CN103483606B - A kind of preparation method of bacterial cellulose composite polymer superfine fiber material - Google Patents
A kind of preparation method of bacterial cellulose composite polymer superfine fiber material Download PDFInfo
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- CN103483606B CN103483606B CN201210190058.8A CN201210190058A CN103483606B CN 103483606 B CN103483606 B CN 103483606B CN 201210190058 A CN201210190058 A CN 201210190058A CN 103483606 B CN103483606 B CN 103483606B
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Abstract
The invention discloses a kind of preparation method of bacterial cellulose composite polymer superfine fiber material, comprise, by polymer dissolution in organic solvent, prepare uniform polymkeric substance spinning solution, method of electrostatic spinning is adopted to be penetrated from spinning nozzle by polymers soln, the polymers soln thread of injection is ejected on the bacteria cellulose diaphragm containing dehydrated alcohol and/or water, through aftertreatment, obtains bacterial cellulose composite polymer superfine fiber material.Preparation process of the present invention is simple, easy to operate, cost is low; Various bacteria Mierocrystalline cellulose composite polymer superfine fiber material can be prepared, expanded the Application Areas of bacteria cellulose composite material, there is very wide industrial applications prospect.
Description
Technical field
The present invention relates to matrix material and preparing technical field thereof, particularly a kind of preparation method of bacterial cellulose composite polymer superfine fiber material.
Background technology
Bacteria cellulose is the macromolecular compound be formed by connecting with β-Isosorbide-5-Nitrae-glycosidic linkage by glucose, and it, as a kind of excellent biomaterial, has the physics of its uniqueness, chemical property: bacteria cellulose has natural three-dimensional manometer network structure; High-tensile and Young's modulus; High-hydrophilic, good ventilative, water suction, water permeability, outstanding retentiveness and high wet strength; Higher biological fitness and good biodegradability; The Modulatory character etc. of performance during biosynthesizing.Therefore, bacteria cellulose has wide commercial use, as the tympanum, Wound care dressing, artificial skin, artificial blood vessel etc. of loud speaker.
In actual use in order to improve the performance of bacteria cellulose further, often obtain bacteria cellulose composite material with other materials compound.Bacteria cellulose composite material preparation method conventional at present has two kinds: one is dissolved in by bacteria cellulose in ionic liquid or other solvents to make solution, mix with another kind of or multiple polymers solution, prepare bacteria cellulose composite material (as Chinese patent CN101613893B) through working methods such as spinning.One adopts dipping method in bacteria cellulose, add polymers soln or polymer monomer initiated polymerization, prepares bacteria cellulose composite material (as Chinese patent CN102250378A, Chinese patent CN101274107A).These methods can obtain bacteria cellulose composite material, but in preparation process, often destroy the three-dimensional manometer network structure of bacteria cellulose itself, are difficult to prepare the mixture with ultra-fine fibre simultaneously.
Therefore, for terrible ultra-fine fibre matrix material keeps the original three-dimensional manometer network structure of bacteria cellulose simultaneously, this patent adopts method of electrostatic spinning, the dry method that squirts commonly used in electrostatic spinning is combined with dry method electrostatic spinning technique, prepares bacterial cellulose composite polymer superfine fiber material.Bacteria cellulose can be synthesized under suitable culture condition in the medium by various bacteria, as acetic acid Pseudomonas (Acetobacter), Agrobacterium (Agrobacterium), rhizobium (Rhizobium) and Sarcina (Sarcina) etc.Its conventional fermentation culture method is tray quiescent culture, after fermentation 4-8 days, the membranaceous cellulosic material of one deck can be formed on substratum top layer, in this application it is called bacteria cellulose diaphragm, its water content can reach more than 95%, and hydraulic pressure wherein goes out by the method by mechanically compress.The size of diaphragm and thickness are all by regulating incubation time to regulate.
Summary of the invention
The object of this invention is to provide a kind of preparation method of bacterial cellulose composite polymer superfine fiber material.Preparation process of the present invention is simple, easy to operate, cost is low; Various bacteria Mierocrystalline cellulose composite polymer superfine fiber material material can be prepared, expanded the Application Areas of bacteria cellulose composite material, there is very wide industrial applications prospect.
