CN112094442A - Bacterial cellulose material with oriented helical structure and preparation method thereof - Google Patents
Bacterial cellulose material with oriented helical structure and preparation method thereof Download PDFInfo
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- CN112094442A CN112094442A CN201910526112.3A CN201910526112A CN112094442A CN 112094442 A CN112094442 A CN 112094442A CN 201910526112 A CN201910526112 A CN 201910526112A CN 112094442 A CN112094442 A CN 112094442A
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Abstract
The invention provides a preparation method of a bacterial cellulose material with an oriented helical structure, which comprises the following steps: stretching the hydrogel in a wet state in any one direction of a plane formed along the x direction and the y direction to obtain a primary treated hydrogel; the hydrogel is one or two of bacterial cellulose hydrogel and bacterial cellulose composite material hydrogel; stacking the primary treatment hydrogel layer by layer in sequence, wherein the stretching direction of the adjacent primary treatment hydrogel forms a certain angle, and compressing to obtain the bacterial cellulose material with the oriented spiral structure. The preparation method provided by the application obtains the bacterial cellulose material with an oriented spiral structure, which has extremely low thermal expansion rate, light weight, high strength and high impact resistance.
Description
Technical Field
The invention relates to the technical field of new material research, in particular to a bacterial cellulose material with an oriented helical structure and a preparation method thereof.
Background
The bacterial cellulose is an unbranched macromolecule formed by polymerizing glucose molecules through beta-1, 4 glycosidic bonds, and the linear glucose chains form a net structure through intramolecular and intermolecular hydrogen bonds; therefore, during the process of forming fibers by glucose, the molecules are subjected to characteristic polymerization and crystallization, and an ultrafine structure of the bacterial cellulose is formed, so that good mechanical properties of the bacterial cellulose are achieved. Therefore, the preparation of novel biological materials by using bacterial cellulose has important significance
The biological material is assembled by simple components with unobvious performance under relatively mild conditions, but shows excellent comprehensive mechanical properties and functional characteristics, which mainly benefits from the complex and ingenious organizational structure of the biological material spanning different scales, in particular to the unique deformation and fracture mechanism and toughening mechanism brought by the complex and ingenious organizational structure. Many organisms in nature construct high-strength and high-toughness materials through oriented spiral structures, for example, the fish skin of the salmon in Amazon river is constructed by one-dimensional nano fibers through oriented spiral structures, and the high-strength and high-toughness materials are good in strength and toughness so as to resist the attack of predators on predators for predation. Therefore, the development and preparation of new materials are of great importance by referring to the reinforcing mechanism and mechanism of the materials in the biological world.
Disclosure of Invention
The invention aims to provide a preparation method of a bacterial cellulose material with an oriented spiral structure, and the bacterial cellulose material with the oriented spiral structure has low thermal expansion rate, mechanical anisotropy and high impact resistance.
In view of the above, the present application provides a method for preparing a bacterial cellulose material with an oriented helical structure, comprising the steps of:
stretching the hydrogel in a wet state in any one direction of a plane formed along the x direction and the y direction to obtain a primary treated hydrogel; the hydrogel is one or two of bacterial cellulose hydrogel and bacterial cellulose composite material hydrogel;
stacking the primary treatment hydrogel layer by layer in sequence, wherein the stretching direction of the adjacent primary treatment hydrogel forms a certain angle, and compressing to obtain the bacterial cellulose material with the oriented spiral structure.
Preferably, the degree of wet stretching is from 1% to 50% of the initial length of the hydrogel.
Preferably, the degree of wet stretching is from 10% to 30% of the initial length of the hydrogel.
Preferably, the angle between adjacent primary treated hydrogels is from 0 ° to 180 °.
Preferably, the angle between adjacent primary treated hydrogels is from 10 ° to 80 °.
Preferably, the number of stacked layers is 20-3000.
Preferably, the compression temperature is 10-200 ℃, and the compression time is 1-800 MPa.
