CN103342825A - Preparation method of chitin nano-fiber/polyving akohol composite membrane - Google Patents
Preparation method of chitin nano-fiber/polyving akohol composite membrane Download PDFInfo
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Abstract
The invention provides a preparation method of a chitin nano-fiber/polyving akohol composite membrane. The preparation method comprises the following steps of: (1) preparing chitin nano-fibers; (2) preparing a chitin nano-fiber membrane; and (3) preparing the chitin nano-fiber/ polyving akohol composite membrane. The chitin nano-fibers prepared by the method has relatively high slenderness ratio, good optical transparency and relatively high heat stability; and the chitin nano-fiber/polyving akohol composite membrane has biodegradability. Known from a stereoscan photograph and a fiber diameter distribution diagram, when only grinding treatment is carried out at neutral environments, the nano-scale fibers cannot be obtained, and thick and big fiber bundles with the diameters mainly distributed in the range of above 100nm are obtained, after ultra-sounding and homogenizing are additionally carried out, the separation degree of the fibers is enhanced, the diameters of the fibers are distributed in the range of 30-70nm, and lots of the thick and big fiber bundles are separated, thus the relatively fine nano-scale fibers are basically obtained.
Description
Technical field
The present invention relates to a kind of preparation method of chitin nanofiber and the chitin nanofiber/composite membrane of polyvinyl alcohol that is obtained by this method, belong to the natural macromolecular material field, also the possession is in chemistry, Forestry Engineering, Packaging Engineering, field of new.
Background technology
Chitin mainly is present in the crustacean shell, as crab shell, shrimp shell, shrimp mushroom shell, king crab shell; The mollusk bone is as Endoconcha Sepiae etc.; Insect pupa and wing are as puparium, maggot skin, cicada slough; And in some microbial cell walls.And these animal shells etc. generally all are wastes, and are therefore with low cost.Because these waste bulk depositions pollute the environment, it is useful to environment to use it to chitin extraction again.Therefore had a lot of scientists to prove chitin itself and degraded product thereof to biological nontoxic, and the occurring in nature chitin content is huge, can be used as environmentally friendly material and be widely used.
Chitin is the abundant biological material of content that occurring in nature exists, and is a kind of inexhaustible, nexhaustible renewable resource.Only just contain a large amount of chitins in the annual shrimp and crab shells waste material that abandons, thereby tackle these waste materials and fully effectively utilize, can alleviate the pressure that these wastes bring environment on the one hand, the exploitation for the novel environment friendly material provides new approach on the other hand.
The content of chitin approximately is 20% ~ 25% in the Carapax Eriocheir sinensis, remaining material as: protein, fat, calcium carbonate, pigment and chitin are closely linked, diameter approximately is that the chitin nanofiber of 2 ~ 5nm has been formed the chitin micro-fibril, this diameter approximately is that the 300nm micro-fibril is embedded in the proteic matrix, has formed chitin-protein fibre.So obtain pure chitin nanofiber, will obtain pure chitin material by chemical treatments such as soda acids earlier, separate thick chitin fiber by mechanical treatment again, preparation chitin nanofiber.In addition, because the chitin nanofiber may form very strong hydrogen bond between fibrous bundle in drying process, this hydrogen bond be unfavorable for fibrous bundle separate fibre, the nanofiber that obtains high length-diameter ratio there is inhibition, so chitin is after having removed substrate substance, whole experiment will make sample remain under the moistening environment, generally sample is made into the aqueous solution or suspension is preserved.
Chitin nanofiber particle size as wild phase reaches Nano grade, and its unique microtexture impels the chitin nano-fiber composite material to have better more specifically optical property, thermal characteristics and mechanical property etc. than general chitin composite material.Chitin output height, source are a kind of biodegradable natural polymers extensively., with chitin nanofiber and a kind of advanced composite material of the compound acquisition of matrix resin, not only can increase approach and the efficient of the utilization of resources, and can alleviate environmental stress day by day under the serious situation in resource exhaustion, environmental degradation problem.
