CN103483606A - Preparation method of bacterial cellulose composite polymer superfine fiber material - Google Patents
Preparation method of bacterial cellulose composite polymer superfine fiber material Download PDFInfo
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- CN103483606A CN103483606A CN201210190058.8A CN201210190058A CN103483606A CN 103483606 A CN103483606 A CN 103483606A CN 201210190058 A CN201210190058 A CN 201210190058A CN 103483606 A CN103483606 A CN 103483606A
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Abstract
The invention discloses a preparation method of a bacterial cellulose composite polymer superfine fiber material. The method comprises following steps: dissolving polymers in an organic solvent to prepare a homogenous polymer spinning solution, ejecting the polymer spinning solution from a spinning nozzle by adopting an electrostatic spinning method, spraying the ejected polymer solution trickles on bacterial cellulose membranes, which contain absolution ethanol or water, and finally subjecting the processed bacterial cellulose membranes to a post-treatment so as to obtain the bacterial cellulose composite polymer superfine fiber material. The preparation method has the advantages of simple and practicable preparation process, convenient operation, and low cost; is capable of manufacturing a plurality of kinds of bacterial cellulose composite polymer superfine fiber materials, enlarges the application area of bacterial cellulose composite materials, and has a very vast industrial application prospect.
Description
Technical field
The present invention relates to matrix material and preparing technical field thereof, particularly a kind of preparation method of bacteria cellulose composition polymer super-fine 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 has its unique physics, chemical property as a kind of good biomaterial: 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; Modulatory character of performance etc. during biosynthesizing.Therefore, bacteria cellulose has wide commercial use, as the tympanum of loud speaker, Wound care dressing, artificial skin, artificial blood vessel etc.
In actual use in order further to improve the performance of bacteria cellulose, often with the compound bacteria cellulose composite material that obtains of other materials.Bacteria cellulose composite material preparation method commonly used has two kinds at present: a kind of is that bacteria cellulose is dissolved in ionic liquid or other solvents and makes solution, mix with another kind or multiple polymers solution, through working methods such as spinning, prepare bacteria cellulose composite material (as Chinese patent CN101613893B).A kind of is to adopt dipping method to add polymers soln or polymer monomer initiated polymerization in bacteria cellulose, prepares bacteria cellulose composite material (as Chinese patent CN102250378A, Chinese patent CN101274107A).These methods can make bacteria cellulose composite material, but tend to destroy the three-dimensional manometer network structure of bacteria cellulose itself in preparation process, 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 of commonly using in electrostatic spinning is combined with the dry method electrostatic spinning technique, prepare bacteria cellulose composition polymer super-fine fiber material.Bacteria cellulose can be synthetic in substratum under suitable culture condition by various bacteria, as acetic acid Pseudomonas (Acetobacter), Agrobacterium (Agrobacterium), rhizobium (Rhizobium) and Sarcina (Sarcina) etc.Its fermentation culture method commonly used is the standing cultivation of tray, after fermentation 4-8 days, can form the membranaceous cellulosic material of one deck on the substratum top layer, in this application it is called to the bacteria cellulose diaphragm, its water content can reach more than 95%, can hydraulic pressure wherein be gone out by the method for mechanically compress.The size of diaphragm and thickness all can be regulated by regulating incubation time.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of bacteria cellulose composition polymer super-fine fiber material.Preparation process of the present invention is simple, easy to operate, cost is low; Can prepare various bacteria Mierocrystalline cellulose composition polymer super-fine fiber material material, expand the Application Areas of bacteria cellulose composite material, there is very wide industrial applications prospect.
A kind of preparation method of bacteria cellulose composition polymer super-fine fiber material, comprise, by polymer dissolution in organic solvent, the uniform polymeric spinning solution that preparation quality percentage ratio is 0.1-40%, adopt method of electrostatic spinning that polymers soln is penetrated from spinning nozzle, the polymers soln thread penetrated is ejected on the bacteria cellulose diaphragm that contains dehydrated alcohol and/or water, through aftertreatment, obtains bacteria cellulose composition polymer super-fine fiber material.
As preferred technical scheme:
Wherein, the preparation method of a kind of bacteria cellulose composition polymer super-fine fiber material as above, described fungin be one or more outputs in acetobacter xylinum, rhizobium, Sarcina, Rhodopseudomonas, achromobacter, Alcaligenes, aerobacter or Azotobacter, remove tropina and stick to the bacteria cellulose obtained after the residual media on cellulose membrane through separating-purifying.Separating and purifying method is a lot, as: bacteria cellulose can be immersed in the NaOH aqueous solution that the quality percentage composition is 1～8%, at the temperature of 60～100 ℃, heat 3～6h.With redistilled water, repeatedly rinse to neutrality again.