Preferably, the bacterial cellulose composite hydrogel is a hydrogel formed by one or more of a polymer and a nano material and bacterial cellulose.
The application also provides a bacterial cellulose material of orientation helical structure, including a plurality of hydrogel layers that the overlap was placed, the hydrogel layer is compressed after drawing by one or two kinds in bacterial cellulose hydrogel and the bacterial cellulose composite hydrogel and is obtained, tensile direction is the arbitrary orientation of the plane of x direction and the y direction formation of hydrogel, and the tensile direction of adjacent hydrogel layer is certain angle.
Preferably, the number of the hydrogel layers is 20-3000.
The application provides a preparation method of a bacterial cellulose material with an oriented spiral structure, which comprises the steps of firstly, carrying out wet-state stretching on hydrogel to obtain primary treatment hydrogel, then, stacking the primary treatment hydrogel layer by layer in sequence, ensuring that the stretching direction of the adjacent primary treatment hydrogel forms a certain angle, and compressing to obtain the bacterial cellulose material with the oriented spiral structure. This application is through stretching bacterial cellulose aquogel or bacterial cellulose composite material aquogel wet state, makes the nanocellulose that constitutes aquogel follow the orientation of tensile direction, will again the aquogel after the wet state is stretched piles up layer by layer, be certain angle along the tensile direction between the adjacent layer, the compression, at this in-process, produce strong hydrogen bond effect between the nanocellulose in the aquogel that has the micro orientation structure, it piles up to be certain angle and makes composite material have helical structure, these structural feature make the nanocellulose material except possessing cellulose panel nature, still have special mechanical properties, make composite material impact property promote like helical structure. In addition, the raw material adopted by the application is natural nano-cellulose which is safe, non-toxic and harmless and can be naturally degraded.
Drawings
FIG. 1 is a photograph of an oriented helical structured bacterial cellulose material prepared in example 1 of the present invention;
FIG. 2 is a photomicrograph (50 μm) of an oriented helical structured bacterial cellulose material prepared in example 1 of the present invention;
FIG. 3 is a photomicrograph (1 μm) of an oriented helical structured bacterial cellulose material prepared in example 1 of the present invention;
FIG. 4 is a bending stress-strain curve of an oriented helical structured bacterial cellulose material prepared in example 1 of the present invention;
FIG. 5 is a schematic drawing showing the direction of stretching of a hydrogel according to the present invention;
FIG. 6 is a drop weight impact graph of an oriented helical structured bacterial cellulose material prepared in example 1 of the present invention;
FIG. 7 is a photograph of an oriented helical structured bacterial cellulose material prepared in example 2 of the present invention;
FIG. 8 is a bending stress-strain curve of the bacterial cellulose bulk material with an oriented helical structure prepared in the embodiment 2 under different strains;
fig. 9 is a drop weight impact curve diagram of the bacterial cellulose bulk material with the oriented helical structure prepared in example 2 of the present invention.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
Aiming at the problem of preparing a high-performance bionic structure material in the prior art, the application provides a preparation method of a bacterial cellulose material with an oriented spiral structure, which is characterized in that orientation is realized by prestretching bacterial cellulose or a bacterial cellulose composite hydrogel, and the stretched bacterial cellulose membranes are spirally stacked layer by layer at a certain angle and compressed to obtain a bacterial cellulose material block material with an oriented spiral structure. The bacterial cellulose material prepared by the method has extremely low thermal expansion rate, light weight, high strength and high impact resistance.