A kind of preparation method of bacterial cellulose composite polymer superfine fiber material, comprise, by polymer dissolution in organic solvent, preparation quality percentage ratio is the uniform polymeric spinning solution of 0.1-40%, method of electrostatic spinning is adopted to be penetrated from spinning nozzle by polymers soln, the polymers soln thread of injection is ejected on the bacteria cellulose diaphragm containing dehydrated alcohol and/or water, through aftertreatment, obtains bacterial cellulose composite polymer superfine fiber material.
As preferred technical scheme:
Wherein, the preparation method of a kind of bacterial cellulose composite polymer superfine fiber material as above, described fungin be by one or more outputs in acetobacter xylinum, rhizobium, Sarcina, Rhodopseudomonas, achromobacter, Alcaligenes, aerobacter or Azotobacter, the bacteria cellulose that obtains after the residual media that separating-purifying removes tropina and sticks on cellulose membrane.Separating and purifying method is a lot, as: bacteria cellulose can be immersed in mass percentage is in the NaOH aqueous solution of 1 ~ 8%, at the temperature of 60 ~ 100 DEG C, heat 3 ~ 6h.Repeatedly rinse to neutrality with redistilled water again.
The preparation method of a kind of bacterial cellulose composite polymer superfine fiber material as above, described polymkeric substance is for spinning superpolymer: chitosan, PGA, poly(lactic acid), PLGA, PPDO, polycaprolactone and/or gelatin.
The preparation method of a kind of bacterial cellulose composite polymer superfine fiber material as above, described organic solvent is aqueous acetic acid, hexafluoroisopropanol, trichloromethane, methylene dichloride, acetone and/or trifluoroethanol.When preparing polymkeric substance spinning solution, one or both above-mentioned solvents can be selected as mixed solvent, under mechanical agitation, make polymer dissolution.General solvent temperature is room temperature, and the heating that also can suitably heat up is to accelerate polymer dissolution rate.
The preparation method of a kind of bacterial cellulose composite polymer superfine fiber material as above, described method of electrostatic spinning, electrostatic spinning process is primarily of injection puopulsion unit, electrostatic power unit and bacteria cellulose receiving trap composition.The syringe that polymers soln is housed is installed on micro-puopulsion unit, and the syringe needle that internal diameter is 0.1-1.0 millimeter is equipped with in syringe front end, and syringe needle is connected with the positive pole of electrostatic power unit.Arranging electrostatic spinning voltage is 1-300kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 5.0-30cm.
The preparation method of a kind of bacterial cellulose composite polymer superfine fiber material as above, described bacteria cellulose diaphragm: the water content receiving the bacteria cellulose diaphragm of polymers soln thread is 50-90%(mass percent); Or bacteria cellulose diaphragm is extruded after most of water through mechanically compress, be immersed in dehydrated alcohol, made containing 50-90%(mass percent) the bacteria cellulose diaphragm of dehydrated alcohol.Solution contained in bacteria cellulose diaphragm also can select to have certain conductivity, volatile, can dissolve each other with spinning polymer solvent and be the organic solvent of polymkeric substance poor solvent.
The preparation method of a kind of bacterial cellulose composite polymer superfine fiber material as above, described bacteria cellulose diaphragm is fixed on dash receiver or swing roller, and is connected with the negative pole of electrostatic spinning apparatus.Bacteria cellulose film is the hygrometric state diaphragm containing conductive soln, can be laid on receiving trap by bacteria cellulose diaphragm, also bacteria cellulose diaphragm can be wrapped in swing roller surface.When electrostatic spinning, spray silk syringe needle is connected with the positive pole of electrostatic power unit, bacteria cellulose diaphragm is connected with the negative pole of electrostatic spinning apparatus, between syringe needle and bacteria cellulose diaphragm, produce electric field, and polymers soln thread uniform fold under the effect of electrical forces is surperficial at bacteria cellulose.Simultaneously polymers soln thread interacts with the solution in bacteria cellulose, and polymer solvent diffuses in bacterial cellulose solution, the shaping of promotion ultra-fine polymer fibre.
The preparation method of a kind of bacterial cellulose composite polymer superfine fiber material as above, the bacterial cellulose composite polymer superfine fiber material that described electrostatic spinning obtains is rinsed repeatedly through 30-100 DEG C of Temperature Treatment and/or distilled water, removing excess of solvent.Obtaining polymer superfine fibre diameter is between 100-1000nm, and ultra-fine fibre becomes network-like uniform fold to obtain bacterial cellulose composite polymer superfine fiber material on bacteria cellulose surface.