The preparation method of a kind of bacteria cellulose composition polymer super-fine fiber material as above, described polymkeric substance is for can spin superpolymer: chitosan, PGA, poly(lactic acid), PLGA, PPDO, polycaprolactone and/or gelatin.
The preparation method of a kind of bacteria cellulose composition polymer super-fine 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, can select one or both above-mentioned solvents as mixed solvent, make polymer dissolution under mechanical agitation.General solvent temperature is room temperature, and the heating that also can suitably heat up is to accelerate polymer dissolution speed.
The preparation method of a kind of bacteria cellulose composition polymer super-fine fiber material as above, described method of electrostatic spinning, the electrostatic spinning process mainly is comprised of injection puopulsion unit, electrostatic power unit and bacteria cellulose receiving trap.The syringe that polymers soln is housed is installed on micro-puopulsion unit, and the syringe front end is equipped with the syringe needle that internal diameter is the 0.1-1.0 millimeter, and syringe needle is connected with the positive pole of electrostatic power unit.It is 1-300kV that electrostatic spinning voltage is set, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 5.0-30cm.
The preparation method of a kind of bacteria cellulose composition polymer super-fine fiber material as above, described bacteria cellulose diaphragm: the water content that receives the bacteria cellulose diaphragm of polymers soln thread is the 50-90%(mass percent); Or by the bacteria cellulose diaphragm after mechanically compress extrudes most of water, it is immersed in dehydrated alcohol, make the mass percent containing 50-90%() the bacteria cellulose diaphragm of dehydrated alcohol.In the bacteria cellulose diaphragm, contained solution also can be selected to have certain conductivity, volatile, can dissolve each other with the spinning polymer solvent and be the organic solvent of polymkeric substance poor solvent.
The preparation method of a kind of bacteria cellulose composition polymer super-fine 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 that contains conductive soln, the bacteria cellulose diaphragm can be laid on receiving trap, also the bacteria cellulose diaphragm can be wrapped in to the swing roller surface.When electrostatic spinning, spray silk syringe needle is connected with the positive pole of electrostatic power unit, the bacteria cellulose diaphragm is connected with the negative pole of electrostatic spinning apparatus, between syringe needle and bacteria cellulose diaphragm, produces electric field, the polymers soln thread under the effect of electrical forces uniform fold on the bacteria cellulose surface.Solution phase mutual effect in polymers soln thread and bacteria cellulose simultaneously, polymer solvent diffuses in bacterial cellulose solution, promotes ultra-fine polymer fibre to be shaped.
The preparation method of a kind of bacteria cellulose composition polymer super-fine fiber material as above, the bacteria cellulose composition polymer super-fine fiber material that described electrostatic spinning obtains rinses repeatedly through 30-100 ℃ of Temperature Treatment and/or distilled water, removes unnecessary solvent.Obtaining the polymer superfine fibre diameter is between 100-1000nm, and ultra-fine fibre becomes network-like uniform fold to obtain bacteria cellulose composition polymer super-fine fiber material on the bacteria cellulose surface.
Compared with prior art, the invention has the beneficial effects as follows: adopt method of electrostatic spinning to prepare bacteria cellulose composition polymer super-fine fiber material, kept the original three-dimensional manometer network structure of bacteria cellulose when preparing polymer superfine fibre.Preparation process of the present invention is simple, easy to operate, cost is low; Can prepare various bacteria Mierocrystalline cellulose composition polymer super-fine fiber material, expand the Application Areas of bacteria cellulose composite material, there is very wide industrial applications prospect.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are not used in and limit the scope of the invention for the present invention is described.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1:
(1) bacteria cellulose that will be obtained by the acetobacter xylinum fermentation culture is immersed in the NaOH aqueous solution that the quality percentage composition is 1%, heats 6h at the temperature of 60 ℃, more repeatedly rinses to neutrality with redistilled water.Remove tropina and stick to the residual media on cellulose membrane.