Chitin is the abundant biological material of content that occurring in nature exists, and is a kind of inexhaustible, nexhaustible renewable resource.Only just contain a large amount of chitins in the annual shrimp and crab shells waste material that abandons, thereby tackle these waste materials and fully effectively utilize, can alleviate the pressure that these wastes bring environment on the one hand, the exploitation for the novel environment friendly material provides new approach on the other hand.
Chitin fiber has stronger adsorptivity, biocompatibility, biodegradability and higher premium propertiess such as physical mechanical strength, and this makes the chitin nanofiber become a kind of strongthener of the nano composite material that gets most of the attention.The mass specific resistance value of chitin fiber is lower, far below 10
9Ω g/cm
2So the chitin fiber work in-process is difficult for producing static.These good characteristics that relative other fiber of chitin fiber shows have opened wide broader field for its development and use.
Summary of the invention
That the present invention proposes is a kind of preparation method of chitin nanofiber/composite membrane of polyvinyl alcohol, its purpose is intended to utilize the chitin nanofiber as the wild phase of polyvinyl alcohol, partial properties to polyvinyl alcohol is carried out modification, improves the performance quality such as resistance to impact shock, tensile strength, Young's modulus and second-order transition temperature of polyvinyl alcohol composite material.
Technical solution of the present invention: a kind of preparation method of chitin nanofiber/composite membrane of polyvinyl alcohol comprises 1) preparation chitin nanofiber; 2) preparation chitin nano fibrous membrane; 3) preparation chitin nanofiber/composite membrane of polyvinyl alcohol.
Chitin fiber has stronger adsorptivity, biocompatibility, biodegradability and higher premium propertiess such as physical mechanical strength, and this makes the chitin nanofiber become a kind of strongthener of the nano composite material that gets most of the attention.The mass specific resistance value of chitin fiber is lower, far below 10
9Ω g/cm
2So the chitin fiber work in-process is difficult for producing static.These good characteristics that relative other fiber of chitin fiber shows have opened wide broader field for its development and use.
Advantage of the present invention: 1) can improve the performance quality such as resistance to impact shock, tensile strength, Young's modulus and second-order transition temperature of polyvinyl alcohol composite material to the polyvinyl alcohol toughening modifying, make its range of application more extensive; 2) the chitin powder has been separated into tiny nanofibrils, and distribution of fiber diameters and is interweaved and reticulates tangled structure between 20 ~ 50nm.Compare with other technology, step is succinct, and easy handling is implemented; 3) chitin is cheap, processing is simple, and chitin nanofiber and a kind of performance of the compound acquisition of polyvinyl alcohol more are better than the matrix material of virgin resin, reduces production costs greatly;
4) chitin nanofiber/polyvinyl alcohol composite material has biodegradability.Stereoscan photograph and fiber diameter distribution profile are as can be known, only milled processed can't obtain required nano-scale fiber under neutral environment, what obtain is that diameter concentrates on the above fibrous bundle of 100nm, and after having increased ultrasonic and homogeneous, the fiber separation degree strengthens, diameter Distribution is between 30 ~ 70nm, and coarse fiber bundle is separated in a large number, has obtained meticulousr nanoscale fiber substantially.5) the present invention prepares the chitin nanometer and has higher slenderness ratio, the good optical transparency and higher thermostability.
Embodiment
A kind of preparation method of chitin nanofiber/composite membrane of polyvinyl alcohol, this method comprises 1) preparation chitin nanofiber; 2) preparation chitin nano fibrous membrane; 3) preparation chitin nanofiber/composite membrane of polyvinyl alcohol.