Compared with prior art, the invention has the beneficial effects as follows: adopt method of electrostatic spinning to prepare bacterial cellulose composite polymer superfine fiber material, while preparing polymer superfine fibre, maintain the original three-dimensional manometer network structure of bacteria cellulose.Preparation process of the present invention is simple, easy to operate, cost is low; Various bacteria Mierocrystalline cellulose composite polymer superfine fiber material can be prepared, expanded the Application Areas of bacteria cellulose composite material, there is very wide industrial applications prospect.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1:
(1) bacteria cellulose obtained by acetobacter xylinum fermentation culture being immersed in mass percentage is in the NaOH aqueous solution of 1%, heats 6h, more repeatedly rinse to neutrality with redistilled water at the temperature of 60 DEG C.Removing tropina and the residual media sticked on cellulose membrane.
(2) chitosan being dissolved in mass percent is in 0.1% aqueous acetic acid, is mixed with the chitosan aqueous acetic acid that mass percent is 0.1% under room temperature.The bacteria cellulose diaphragm containing dehydrated alcohol mass percent being 90% is covered on swing roller, and is connected with the negative pole of electrostatic spinning apparatus.Arranging electrostatic spinning voltage is 1kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 5.0cm.The Fibre diameter obtained is that the chitin fiber uniform fold of 100nm is on bacteria cellulose surface.Matrix material rinses to neutrality repeatedly through distilled water, obtains bacteria cellulose recombination chitosan filamentary material.
Embodiment 2:
(1) strain fermentation that can be synthesized bacteria cellulose by rhizobium being cultivated the bacteria cellulose obtained, to be immersed in mass percentage be in the NaOH aqueous solution of 2%, heats 5h, more repeatedly rinse to neutrality with redistilled water at the temperature of 70 DEG C.Removing tropina and the residual media sticked on cellulose membrane.
(2) PGA is dissolved in hexafluoroisopropanol, under room temperature, is mixed with the PGA solution that mass percent is 10%.The aqueous ethanolic solution containing dehydrated alcohol mass percent being 75% is immersed in bacteria cellulose diaphragm, make containing aqueous ethanolic solution mass percent be 50% bacteria cellulose diaphragm.Bacteria cellulose diaphragm is laid on dash receiver, and is connected with the negative pole of electrostatic spinning apparatus.Arranging electrostatic spinning voltage is 50kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 10.0cm.The Fibre diameter obtained is that the polyglycollide fibre uniform fold of 200nm is on bacteria cellulose surface.Matrix material is through 60 DEG C of pyroprocessing, and removing excess of solvent, obtains bacteria cellulose compound polyglycollide fibre material.
Embodiment 3:
(1) strain fermentation that can be synthesized bacteria cellulose by Sarcina being cultivated the bacteria cellulose obtained, to be immersed in mass percentage be in the NaOH aqueous solution of 3%, heats 4h, more repeatedly rinse to neutrality with redistilled water at the temperature of 80 DEG C.Removing tropina and the residual media sticked on cellulose membrane.
(2) poly(lactic acid) is dissolved in trichloromethane, under room temperature, is mixed with the PLA solution that mass percent is 1%.By moisture mass percent be 60% bacteria cellulose diaphragm cover on swing roller, and to be connected with the negative pole of electrostatic spinning apparatus.Arranging electrostatic spinning voltage is 100kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 15.0cm.The Fibre diameter obtained is that the acid fiber by polylactic uniform fold of 1000nm is on bacteria cellulose surface.Matrix material is through 80 DEG C of pyroprocessing, and removing excess of solvent, obtains bacteria cellulose composite polylactic acid filamentary material.
Embodiment 4:
(1) strain fermentation that can be synthesized bacteria cellulose by Rhodopseudomonas being cultivated the bacteria cellulose obtained, to be immersed in mass percentage be in the NaOH aqueous solution of 4%, heats 3h, more repeatedly rinse to neutrality with redistilled water at the temperature of 90 DEG C.Removing tropina and the residual media sticked on cellulose membrane.
(2) PLGA is dissolved in methylene dichloride, under room temperature, is mixed with the PLGA solution that mass percent is 20%.The aqueous ethanolic solution containing dehydrated alcohol mass percent being 90% is immersed in bacteria cellulose diaphragm, make containing aqueous ethanolic solution mass percent be 70% bacteria cellulose diaphragm.Bacteria cellulose diaphragm is laid on dash receiver, and is connected with the negative pole of electrostatic spinning apparatus.Arranging electrostatic spinning voltage is 300kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 20.0cm.The Fibre diameter obtained is that the PLGA fiber uniform fold of 800nm is on bacteria cellulose surface.Matrix material is through 100 DEG C of pyroprocessing, and removing excess of solvent, obtains bacteria cellulose composite polylactic acid ethanol copolymer filamentary material.