(2) chitosan being dissolved in to mass percent is in 0.1% aqueous acetic acid, the chitosan aqueous acetic acid that to be mixed with mass percent under room temperature be 0.1%.The bacteria cellulose diaphragm that will be 90% containing the dehydrated alcohol mass percent covers on swing roller, and is connected with the negative pole of electrostatic spinning apparatus.It is 1kV that electrostatic spinning voltage is set, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 5.0cm.The chitin fiber uniform fold that the Fibre diameter obtained is 100nm is on the 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 will can synthesize bacteria cellulose by rhizobium is cultivated the bacteria cellulose obtain and is immersed in the NaOH aqueous solution that the quality percentage composition is 2%, heats 5h at the temperature of 70 ℃, more repeatedly rinses to neutrality with redistilled water.Remove tropina and stick to the residual media on cellulose membrane.
(2) PGA is dissolved in hexafluoroisopropanol to the PGA solution that to be mixed with mass percent under room temperature be 10%.The aqueous ethanolic solution that will be 75% containing the dehydrated alcohol mass percent immerses in the bacteria cellulose diaphragm, the bacteria cellulose diaphragm that to make containing the aqueous ethanolic solution mass percent be 50%.The bacteria cellulose diaphragm is laid on dash receiver, and is connected with the negative pole of electrostatic spinning apparatus.It is 50kV that electrostatic spinning voltage is set, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 10.0cm.The polyglycollide fibre uniform fold that the Fibre diameter obtained is 200nm is on the bacteria cellulose surface.Matrix material, through 60 ℃ of pyroprocessing, is removed unnecessary solvent, obtains the compound polyglycollide fibre material of bacteria cellulose.
Embodiment 3:
(1) strain fermentation that will can synthesize bacteria cellulose by Sarcina is cultivated the bacteria cellulose obtain and is immersed in the NaOH aqueous solution that the quality percentage composition is 3%, heats 4h at the temperature of 80 ℃, more repeatedly rinses to neutrality with redistilled water.Remove tropina and stick to the residual media on cellulose membrane.
(2) poly(lactic acid) is dissolved in trichloromethane to the poly(lactic acid) solution that to be mixed with mass percent under room temperature be 1%.The bacteria cellulose diaphragm that is 60% by moisture mass percent covers on swing roller, and is connected with the negative pole of electrostatic spinning apparatus.It is 100kV that electrostatic spinning voltage is set, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 15.0cm.The acid fiber by polylactic uniform fold that the Fibre diameter obtained is 1000nm is on the bacteria cellulose surface.Matrix material, through 80 ℃ of pyroprocessing, is removed unnecessary solvent, obtains the compound acid fiber by polylactic material of bacteria cellulose.
Embodiment 4:
(1) strain fermentation that will can synthesize bacteria cellulose by Rhodopseudomonas is cultivated the bacteria cellulose obtain and is immersed in the NaOH aqueous solution that the quality percentage composition is 4%, heats 3h at the temperature of 90 ℃, more repeatedly rinses to neutrality with redistilled water.Remove tropina and stick to the residual media on cellulose membrane.
(2) PLGA is dissolved in methylene dichloride to the PLGA solution that to be mixed with mass percent under room temperature be 20%.The aqueous ethanolic solution that will be 90% containing the dehydrated alcohol mass percent immerses in the bacteria cellulose diaphragm, the bacteria cellulose diaphragm that to make containing the aqueous ethanolic solution mass percent be 70%.The bacteria cellulose diaphragm is laid on dash receiver, and is connected with the negative pole of electrostatic spinning apparatus.It is 300kV that electrostatic spinning voltage is set, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 20.0cm.The PLGA fiber uniform fold that the Fibre diameter obtained is 800nm is on the bacteria cellulose surface.Matrix material, through 100 ℃ of pyroprocessing, is removed unnecessary solvent, obtains the compound PLGA filamentary material of bacteria cellulose.
Embodiment 5:
(1) strain fermentation that will can synthesize bacteria cellulose by achromobacter is cultivated the bacteria cellulose obtain and is immersed in the NaOH aqueous solution that the quality percentage composition is 5%, heats 3h at the temperature of 100 ℃, more repeatedly rinses to neutrality with redistilled water.Remove tropina and stick to the residual media on cellulose membrane.