Described preparation chitin nanofiber comprises chemical treatment, mechanical treatment, wherein chemical treatment, and step is as follows:
(1) uses electronic balance accurately to take by weighing 10g 60 purpose chitin powder, in vacuum drying oven, dry 6h, be dissolved in the deionized water of 1000ml, be configured to the suspension of 1% concentration;
(2) under room temperature environment, the HCl processing chitin powder 24h with 7% concentration removes remaining calcium carbonate material in the chitin, is filtered to neutrality with a large amount of deionized waters afterwards;
(3) under room temperature environment, handle chitin about 12h that suspends with the NaOH/KOH of 5% concentration, remove remaining proteinaceous substances in the chitin, be filtered to neutrality with a large amount of deionized waters afterwards; This process will repeat four times to guarantee fully to remove proteinaceous substances;
(4) under room temperature environment, with this suspension of Ethanol Treatment 12h of 50% concentration, remove pigment composition, filter with a large amount of deionized water rinsings afterwards;
(5) obtained pure chitin through above step;
Described mechanical treatment, step is as follows:
(1) the chitin suspension that obtains is made into 0.2% solution, handles by shredder, the shredder rotating speed is 1500rpm, and spacing be-1.5, grinds acquisition chitin nanofiber solution respectively 5 ~ 15 times;
(2) this chitin nanofiber solution is prepared different chitin nanofibers with the method that ultrasonic wave vegetable cell pulverizer, high-pressure homogeneous instrument, supercentrifuge combine respectively again;
(3) combination is as follows: grind the ultrasonic 30min in back, grind the back homogeneous 10 times; Grind the ultrasonic 30min in back, homogeneous is 10 times again; Grind the ultrasonic 30min in back, homogeneous 10 times, last centrifugal 10min, rotating speed 10000r/min.
Described preparation chitin nano fibrous membrane, its method comprises:
(1) prepared chitin nanofiber solution being made into fiber concentration is 0.2% suspension, manually stirs to make with glass stick and pours in the B after chitin fiber is uniformly dispersed in this solution, opens vacuum pump and carries out suction filtration; The filter paper of the two-layer 9mm of pad or 7mm diameter in B earlier before the filter membrane, the millipore filtration with same diameter is attached to the filter paper surface again, with the wetting filter paper of deionized water and extrude bubble below the filter membrane, makes its smooth being laid in the B;
(2) suction filtration to deionized water is drained the back end fully, close vacuum pump, chitin nano fibrous membrane and the filter paper and the millipore filtration that fit together are together taken out from B, gently outermost tunica fibrosa is peeled away from filter membrane with have gentle hands, if the tunica fibrosa that leaches is too thin, then may cause tunica fibrosa to break with the filter membrane manual separation and then two kinds of membrane sepn need need not be put into together and taked corresponding measure again after baking oven is waited to dry earlier, obtain wet chitin nano fibrous membrane;
(3) this wet fiber film is sandwiched in the middle of two new filter paper, together places two sheet glass or iron plate (film shrinks crooked crumple when preventing from drying) again, put into about 55 ℃ electric heating constant temperature air dry oven and dried 24 ~ 48 hours.Treat to take out after fiber membrane is dried fully, make the chitin nano fibrous membrane.
Described preparation chitin nanofiber/composite membrane of polyvinyl alcohol comprises that miscible legal system is equipped with chitin nanofiber/composite membrane of polyvinyl alcohol and two kinds of methods of immersion process for preparing chitin nanofiber/composite membrane of polyvinyl alcohol; Wherein
Miscible legal system is equipped with chitin nanofiber/composite membrane of polyvinyl alcohol: chitin nanofiber solution and the polyvinyl alcohol water solution of measuring 150ml respectively, two kinds of solution are mixed, mix liquid with dispersion machine two kinds of solution are mixed, in air, leave standstill and slough bubble.Get an amount of mixing solutions and pour in the culture dish of specifying size (according to the amounts of the required mixing solutions of thickness different control curtain coating of the concentration of mixed solution and required composite membrane) into, guarantee not have in the mixed solution behind the bubble culture dish put into 55 ℃ vacuum drying oven drying 2 ~ 3 days.Culture dish is taken out in complete back to be dried, at room temperature takes the film in the culture dish off, namely makes chitin nanofiber/composite membrane of polyvinyl alcohol.
Immersion process for preparing chitin nanofiber/composite membrane of polyvinyl alcohol: get an amount of polyvinyl alcohol water solution and pour in the culture dish, the chitin nano fibrous membrane for preparing is in advance immersed in the polyvinyl alcohol solution gently with tweezers, and stir film and make it smooth and be dipped in the polyvinyl alcohol fully.In order to prevent that magazines such as koniology from polluting this solution, cover one deck preservative film at culture dish, at room temperature flood after about 12 hours tunica fibrosa is taken out, with suspension method sample being hung on temperature is in 55 ℃ the electric heating constant temperature air dry oven about about 12 hours, treat film oven dry back taking-up, namely make chitin nanofiber/composite membrane of polyvinyl alcohol.