Embodiment 5:
(1) strain fermentation that can be synthesized bacteria cellulose by achromobacter being cultivated the bacteria cellulose obtained, to be immersed in mass percentage be in the NaOH aqueous solution of 5%, heats 3h, more repeatedly rinse to neutrality with redistilled water at the temperature of 100 DEG C.Removing tropina and the residual media sticked on cellulose membrane.
(2) PPDO is dissolved in hexafluoroisopropanol, under room temperature, is mixed with the PPDO solution that mass percent is 5%.The aqueous ethanolic solution containing dehydrated alcohol mass percent being 90% is immersed in bacteria cellulose diaphragm, make containing aqueous ethanolic solution mass percent be 80% bacteria cellulose diaphragm.Bacteria cellulose diaphragm is laid on dash receiver, and is connected with the negative pole of electrostatic spinning apparatus.Arranging electrostatic spinning voltage is 200kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 25.0cm.The Fibre diameter obtained is that the PPDO fiber uniform fold of 400nm is on bacteria cellulose surface.Matrix material is through 30 DEG C of pyroprocessing, and removing excess of solvent, obtains bacteria cellulose compound PPDO filamentary material.
Embodiment 6:
(1) strain fermentation that can be synthesized bacteria cellulose by Alcaligenes being cultivated the bacteria cellulose obtained, to be immersed in mass percentage be in the NaOH aqueous solution of 6%, heats 4h, more repeatedly rinse to neutrality with redistilled water at the temperature of 100 DEG C.Removing tropina and the residual media sticked on cellulose membrane.
(2) polycaprolactone is dissolved in acetone, under room temperature, is mixed with the polycaprolactone solution that mass percent is 15%.The bacteria cellulose diaphragm containing dehydrated alcohol mass percent being 80% is covered on swing roller, and is connected with the negative pole of electrostatic spinning apparatus.Arranging electrostatic spinning voltage is 150kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 30.0cm.The Fibre diameter obtained is that the polycaprolactone fiber uniform fold of 300nm is on bacteria cellulose surface.Matrix material is through 40 DEG C of pyroprocessing, and removing excess of solvent, obtains bacteria cellulose compound polycaprolactone filamentary material.
Embodiment 7:
(1) strain fermentation that can be synthesized bacteria cellulose by aerobacter being cultivated the bacteria cellulose obtained, to be immersed in mass percentage be in the NaOH aqueous solution of 7%, heats 5h, more repeatedly rinse to neutrality with redistilled water at the temperature of 100 DEG C.Removing tropina and the residual media sticked on cellulose membrane.
(2) gelatin is dissolved in trifluoroethanol, at 37 DEG C, is mixed with the gelatin solution that mass percent is 40%.The aqueous ethanolic solution containing dehydrated alcohol mass percent being 95% is immersed in bacteria cellulose diaphragm, make containing aqueous ethanolic solution mass percent be 60% bacteria cellulose diaphragm.Bacteria cellulose diaphragm is covered on swing roller, and is connected with the negative pole of electrostatic spinning apparatus.Arranging electrostatic spinning voltage is 250kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 15.0cm.The Fibre diameter obtained is that the gelatin fiber uniform fold of 500nm is on bacteria cellulose surface.Matrix material rinses repeatedly through distilled water, and removing excess of solvent, obtains bacteria cellulose composite gelatin filamentary material.
Embodiment 8:
(1) strain fermentation that can be synthesized bacteria cellulose by Azotobacter being cultivated the bacteria cellulose obtained, to be immersed in mass percentage be in the NaOH aqueous solution of 8%, heats 6h, more repeatedly rinse to neutrality with redistilled water at the temperature of 100 DEG C.Removing tropina and the residual media sticked on cellulose membrane.