(2) PPDO is dissolved in hexafluoroisopropanol to the PPDO solution that to be mixed with mass percent under room temperature be 5%.The aqueous ethanolic solution that will be 90% containing the dehydrated alcohol mass percent immerses in the bacteria cellulose diaphragm, the bacteria cellulose diaphragm that to make containing the aqueous ethanolic solution mass percent be 80%.The bacteria cellulose diaphragm is laid on dash receiver, and is connected with the negative pole of electrostatic spinning apparatus.It is 200kV that electrostatic spinning voltage is set, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 25.0cm.The PPDO fiber uniform fold that the Fibre diameter obtained is 400nm is on the bacteria cellulose surface.Matrix material, through 30 ℃ of pyroprocessing, is removed unnecessary solvent, obtains the compound PPDO filamentary material of bacteria cellulose.
Embodiment 6:
(1) strain fermentation that will can synthesize bacteria cellulose by Alcaligenes is cultivated the bacteria cellulose obtain and is immersed in the NaOH aqueous solution that the quality percentage composition is 6%, heats 4h at the temperature of 100 ℃, more repeatedly rinses to neutrality with redistilled water.Remove tropina and stick to the residual media on cellulose membrane.
(2) polycaprolactone is dissolved in acetone to the polycaprolactone solution that to be mixed with mass percent under room temperature be 15%.The bacteria cellulose diaphragm that will be 80% containing the dehydrated alcohol mass percent covers on swing roller, and is connected with the negative pole of electrostatic spinning apparatus.It is 150kV that electrostatic spinning voltage is set, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 30.0cm.The polycaprolactone fiber uniform fold that the Fibre diameter obtained is 300nm is on the bacteria cellulose surface.Matrix material, through 40 ℃ of pyroprocessing, is removed unnecessary solvent, obtains the compound polycaprolactone filamentary material of bacteria cellulose.
Embodiment 7:
(1) strain fermentation that will can synthesize bacteria cellulose by aerobacter is cultivated the bacteria cellulose obtain and is immersed in the NaOH aqueous solution that the quality percentage composition is 7%, heats 5h at the temperature of 100 ℃, more repeatedly rinses to neutrality with redistilled water.Remove tropina and stick to the residual media on cellulose membrane.
(2) gelatin is dissolved in trifluoroethanol, is mixed with the gelatin solution that mass percent is 40% under 37 ℃.The aqueous ethanolic solution that will be 95% containing the dehydrated alcohol mass percent immerses in the bacteria cellulose diaphragm, the bacteria cellulose diaphragm that to make containing the aqueous ethanolic solution mass percent be 60%.The bacteria cellulose diaphragm is covered on swing roller, and be connected with the negative pole of electrostatic spinning apparatus.It is 250kV that electrostatic spinning voltage is set, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 15.0cm.The gelatin fiber uniform fold that the Fibre diameter obtained is 500nm is on the bacteria cellulose surface.Matrix material rinses repeatedly through distilled water, removes unnecessary solvent, obtains bacteria cellulose composite gelatin filamentary material.
Embodiment 8:
(1) strain fermentation that will can synthesize bacteria cellulose by Azotobacter is cultivated the bacteria cellulose obtain and is immersed in the NaOH aqueous solution that the quality percentage composition is 8%, heats 6h at the temperature of 100 ℃, more repeatedly rinses to neutrality with redistilled water.Remove tropina and stick to the residual media on cellulose membrane.
(2) by polycaprolactone and poly(lactic acid) in mass ratio rate be that 1:1 is dissolved in methylene dichloride, polycaprolactone and poly(lactic acid) mixing solutions that at room temperature to be mixed with mass percent be 10%.The aqueous ethanolic solution that will be 80% containing the dehydrated alcohol mass percent immerses in the bacteria cellulose diaphragm, the bacteria cellulose diaphragm that to make containing the aqueous ethanolic solution mass percent be 90%.The bacteria cellulose diaphragm is laid on dash receiver, and is connected with the negative pole of electrostatic spinning apparatus.It is 250kV that electrostatic spinning voltage is set, and the distance between spray silk syringe needle and bacteria cellulose diaphragm is 20.0cm.The polycaprolactone that the Fibre diameter obtained is 700nm and poly(lactic acid) blend fiber uniform fold are on the bacteria cellulose surface.Matrix material is through 50 ℃ of pyroprocessing, and distilled water rinses repeatedly, removes unnecessary solvent, obtains the compound polycaprolactone of bacteria cellulose and poly(lactic acid) blend fiber material.
The bacteria cellulose composition polymer super-fine fiber material that the application obtains, on the basis that keeps the original three-dimensional manometer network structure of bacteria cellulose, is compounded with ultra-fine fibre, has good handlability, and Application Areas is extensive.