Embodiment 1
The preparation method of chitin nanofiber and process: one, chemical treatment: (1) uses electronic balance accurately to take by weighing 10g 60 purpose chitin powder, dries 6h in vacuum drying oven, is dissolved in the deionized water of 1000ml, is configured to the suspension of 1% concentration.(2) under room temperature environment, the HCl processing chitin powder 24h with 7% concentration removes remaining calcium carbonate material in the chitin, is filtered to neutrality with a large amount of deionized waters afterwards.(3) under room temperature environment, handle chitin about 12h that suspends with the NaOH/KOH of 5% concentration, remove remaining proteinaceous substances in the chitin, be filtered to neutrality with a large amount of deionized waters afterwards; This process will repeat four times to guarantee fully to remove proteinaceous substances.(4) under room temperature environment, with this suspension of Ethanol Treatment 12h of 50% concentration, remove pigment composition, filter with a large amount of deionized water rinsings afterwards.Obtained pure chitin through above step.Two, mechanical treatment: the chitin suspension that obtains is made into 0.2% solution, handles by shredder, the shredder rotating speed is 1500rpm, and scale is adjusted to-1.5, grinds respectively 5 ~ 15 times, obtains chitin nanofiber solution.This chitin nanofiber solution is prepared different chitin nanofibers with the method that ultrasonic wave vegetable cell pulverizer, high-pressure homogeneous instrument, supercentrifuge combine respectively again.
Embodiment 2
Grind the ultrasonic 30min in back, grind the back homogeneous 10 times.
Embodiment 3
Grind the ultrasonic 30min in back, homogeneous is 10 times again.
Embodiment 4
Grind the ultrasonic 30min in back, homogeneous 10 times, last centrifugal 10min(rotating speed 10000r/min).
Embodiment 5
The preparation of chitin nano fibrous membrane: (1) is made into fiber concentration with prepared chitin nanofiber solution and is approximately 0.2% suspension, manually stir to make with glass stick and pour in the B after chitin fiber is uniformly dispersed in this solution, open vacuum pump and carry out suction filtration.The filter paper of the two-layer 9mm of pad or 7mm diameter in B earlier before the filter membrane, the millipore filtration with same diameter is attached to the filter paper surface again, with the wetting filter paper of deionized water and extrude bubble below the filter membrane, makes its smooth being laid in the B.(2) suction filtration to deionized water is drained the back end fully, close vacuum pump, chitin nano fibrous membrane and the filter paper and the millipore filtration that fit together are together taken out from B, gently outermost tunica fibrosa is peeled away (if the tunica fibrosa that leaches is too thin from filter membrane with have gentle hands, may cause tunica fibrosa to break with the filter membrane manual separation then earlier need not be with two kinds of membrane sepn, need put into together and take corresponding measure again after baking oven is waited to dry), obtain wet chitin nano fibrous membrane.(3) this wet fiber film is sandwiched in the middle of two new filter paper, together places two sheet glass or iron plate (film shrinks crooked crumple when preventing from drying) again, put into about 55 ℃ electric heating constant temperature air dry oven and dried 24 ~ 48 hours.Treat to take out after fiber membrane is dried fully, make the chitin nano fibrous membrane.(4) clear and reduce sample error for the uniform data that test experiments is obtained, need control the thickness of nano fibrous membrane well, because different mechanical processes are to the concentration requirement difference of fiber solution, the fiber solution concentration disunity of preparation, so the solubility of the nanofiber solution that will prepare according to different mechanical treatments during nano fibrous membrane in preparation and the diameter of required film are measured the fiber solution of respective amount, thus the gauge control that guarantees tunica fibrosa in a unified substantially scope to make things convenient for the carrying out of follow-up test experiment.
Embodiment 6
Take by weighing a certain amount of polyvinyl alcohol with electronic balance and pour in the beaker, add deionized water again, in beaker, put into a fritter magnetite.Beaker is placed the water-bath of heat collecting type magnetic force heating stirrer, design temperature is 80 ~ 90 ℃, in order to prevent that moisture is subjected to thermal evaporation, cover one deck preservative film at the beaker mouth, treat that polyvinyl alcohol dissolves the back fully and takes out from water-bath, at room temperature leave standstill cooling and slough bubble, namely make polyvinyl alcohol water solution.
