CN103144382A - Nano fibrillated natural high-polymer-reinforced transparent composite film and preparation method thereof - Google Patents
Nano fibrillated natural high-polymer-reinforced transparent composite film and preparation method thereof Download PDFInfo
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Abstract
The invention provides a nano fibrillated natural high-polymer-reinforced transparent composite film and a preparation method thereof, relating to the field of a transparent composite film and a preparation method thereof. The invention aims to solve the problem that the film prepared by the existing reinforced transparent film method has higher mechanical properties but much lower transparency. The nano fibrillated natural high-polymer-reinforced transparent composite film is prepared from a first transparent film layer, a second nano fibrillated natural high-polymer sandwich layer and a third transparent film layer. The preparation method comprises the following steps: 1. preparing a nano fibrillated natural high-polymer dispersion solution; 2. preparing the first transparent film layer; 3. preparing the second sandwich layer on the first transparent film layer; and 4. preparing the third transparent film layer on the sandwich layer. The tensile strength of the transparent composite film can reach 60.5 MPa, and the transparency reaches 89.2%; and the film is continuous, uniform, soft and flexible. The invention is applicable to the field of composite films.
Description
Technical field
The present invention relates to a kind of transparent composite film and preparation method thereof.
Background technology
The nanofibrils natural polymer has the advantages such as nanometer level superfine yardstick, high strength, high-specific surface area, high length-diameter ratio, extensively is present in the various biological materials such as various forest tree castoffs, plant stem, waste newspaper, cotton, fiber crops, bamboo, stalk, bagasse and shrimp shell, crab shell.How Efficient Development utilizes the nanofibrils natural macromolecular material is the outer emphasis of paying close attention to and studying of Present Domestic.
Self-assembling technique refers to that the construction units such as molecule and nano particle are not in the situation that there is no outside interference, spontaneously found into the process of the aggregation of Thermodynamically stable, Stability Analysis of Structures, organization regulation by the non-covalent bond effect, self assembling process by simulating nature circle improves existing or finds new high performance material, and then make the functional material that makes new advances, be mainly to utilize between molecule to have the process of the aggregation of certain 26S Proteasome Structure and Function by the spontaneous formation of non-covalent bond active force (comprising electrostatic interaction, Van der Waals force, hydrophobic effect power, hydrogen bond etc.).Self-assembling technique is as a kind of interface Supramolecular Assembling technology, can be used for the nanofibrils natural polymer and other macromolecular materials prepare new material by hydrogen bond action.
Existing transparent membrane exists the shortcoming that matter is crisp, hot strength is not high, easy to crack, can't satisfy the requirement of growing engineering, thereby has limited the further application of transparent membrane.For improving these shortcomings of transparent membrane, that people have adopted is monomer modified to resin modified, Film synthesis, it is organic to add or inorganic filler improves the mechanical property of film, but when thin film mechanical performance improves, it is very serious that the transparency of film but descends, have a strong impact on transparent membrane range of application and use field.
Summary of the invention
The present invention will solve film that the method for existing enhancing transparent membrane prepares when strengthening mechanical property, the transparency serious problems that but descend, and transparent composite film that a kind of nanofibrils natural polymer strengthens and preparation method thereof is provided.
The transparent composite film that a kind of nanofibrils natural polymer strengthens is composited by ground floor transparent membrane, second layer nanofibrils natural polymer sandwich of layers and the 3rd layer of transparent membrane.
Described nanofibrils natural polymer is the nanofibrils of cellulose or chitin, and the diameter of nanofibrils natural polymer is not more than 100nm, and length is greater than 10 μ m.
Described transparent membrane is polyvinyl alcohol transparent membrane, PLA transparent membrane, melamine transparent membrane, pollopas transparent membrane, transparent epoxy resin film or polyethylene transparent membrane.
The preparation method of the transparent composite film that a kind of nanofibrils natural polymer strengthens, specifically complete according to the following steps:
One, the nanofibrils natural polymer is disperseed in dispersant, be mixed with mass percent concentration and be 0.01%～15% nanofibrils natural polymer dispersion liquid;
Two, the film forming liquid of preparation transparent membrane;
Three, with the film forming liquid of transparent membrane, adopt the tape casting, prepared the ground floor transparent membrane;
Four, the nanofibrils natural polymer dispersion liquid that step 1 is obtained is dispersed on the ground floor transparent membrane that step 3 obtains, nature curtain coating stratification, air-dry under room temperature, obtain being coated with the ground floor transparent membrane of second layer nanofibrils natural polymer sandwich of layers;
Five, with the film forming liquid of transparent membrane, adopt the tape casting, on the second layer nanofibrils natural polymer sandwich of layers that step 4 obtains, prepare the 3rd layer of transparent membrane, namely completed the preparation of the transparent composite film of nanofibrils natural polymer enhancing.