(2) by polycaprolactone and poly(lactic acid) in mass ratio rate be that 1:1 is dissolved in methylene dichloride, be at room temperature mixed with polycaprolactone and poly(lactic acid) mixing solutions that mass percent is 10%.The aqueous ethanolic solution containing dehydrated alcohol mass percent being 80% is immersed in bacteria cellulose diaphragm, make containing aqueous ethanolic solution mass percent be 90% bacteria cellulose diaphragm.Bacteria cellulose diaphragm is laid on dash receiver, and is connected with the negative pole of electrostatic spinning apparatus.Arranging electrostatic spinning voltage is 250kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 20.0cm.The Fibre diameter obtained is that the polycaprolactone of 700nm and poly(lactic acid) blend fiber uniform fold are on bacteria cellulose surface.Matrix material is through 50 DEG C of pyroprocessing, and distilled water rinses repeatedly, and removing excess of solvent, obtains bacteria cellulose compound polycaprolactone and poly(lactic acid) blend fiber material.
The bacterial cellulose composite polymer superfine fiber material that the application obtains is on the basis keeping the original three-dimensional manometer network structure of bacteria cellulose, and be compounded with ultra-fine fibre, have excellent handlability, Application Areas is extensive.
Claims (5)
1. the preparation method of a bacterial cellulose composite polymer superfine fiber material, it is characterized in that: by polymer dissolution in organic solvent, preparation quality percentage ratio is the uniform polymeric spinning solution of 0.1-40%, method of electrostatic spinning is adopted to be penetrated from spinning nozzle by polymers soln, the polymers soln thread of injection is ejected on the bacteria cellulose diaphragm containing dehydrated alcohol, through aftertreatment, obtain bacterial cellulose composite polymer superfine fiber material; The described bacteria cellulose diaphragm containing dehydrated alcohol is extruded after most of water through mechanically compress by bacteria cellulose diaphragm, is immersed in dehydrated alcohol, makes the bacteria cellulose diaphragm containing mass percent 50-90% dehydrated alcohol; Described bacteria cellulose diaphragm is fixed on dash receiver or swing roller, and is connected with the negative pole of electrostatic spinning apparatus; Described aftertreatment be bacterial cellulose composite polymer superfine fiber material that method of electrostatic spinning is obtained through 30-100 DEG C of Temperature Treatment, more repeatedly to rinse with distilled water, removing excess of solvent.
2. the preparation method of bacterial cellulose composite polymer superfine fiber material according to claim 1, it is characterized in that: described polymkeric substance, for can spin superpolymer, comprising: chitosan, PGA, poly(lactic acid), PLGA, PPDO, polycaprolactone and/or gelatin.
3. the preparation method of bacterial cellulose composite polymer superfine fiber material according to claim 1, is characterized in that: described organic solvent is aqueous acetic acid, hexafluoroisopropanol, trichloromethane, methylene dichloride, acetone and/or trifluoroethanol.
4. the preparation method of bacterial cellulose composite polymer superfine fiber material according to claim 1, is characterized in that: the electrostatic spinning voltage of described method of electrostatic spinning is 1-300kV, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 5.0-30cm.
5. the preparation method of bacterial cellulose composite polymer superfine fiber material according to claim 1, it is characterized in that: polymer superfine fibre diameter prepared by described method of electrostatic spinning is between 100-1000nm, ultra-fine fibre becomes network-like uniform fold to obtain bacterial cellulose composite polymer superfine fiber material on bacteria cellulose surface.
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| CN104383585B (en) * | 2014-11-29 | 2016-08-24 | 山东省立医院 | A kind of three-dimensional manometer composite adhesive bandage and preparation and application thereof |
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| CN106757787B (en) * | 2016-12-20 | 2018-09-04 | 海南大学 | A kind of preparation method of the compound blood compatibility material of chitosan/bacterial cellulose sulfate ester |
| CN107177048B (en) * | 2017-05-12 | 2023-04-07 | 陕西科技大学 | Bacterial cellulose-polylactic acid composite membrane and preparation method thereof, and drug-loaded gauze based on composite membrane and preparation method thereof |
| CN108250460B (en) * | 2018-02-01 | 2021-07-30 | 浙江纺织服装职业技术学院 | Preparation method and application of cellulose solution |
| CN108273130B (en) * | 2018-02-27 | 2021-02-09 | 华东交通大学 | Three-dimensional micro-nano fiber composite support and preparation method thereof |
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| CN114351316B (en) * | 2022-01-13 | 2023-09-19 | 碧菲分离膜（大连）有限公司 | Nanometer bacterial cellulose superfine fiber processing equipment |
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| CN101302486A (en) * | 2008-05-21 | 2008-11-12 | 华中科技大学 | Acetobacter xylinum and method for preparing nano-cellulose skin tissue repair material by using the same |
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