Embodiment 7
Prepare the pure film of polyvinyl alcohol with casting method, get an amount of polyvinyl alcohol water solution and slowly pour (according to the concentration of polyvinyl alcohol and the different amounts of controlling the required polyvinyl alcohol of curtain coating of thickness of required pure film) in the culture dish of specifying size into, guarantee not have in the aqueous solution behind the bubble culture dish put into 55 ℃ dry about 2 days of vacuum drying oven, notice that time of drying can not be long, otherwise PVA (PVOH) FILM can can't be taken with the culture dish close adhesion off.Take out complete back to be dried, at room temperature takes film from culture dish off, namely makes pure polyvinyl alcohol film.
Embodiment 8
Miscible legal system is equipped with chitin nanofiber/composite membrane of polyvinyl alcohol: chitin nanofiber solution and the polyvinyl alcohol water solution of measuring 150ml respectively, two kinds of solution are mixed, mix liquid with dispersion machine two kinds of solution are mixed, in air, leave standstill and slough bubble.Get an amount of mixing solutions and pour in the culture dish of specifying size (according to the amounts of the required mixing solutions of thickness different control curtain coating of the concentration of mixed solution and required composite membrane) into, guarantee not have in the mixed solution behind the bubble culture dish put into 55 ℃ vacuum drying oven drying 2 ~ 3 days.Culture dish is taken out in complete back to be dried, at room temperature takes the film in the culture dish off, namely makes chitin nanofiber/composite membrane of polyvinyl alcohol.
Embodiment 9
Immersion process for preparing chitin nanofiber/composite membrane of polyvinyl alcohol: get an amount of polyvinyl alcohol water solution and pour in the culture dish, the chitin nano fibrous membrane for preparing is in advance immersed in the polyvinyl alcohol solution gently with tweezers, and stir film and make it smooth and be dipped in the polyvinyl alcohol fully.Pollute this solution in order to prevent koniology etc., cover one deck preservative film at culture dish, at room temperature flood after about 12 hours tunica fibrosa is taken out, with suspension method sample being hung on temperature is in 55 ℃ the electric heating constant temperature air dry oven about about 12 hours, treat film oven dry back taking-up, namely make chitin nanofiber/composite membrane of polyvinyl alcohol.In order to calculate fibre content in the composite membrane, with electronic balance weighing film weight and record, the fibre content of prepared composite membrane approximately is 60% in this experiment before and after dipping.
Embodiment 10: the mechanical property of the chitin nano fibrous membrane of different mechanical treatment preparations
Table 1: the mechanical property of the chitin nano fibrous membrane of different mechanical treatment preparations
Table 1 explanation, the mechanical performance data of the tunica fibrosa of different mechanical treatment preparations is done accurate analysis to the mechanical property of these different chitin nano fibrous membranes.After the grinding more ultrasonic tensile strength be 108.4MPa, Young's modulus is 5.1GPa, this compares numerical value after only grinding, and (81.7MPa 4.1GPa) has improved 32.7% and 24.4% respectively; Tensile strength and the Young's modulus of homogeneous are respectively 122.4MPa and 5.4 GPa again and after grinding, that compares only grinding has improved 49.8% and 31.7% respectively, and the elongation at break of the tunica fibrosa after the homogenization treatment is 5%, as seen chitin fiber to be carried out homogenization treatment more obvious than ultrasonic effect than grinding ultrasonic high 2.6%, higher to the raising degree of fibre property.When grind, ultrasonic and three kinds of mechanical means of homogeneous in conjunction with after, the tunica fibrosa performance of preparation increases again, tensile strength and Young's modulus are respectively 136.4MPa and 6.7Gpa, this processing that these three kinds of mechanical bond are described is strengthened the centrifugation of fiber, length-to-diameter ratio and the specific surface area of fiber are increased, and single fiber quality improves; And elongation at break is 4.7%, slightly descends before comparing, and the increase that physical strength be described can produce a bit the plasticity of fiber to be influenced, but effect is not clearly.Increasing high speed centrifugation at last on these three kinds of mechanical means bases again handles, tensile strength and the Young's modulus of the chitin nano fibrous membrane of preparation are respectively 162MPa and 7.2GPa, comparing does not increase the tunica fibrosa that three kinds of centrifugal mechanical bond are handled, the two performance has improved 18.8% and 7.5% respectively, elongation at break has reduction slightly again, so the fibre property for preparing after the centrifugal treating is best, because the thick fibrous bundle of failing to separate is separated by centrifugal force, remaining fiber all is high length-diameter ratios and finely dispersed, thereby can prepare high performance chitin nano fibrous membrane.