Described nanofibrils natural polymer is the nanofibrils of cellulose or chitin, and the diameter of nanofibrils natural polymer is not more than 100nm, and length is greater than 10 μ m.
Described dispersant is a kind of in distilled water, deionized water, ethanol, acetone, cyclohexane, the tert-butyl alcohol and dimethyl sulfoxide (DMSO) or several mixture wherein, wherein, in mixture each component be arbitrarily than.
Described transparent membrane is polyvinyl alcohol transparent membrane, PLA transparent membrane, melamine transparent membrane, pollopas transparent membrane, transparent epoxy resin film or polyethylene transparent membrane.
The film forming liquid of the transparent membrane in described step 2 is for the preparation of transparent membrane, and the mass percent concentration of film forming liquid is 0.5%～15%,
The tape casting of described step 3, specifically complete according to the following steps: the film forming liquid of getting transparent membrane prolongs the stream film forming on smooth polyfluortetraethylene plate, and with polytetrafluoroethylene (PTFE) scraper plate drawout, drying has namely obtained the first transparent membrane; The tape casting of described step 5, specifically complete according to the following steps: the film forming liquid of getting transparent membrane prolongs the stream film forming on second layer nanofibrils natural polymer sandwich of layers, and with polytetrafluoroethylene (PTFE) scraper plate drawout, drying has namely obtained the 3rd layer of transparent membrane.
The method of described drying is natural wind dry method and vacuum drying oven seasoning.
Advantage of the present invention: one, the transparent composite film of a kind of nanofibrils natural polymer enhancing provided by the invention, hot strength can reach 60.5MPa, hot strength with respect to existing polyvinyl alcohol transparent membrane is 41.4MPa, improved 46%, simultaneously, the transparency of transparent composite film provided by the invention can realize under the prerequisite that guarantees transparency the mechanical property of enhanced film still up to 89.2%;
Two, the preparation method of the transparent composite film of a kind of nanofibrils natural polymer enhancing provided by the invention, technique is simple, can generate homogeneous, transparent high-quality laminated film through simple curtain coating, the transparent composite film for preparing continuously, homogeneous, soft bent.
Description of drawings
Fig. 1 is the mechanism figure of the transparent composite film of the nanofibrils natural polymer enhancing of test one;
Fig. 2 is the transparent composite film photomacrograph figure of the nanofibrils natural polymer enhancing of test one;
Fig. 3 is the scanning electron microscope diagram of the transparent composite film of the nanofibrils natural polymer enhancing of test one.
The specific embodiment
The specific embodiment one: present embodiment is the transparent composite film that a kind of nanofibrils natural polymer strengthens, and is prepared from by ground floor transparent membrane, second layer nanofibrils natural polymer sandwich of layers and the 3rd layer of transparent membrane.
Present embodiment selects film forming matter as matrix, utilize dispersant in nanofibrils natural polymer dispersion liquid with its surface active swollen, make the ground floor film expose top layer hydroxyl and nanofibrils natural polymer generation hydrogen bond action, absorption is deposited on the film top layer; Simultaneously, this directionally suction-operated makes the nanofibrils natural polymer with high-crystallinity closely be arranged on transparent thin film layer, avoid the nanofibrils natural polymer to relax and arranged on the impact of light transmittance, thereby made laminated film have the characteristics of high transmission rate, high stretch strong and high thermal stability.
The advantage of present embodiment: one, the transparent composite film that strengthens of a kind of nanofibrils natural polymer that provides of present embodiment, hot strength can reach 60.5MPa, hot strength with respect to existing polyvinyl alcohol transparent membrane is 41.4MPa, improved 46%, simultaneously, the transparency of the transparent composite film that present embodiment provides can realize under the prerequisite that guarantees transparency the mechanical property of enhanced film still up to 89.2%; Two, the preparation method of the transparent composite film that strengthens of a kind of nanofibrils natural polymer that provides of present embodiment, technique is simple, can generate homogeneous, transparent high-quality laminated film through simple curtain coating, the transparent composite film for preparing continuously, homogeneous, soft bent.
