size, with low-temperature oxygen plasma, ultraviolet surface graft or aqueous slkali, processes; Fabric is taken out and to be placed in container, after sterilizing, transfer them in the baking oven of 60-80 ℃ and dry;
(3) get above-mentioned flocculent culture medium and be placed in culture dish, processed good fabric is spread on bacterium liquid, more flocculent culture medium is added on fabric, be placed in the biochemical cultivation case of 25-30 ℃, until form laminar composite;
(4) under normal temperature, above-mentioned gained composite is soaked after 2-4 days with deionized water, use 0.1-0.3molL
-1sodium hydroxide solution soak two days, finally with deionized water, be dipped to again neutral.
2. method according to claim 1, is characterized in that, the pore diameter range of described fabric is 5-200 micron, and porosity is 40%-90%, and thickness is 0.1-1.5mm, and weight per unit area is 10-300g/m
2.
3. method according to claim 2, is characterized in that, described fabric is jute, cotton, wood pulp, polyacrylic acid, nylon, polyethylene, polypropylene, polyester or viscose.
4. according to the method described in claim 1 or 2 or 3, it is characterized in that the power output 100-300W that described low-temperature oxygen plasma is processed, chamber pressure 1.0 * 10-1.0 * 10
2pa, the time is 4-7min.
5. according to the method described in claim 1 or 2 or 3, it is characterized in that, described fabric is processed and is comprised gas phase Graft Method and liquid-phase grafting method with ultraviolet radiation graft, gas phase grafting refers to fabric and treats that grafted monomers, photoinitiator solution are placed in same closed container, pass into inert gas, heating makes light trigger evaporation, photosensitizer molecule in gaseous state produces initator free radical under UV-irradiation, capture the hydrogen atom of fabric face, produce surface free radical, trigger monomer molecule generation graft reaction; Liquid-phase grafting refers to fabric is directly placed in and treats that the solution that grafted monomers, photosensitizer and auxiliary agent are made into carries out UV-irradiation grafting.
6. according to the method described in claim 1 or 2 or 3, it is characterized in that the high-temperature water solution that described aqueous slkali is alkali or the ethanolic solution of alkali.
7. according to the method described in claim 1 or 2 or 3, it is characterized in that, described fabric sterilization method is: high temperature and high pressure steam sterilizing, ethylene oxide sterilizing or absolute ethyl alcohol sterilizing.
8. according to the method described in claim 1 or 2 or 3, it is characterized in that, in described fluid nutrient medium, add the nutritional labeling of high bioactivity, the nutritional labeling of described high bioactivity comprises carbohydrate, lipid, protein and peptide class.
9. method according to claim 8, is characterized in that, the composition of described fluid nutrient medium is: in 1L Coconut Juice, contain dusty yeast 5-20g, peptone 5-15g, MgSO
40.1-1.0g, CaCl
20.1-0.6g, glucose 15-30g.
10. bacteria cellulose/fabric laminar composite that prepared by claim 1～9 any one method, it is characterized in that, it is comprised of three-decker, mid portion is fabric, the upper and lower two-layer bacteria cellulose that is respectively, bacteria cellulose sticks to the upper and lower surface of fabric, and the microfiber of bacteria cellulose is penetrated in the middle of fabric.
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