Embodiment 11
Different mechanical treatments are to the influence of film hot expansibility: only the thermal expansivity through the tunica fibrosa of milled processed preparation is 14.63ppm/K; Grind back ultrasonic and high-pressure homogeneous processing more respectively, the thermal expansivity of the tunica fibrosa that makes is respectively 13.04ppm/K and 12.12ppm/K; After having increased mechanical treatment as can be seen, the CTE of tunica fibrosa descends to some extent, the decline after ultrasonic about 10.8%, and it is about 17% to have descended after high-pressure homogeneous, visible homogenization treatment is stronger than ultrasonic to the separating effect of fiber; Grind, after ultrasonic and high-pressure homogeneous three kinds of methods combine, the CTE of tunica fibrosa has been reduced to 11.35ppm/K, only compare grind reduced by 22.4% again, the decline degree is than higher, as seen these three kinds of mechanical means in conjunction with the back to the action effect of chitin fibril clearly.
Claims (4)
1. the preparation method of a chitin nanofiber/composite membrane of polyvinyl alcohol is characterized in that this method comprises 1) preparation chitin nanofiber; 2) preparation chitin nano fibrous membrane; 3) preparation chitin nanofiber/composite membrane of polyvinyl alcohol.
2. according to the preparation method of the described a kind of chitin nanofiber/composite membrane of polyvinyl alcohol of claim 1, it is characterized in that described preparation chitin nanofiber, comprise chemical treatment, mechanical treatment, wherein chemical treatment, step is as follows:
(1) uses electronic balance accurately to take by weighing 10g 60 purpose chitin powder, in vacuum drying oven, dry 6h, be dissolved in the deionized water of 1000ml, be configured to the suspension of 1% concentration;
(2) under room temperature environment, the HCl processing chitin powder 24h with 7% concentration removes remaining calcium carbonate material in the chitin, is filtered to neutrality with a large amount of deionized waters afterwards;
(3) under room temperature environment, handle chitin about 12h that suspends with the NaOH/KOH of 5% concentration, remove remaining proteinaceous substances in the chitin, be filtered to neutrality with a large amount of deionized waters afterwards; This process will repeat four times to guarantee fully to remove proteinaceous substances;
(4) under room temperature environment, with this suspension of Ethanol Treatment 12h of 50% concentration, remove pigment composition, filter with a large amount of deionized water rinsings afterwards;
(5) obtained pure chitin through above step;
Described mechanical treatment, step is as follows:
(1) the chitin suspension that obtains is made into 0.2% solution, handles by shredder, the shredder rotating speed is 1500rpm, and spacing be-1.5, grinds acquisition chitin nanofiber solution respectively 5 ~ 15 times;
(2) this chitin nanofiber solution is prepared different chitin nanofibers with the method that ultrasonic wave vegetable cell pulverizer, high-pressure homogeneous instrument, supercentrifuge combine respectively again;
(3) combination is as follows: grind the ultrasonic 30min in back, grind the back homogeneous 10 times; Grind the ultrasonic 30min in back, homogeneous is 10 times again; Grind the ultrasonic 30min in back, homogeneous 10 times, last centrifugal 10min, rotating speed 10000r/min.