The specific embodiment two: the difference of present embodiment and the specific embodiment one is: described nanofibrils natural polymer is the nanofibrils of cellulose or chitin, and the diameter of nanofibrils natural polymer is not more than 100nm, and length is greater than 10 μ m.Other is identical with the specific embodiment one.
The specific embodiment three: present embodiment and the specific embodiment one or twos' difference is: described transparent membrane is polyvinyl alcohol transparent membrane, PLA transparent membrane, melamine transparent membrane, pollopas transparent membrane, transparent epoxy resin film or polyethylene transparent membrane.Other is identical with the specific embodiment one or two.
The specific embodiment four: the preparation method that present embodiment provides a kind of transparent composite film of nanofibrils natural polymer enhancing, specifically complete according to the following steps:
One, the nanofibrils natural polymer is disperseed in dispersant, being mixed with mass percent concentration is 0.01%～15% nanofibrils natural polymer dispersion liquid;
Two, the film forming liquid of preparation transparent membrane;
Three, with the film forming liquid of transparent membrane, adopt the tape casting, prepared the ground floor transparent membrane;
Four, the nanofibrils natural polymer dispersion liquid that step 1 is obtained is dispersed on the ground floor transparent membrane that step 3 obtains, nature curtain coating stratification, air-dry under room temperature, obtain being coated with the ground floor transparent membrane of second layer nanofibrils natural polymer sandwich of layers;
Five, with the film forming liquid of transparent membrane, adopt the tape casting, on the second layer nanofibrils natural polymer sandwich of layers that step 4 obtains, prepare the 3rd layer of transparent membrane, namely completed the preparation of the transparent composite film of nanofibrils natural polymer enhancing.
Present embodiment selects film forming matter as matrix, utilize dispersant in nanofibrils natural polymer dispersion liquid with its surface active swollen, make the ground floor film expose top layer hydroxyl and nanofibrils natural polymer generation hydrogen bond action, absorption is deposited on the film top layer; Simultaneously, this directionally suction-operated makes the nanofibrils natural polymer with high-crystallinity closely be arranged on transparent thin film layer, avoid the nanofibrils natural polymer to relax and arranged on the impact of light transmittance, thereby prepared high transmission rate, the high stretching by force and the laminated film of high thermal stability.
The advantage of present embodiment: one, the transparent composite film that strengthens of a kind of nanofibrils natural polymer that provides of present embodiment, hot strength can reach 60.5MPa, hot strength with respect to existing polyvinyl alcohol transparent membrane is 41.4MPa, improved 46%, simultaneously, the transparency of the transparent composite film that present embodiment provides can realize under the prerequisite that guarantees transparency the mechanical property of enhanced film still up to 89.2%; Two, the preparation method of the transparent composite film that strengthens of a kind of nanofibrils natural polymer that provides of present embodiment, technique is simple, can generate homogeneous, transparent high-quality laminated film through simple curtain coating, the transparent composite film for preparing continuously, homogeneous, soft bent.
The specific embodiment five: the difference of present embodiment and the specific embodiment four is: described nanofibrils natural polymer is the nanofibrils of cellulose or chitin, and the diameter of nanofibrils natural polymer is not more than 100nm, and length is greater than 10 μ m.Other is identical with the specific embodiment four.
The specific embodiment six: present embodiment and the specific embodiment four or fives' difference is: described dispersant is a kind of in distilled water, deionized water, ethanol, acetone, cyclohexane, the tert-butyl alcohol and dimethyl sulfoxide (DMSO) or several mixture wherein.Other is identical with the specific embodiment four or five.
In the described mixture of present embodiment each component be arbitrarily than.
The specific embodiment seven: the difference of one of present embodiment and specific embodiment four to six is: described transparent membrane is polyvinyl alcohol transparent membrane, PLA transparent membrane, melamine transparent membrane, pollopas transparent membrane, transparent epoxy resin film or polyethylene transparent membrane.Other is identical with the specific embodiment four to six.
The specific embodiment eight: the difference of one of present embodiment and specific embodiment four to seven is: the film forming liquid of the transparent membrane in described step 2 is for the preparation of transparent membrane, and the mass percent concentration of film forming liquid is 0.5%～15%.Other is identical with the specific embodiment four to seven.