Claims (9)
1. the preparation method of a bacteria cellulose composition polymer super-fine fiber material, it is characterized in that: by polymer dissolution in organic solvent, the uniform polymeric spinning solution that preparation quality percentage ratio is 0.1-40%, adopt method of electrostatic spinning that polymers soln is penetrated from spinning nozzle, the polymers soln thread penetrated is ejected on the bacteria cellulose diaphragm that contains dehydrated alcohol and/or water, through aftertreatment, obtain bacteria cellulose composition polymer super-fine fiber material.
2. the preparation method of bacteria cellulose composition polymer super-fine 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 bacteria cellulose composition polymer super-fine fiber material according to claim 1, it is characterized in that: described organic solvent is aqueous acetic acid, hexafluoroisopropanol, trichloromethane, methylene dichloride, acetone and/or trifluoroethanol.
4. the preparation method of bacteria cellulose composition polymer super-fine fiber material according to claim 1, it is characterized in that: the electrostatic spinning voltage of described method of electrostatic spinning is 1-300kV, between spray silk syringe needle and bacteria cellulose diaphragm apart from being 5.0-30cm.
5. the preparation method of bacteria cellulose composition polymer super-fine fiber material according to claim 1, it is characterized in that: the water content of described bacteria cellulose diaphragm is 50-90%; Or by the bacteria cellulose diaphragm after mechanically compress extrudes most of water, it is immersed in dehydrated alcohol, make the bacteria cellulose diaphragm containing mass percent 50-90% dehydrated alcohol.
6. the preparation method of bacteria cellulose composition polymer super-fine fiber material according to claim 1, it is characterized in that: described bacteria cellulose diaphragm is fixed on dash receiver or swing roller, and is connected with the negative pole of electrostatic spinning apparatus.
7. the preparation method of bacteria cellulose composition polymer super-fine fiber material according to claim 1, it is characterized in that: the bacteria cellulose composition polymer super-fine fiber material that described method of electrostatic spinning obtains rinses repeatedly through 30-100 ℃ of Temperature Treatment and/or distilled water, removes unnecessary solvent.
8. the preparation method of bacteria cellulose composition polymer super-fine 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, and ultra-fine fibre becomes network-like uniform fold to obtain bacteria cellulose composition polymer super-fine fiber material on the bacteria cellulose surface.
9. the bacteria cellulose composition polymer super-fine fiber material that the described preparation method of claim 1-8 any one prepares.
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| CN104383585A (en) * | 2014-11-29 | 2015-03-04 | 山东省立医院 | Three-dimensional nanocomposite adhesive bandage as well as preparation method and use method thereof |
| CN105113038A (en) * | 2015-06-24 | 2015-12-02 | 南通纺织丝绸产业技术研究院 | Material for diaphragm of loudspeaker and preparation method thereof |
| CN106757787A (en) * | 2016-12-20 | 2017-05-31 | 海南大学 | A kind of preparation method of the compound blood compatibility material of shitosan/bacterial cellulose sulfate ester |
| CN107177048A (en) * | 2017-05-12 | 2017-09-19 | 陕西科技大学 | A kind of bacteria cellulose polymeric lactic acid compound film and preparation method thereof and load medicine gauze and preparation method based on the composite membrane |
| CN108250460A (en) * | 2018-02-01 | 2018-07-06 | 浙江纺织服装职业技术学院 | A kind of preparation method and application of cellulose solution |
| CN108273130A (en) * | 2018-02-27 | 2018-07-13 | 华东交通大学 | A kind of three-D micro-nano fibrous composite scaffold and preparation method |
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| CN104383585A (en) * | 2014-11-29 | 2015-03-04 | 山东省立医院 | Three-dimensional nanocomposite adhesive bandage as well as preparation method and use method thereof |
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| CN105113038B (en) * | 2015-06-24 | 2017-05-31 | 南通纺织丝绸产业技术研究院 | A kind of loudspeaker diaphragm materials and preparation method thereof |
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| CN109091412A (en) * | 2018-09-20 | 2018-12-28 | 江南大学 | ALA-PDT light skin rejuvenating facial mask and preparation method thereof |
| CN110251728A (en) * | 2019-07-01 | 2019-09-20 | 北京诺康达医药科技股份有限公司 | It is a kind of biology surgical patch preparation method and based on this method preparation biological surgical patch |
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| CN114351316A (en) * | 2022-01-13 | 2022-04-15 | 张国拴 | Nanometer bacterial cellulose superfine fiber processing equipment |
| 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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