3. according to the preparation method of the described a kind of chitin nanofiber/composite membrane of polyvinyl alcohol of claim 1, it is characterized in that described preparation chitin nano fibrous membrane, its method comprises:
(1) prepared chitin nanofiber solution being made into fiber concentration is 0.2% suspension, manually stirs to make with glass stick and pours in the B after chitin fiber is uniformly dispersed in this solution, opens vacuum pump and carries out suction filtration; The filter paper of the two-layer 9mm of pad or 7mm diameter in B earlier before the filter membrane, the millipore filtration with same diameter is attached to the filter paper surface again, with the wetting filter paper of deionized water and extrude bubble below the filter membrane, makes its smooth being laid in the B;
(2) suction filtration to deionized water is drained the back end fully, close vacuum pump, chitin nano fibrous membrane and the filter paper and the millipore filtration that fit together are together taken out from B, gently outermost tunica fibrosa is peeled away from filter membrane with have gentle hands, if the tunica fibrosa that leaches is too thin, then may cause tunica fibrosa to break with the filter membrane manual separation and then two kinds of membrane sepn need need not be put into together and taked corresponding measure again after baking oven is waited to dry earlier, obtain wet chitin nano fibrous membrane;
(3) this wet fiber film is sandwiched in the middle of two new filter paper, together place two sheet glass or iron plate (film shrinks crooked crumple when preventing from drying) again, putting into about 55 ℃ electric heating constant temperature air dry oven dried 24 ~ 48 hours, treat to take out after fiber membrane is dried fully, make the chitin nano fibrous membrane.
4. according to the preparation method of the described a kind of chitin nanofiber/composite membrane of polyvinyl alcohol of claim 1, it is characterized in that described preparation chitin nanofiber/composite membrane of polyvinyl alcohol comprises that miscible legal system is equipped with chitin nanofiber/composite membrane of polyvinyl alcohol and two kinds of methods of immersion process for preparing chitin nanofiber/composite membrane of polyvinyl alcohol; Wherein
Miscible legal system is equipped with chitin nanofiber/composite membrane of polyvinyl alcohol: chitin nanofiber solution and the polyvinyl alcohol water solution of measuring 150ml respectively, two kinds of solution are mixed, mixing liquid with dispersion machine makes two kinds of solution mix about 5 ~ 10 minutes, in air, leave standstill and slough bubble, get an amount of mixing solutions and pour (according to the concentration of mixed solution and the different amounts of controlling the required mixing solutions of curtain coating of thickness of required composite membrane) in the culture dish of specifying size into, guarantee not have in the mixed solution behind the bubble culture dish put into 55 ℃ dry 2 ~ 3 days of vacuum drying oven, culture dish is taken out in complete back to be dried, at room temperature take the film in the culture dish off, namely make chitin nanofiber/composite membrane of polyvinyl alcohol;
Immersion process for preparing chitin nanofiber/composite membrane of polyvinyl alcohol: get an amount of polyvinyl alcohol water solution and pour in the culture dish, gently immerse in polyvinyl alcohol solution with tweezers the chitin nano fibrous membrane for preparing in advance, and stir film and make it smooth and be dipped in the polyvinyl alcohol fully, in order to prevent that magazines such as koniology from polluting this solution, cover one deck preservative film at culture dish, at room temperature flood after about 12 hours tunica fibrosa is taken out, with suspension method sample being hung on temperature is in 55 ℃ the electric heating constant temperature air dry oven about about 12 hours, treat film oven dry back taking-up, namely make chitin nanofiber/composite membrane of polyvinyl alcohol.
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| CN111925551A (en) * | 2020-08-17 | 2020-11-13 | 四川大学 | Natural polysaccharide composite material with brick-mud structure, preparation method and application |
| CN111925551B (en) * | 2020-08-17 | 2021-03-26 | 四川大学 | Natural polysaccharide composite material with brick-mud structure, preparation method and application |
| CN112691236A (en) * | 2020-12-24 | 2021-04-23 | 无锡中科光远生物材料有限公司 | Bionic Janus type chitin nanofiber membrane and preparation method thereof |
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| CN115198390A (en) * | 2022-07-28 | 2022-10-18 | 南京林业大学 | High-strength partially deacetylated chitin nanofiber-based composite silk thread and forming preparation method thereof |
| CN115198390B (en) * | 2022-07-28 | 2024-03-19 | 南京林业大学 | High-strength partially deacetylated chitin nanofiber-based composite yarn and molding preparation method thereof |
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