The specific embodiment nine: the difference of present embodiment and the specific embodiment four is: the tape casting of described step 3, specifically complete according to the following steps: the film forming liquid of getting transparent membrane prolongs the stream film forming on smooth polyfluortetraethylene plate, with polytetrafluoroethylene (PTFE) scraper plate drawout, drying has namely obtained the first transparent membrane; The tape casting of described step 5, specifically complete according to the following steps: the film forming liquid of getting transparent membrane prolongs the stream film forming on second layer nanofibrils natural polymer sandwich of layers, and with polytetrafluoroethylene (PTFE) scraper plate drawout, drying has namely obtained the 3rd layer of transparent membrane.Other is identical with the specific embodiment four.
The specific embodiment ten: the difference of present embodiment and the specific embodiment nine is: the method for described drying is natural wind dry method and vacuum drying oven seasoning.Other is identical with the specific embodiment nine.
Adopt following verification experimental verification effect of the present invention:
The transparent composite film that a kind of nanofibrils natural polymer strengthens is prepared from by ground floor polyvinyl alcohol transparent membrane, second layer nanofibrils natural polymer sandwich of layers and three-layer polyethylene alcohol transparent membrane.
The preparation method specifically completes according to the following steps:
One, the nanofibrils natural polymer is disperseed in deionized water, through vacuum defoamation, be mixed with mass percent concentration and be the aqueous dispersions of 0.5% nanofibrils natural polymer;
Two, the film forming liquid of preparation polyvinyl alcohol transparent membrane, vacuum defoamation; Wherein, the mass percent concentration of film forming liquid is for being 5%;
Three, with the film forming liquid of polyvinyl alcohol transparent membrane, plastic film mulch on smooth polyfluortetraethylene plate is used polytetrafluoroethylene (PTFE) scraper plate drawout, and is air-dry under room temperature, obtains polyvinyl alcohol film, prepared ground floor polyvinyl alcohol transparent membrane;
Four, the nanofibrils natural polymer dispersion liquid that step 1 is obtained is dispersed on the ground floor polyvinyl alcohol transparent membrane that step 3 obtains, nature curtain coating stratification, air-dry under room temperature, obtain being coated with the ground floor polyvinyl alcohol transparent membrane of second layer nanofibrils natural polymer sandwich of layers;
Five, with the film forming liquid of polyvinyl alcohol transparent membrane, adopt the tape casting, on the second layer nanofibrils natural polymer sandwich of layers that step 4 obtains, prepare three-layer polyethylene alcohol transparent membrane, namely completed the preparation of the transparent composite film of nanofibrils natural polymer enhancing.
The light transmittance of the transparent composite film that the nanofibrils natural polymer of test one strengthens is 89.2%, and hot strength is 60.5MPa, and purer polyvinyl alcohol transparent membrane (hot strength is 41.4MPa) has increased by 46%.
Fig. 1 is the mechanism figure of the transparent composite film of the nanofibrils natural polymer enhancing of test one.From Fig. 1, can observe this test selects the polyvinyl alcohol transparent membrane as matrix, utilize water in nanofibrils natural polymer dispersion liquid with its surface active swollen, make the ground floor film expose top layer hydroxyl and nanofibrils natural polymer generation hydrogen bond action, absorption is deposited on the film top layer; Simultaneously, this directionally suction-operated closely is arranged on transparent thin film layer the nanofibrils natural polymer with high-crystallinity, has avoided the nanofibrils natural polymer to relax and has arranged on the impact of light transmittance; The light transmittance of the transparent composite film that the nanofibrils natural polymer of test one strengthens is 89.2%, and hot strength is 60.5MPa, and purer polyvinyl alcohol transparent membrane (hot strength is 41.4MPa) has increased by 46%.
Fig. 2 is the transparent composite film photomacrograph figure of the nanofibrils natural polymer enhancing of test one.From Fig. 2, the composite transparent film surface that can observe preparation is smooth, can clearly see object thereafter, illustrates that this nanofibrils natural polymer is uniformly distributed in thin-film body and shows very high transparency.
Carry out scanning electron microscope test to testing the transparent composite film that one nanofibrils natural polymer strengthens, obtain Fig. 3.From Fig. 3, can observe the nanofibrils natural polymer and form one deck thin layer clearly, illustrate that the even film forming of nanofibrils natural polymer between two-layer base film, closely is arranged on transparent thin film layer, played good humidification.
Claims (10)
1. the transparent composite film that strengthens of a nanofibrils natural polymer, it is characterized in that: it is composited by ground floor transparent membrane, second layer nanofibrils natural polymer sandwich of layers and the 3rd layer of transparent membrane.
2. the transparent composite film that strengthens of a kind of nanofibrils natural polymer according to claim 1, it is characterized in that: described nanofibrils natural polymer is cellulose or chitin nanofibrils, and the diameter of nanofibrils natural polymer is not more than 100nm, and length is greater than 10 μ m.
3. the transparent composite film that strengthens of a kind of nanofibrils natural polymer according to claim 1 and 2, it is characterized in that: described transparent membrane is polyvinyl alcohol transparent membrane, PLA transparent membrane, melamine transparent membrane, pollopas transparent membrane, transparent epoxy resin film or polyethylene transparent membrane.
4. prepare the method for the transparent composite film of a kind of nanofibrils natural polymer enhancing as claimed in claim 1, it is characterized in that: the preparation method specifically completes according to the following steps:
One, the nanofibrils natural polymer is disperseed in dispersant, be mixed with mass percent concentration and be 0.01%～15% nanofibrils natural polymer dispersion liquid;
Two, the film forming liquid of preparation transparent membrane;
Three, with the film forming liquid of transparent membrane, adopt the tape casting, prepared the ground floor transparent membrane;
Four, the nanofibrils natural polymer dispersion liquid that step 1 is obtained is dispersed on the ground floor transparent membrane that step 3 obtains, nature curtain coating stratification, air-dry under room temperature, obtain being coated with the ground floor transparent membrane of second layer nanofibrils natural polymer sandwich of layers;
Five, with the film forming liquid of transparent membrane, adopt the tape casting, on the second layer nanofibrils natural polymer sandwich of layers that step 4 obtains, prepare the 3rd layer of transparent membrane, namely completed the preparation of the transparent composite film of nanofibrils natural polymer enhancing.
5. the preparation method of the transparent composite film that strengthens of a kind of nanofibrils natural polymer according to claim 4, it is characterized in that: described nanofibrils natural polymer is cellulose or chitin nanofibrils, and the diameter of nanofibrils natural polymer is not more than 100nm, and length is greater than 10 μ m.
6. the preparation method of the transparent composite film that strengthens of according to claim 4 or 5 described a kind of nanofibrils natural polymers is characterized in that: described dispersant is a kind of in distilled water, deionized water, ethanol, acetone, cyclohexane, the tert-butyl alcohol and dimethyl sulfoxide (DMSO) or several mixture wherein.
7. the preparation method of the transparent composite film that strengthens of according to claim 4 or 5 described a kind of nanofibrils natural polymers, it is characterized in that: described transparent membrane is polyvinyl alcohol transparent membrane, PLA transparent membrane, melamine transparent membrane, pollopas transparent membrane, transparent epoxy resin film or polyethylene transparent membrane.
8. the preparation method of the transparent composite film that strengthens of according to claim 4 or 5 described a kind of nanofibrils natural polymers, it is characterized in that: the film forming liquid in described step 2 is for the preparation of transparent membrane, and the mass percent concentration of film forming liquid is 0.5%～15%.
9. the preparation method of the transparent composite film that strengthens of a kind of nanofibrils natural polymer according to claim 4, it is characterized in that: the tape casting of described step 3, specifically complete according to the following steps: the film forming liquid of getting transparent membrane prolongs the stream film forming on smooth polyfluortetraethylene plate, with polytetrafluoroethylene (PTFE) scraper plate drawout, drying has namely obtained the first transparent membrane; The tape casting of described step 5, specifically complete according to the following steps: the film forming liquid of getting transparent membrane prolongs the stream film forming on second layer nanofibrils natural polymer sandwich of layers, and with polytetrafluoroethylene (PTFE) scraper plate drawout, drying has namely obtained the 3rd layer of transparent membrane.
10. the preparation method of the transparent composite film that strengthens of according to claim 4 or 9 described a kind of nanofibrils natural polymers, it is characterized in that: the method for described drying is natural wind dry method and vacuum drying oven seasoning.
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Application publication date: 20130612 |