During the preparation process of the bacterial cellulose material with the oriented spiral structure, firstly, the bacterial cellulose hydrogel or the bacterial cellulose composite hydrogel is subjected to wet state stretching along the plane direction, so that the nano cellulose forming the hydrogel is oriented along the stretching direction, then the bacterial cellulose hydrogel or the bacterial cellulose composite hydrogel after the wet state stretching is stacked layer by layer, the stretching direction between adjacent layers is at a certain angle, and the bacterial cellulose material with the oriented spiral structure is obtained after compression. Specifically, the embodiment of the invention discloses a preparation method of the bacterial cellulose material with the oriented helical structure, which comprises the following steps:
stretching the hydrogel in a wet state in any one direction of a plane formed along the x direction and the y direction to obtain a primary treated hydrogel; the hydrogel is one or two of bacterial cellulose hydrogel and bacterial cellulose composite material hydrogel;
stacking the primary treatment hydrogel layer by layer in sequence, wherein the stretching direction of the adjacent primary treatment hydrogel forms a certain angle, and compressing to obtain the bacterial cellulose material with the oriented spiral structure.
According to the present invention, in the process of preparing a bacterial cellulose material having an oriented helical structure, first, a hydrogel is stretched in a wet state in either direction of a plane formed in the x-direction and the y-direction to obtain an initial hydrogel; in the wet stretching process, nanocellulose constituting the hydrogel is oriented in the stretching direction, and the nanocellulose of the hydrogel is oriented. As shown in FIG. 5, FIG. 5 is a schematic drawing showing the direction of stretching of the hydrogel. In the wet stretching, the stretching direction is in either direction of a plane formed by the x direction and the y direction, and for example, the stretching direction may be in the x direction, the stretching direction may be in the y direction, or the stretching direction may be in the other direction within the plane. The bacterial cellulose is microscopically a network formed by a large number of one-dimensional nano fibers, and the nano fibers can be oriented and arranged along the stretching direction through wet stretching. The degree of wet stretching is 1% to 50% of the initial length of the hydrogel, and in particular embodiments, the degree of wet stretching is 10% to 30% of the initial length of the hydrogel. The wet stretching is a technique known to those skilled in the art, and there is no particular limitation in this application.
The hydrogel related to the application is one or two of bacterial cellulose hydrogel and bacterial cellulose composite hydrogel, wherein the bacterial cellulose composite hydrogel is hydrogel of one or more of high molecules and nanometer materials and bacterial cellulose. The sources of the bacterial cellulose hydrogel and the bacterial cellulose composite hydrogel are not particularly limited in the application, and the bacterial cellulose hydrogel and the bacterial cellulose composite hydrogel can be commercially available products and can also be prepared according to methods in the prior art.
And after the wet state stretching, stacking the obtained primary treatment hydrogel layer by layer, wherein the stretching direction of the adjacent primary treatment hydrogel forms a certain angle, and compressing to obtain the bacterial cellulose material with the oriented spiral structure. In the stacking process, the stretched bacterial cellulose hydrogels can be sequentially stacked, the stretched bacterial cellulose composite hydrogels can be sequentially stacked, and the stretched bacterial cellulose hydrogels and the stretched bacterial cellulose composite hydrogels can be sequentially stacked, so that the method is not particularly limited; also, the angles of adjacent layers to the stretching direction may be the same or different, and there is no particular limitation in this application. In the above stack, the interlaminar angle of adjacent as-treated hydrogels is between 0 ° and 180 °, and in particular embodiments, the interlaminar angle of adjacent as-treated hydrogels is between 10 ° and 80 °.
After the treatment, compressing the mixture at a certain temperature and under a certain pressure to obtain a multilayer structure material block; the compression temperature is 0-200 ℃, and the compression pressure is 1-200 MPa; in a specific embodiment, the mixing temperature is 30-120 ℃, and the mixing time is 20-150 MPa.
The application also provides a bacterial cellulose material with an oriented spiral structure prepared by the method, which comprises a plurality of hydrogel layers arranged in an overlapped mode, wherein the hydrogel layers are obtained by one or two of bacterial cellulose hydrogel and bacterial cellulose composite hydrogel through compression after stretching, the stretching direction is any direction of a plane formed by the x direction and the y direction of the hydrogel, and the stretching direction of the adjacent hydrogel layers is a certain angle.
In the bacterial cellulose material, the number of the hydrogel layers is 20-3000.
According to the method, the bacterial cellulose hydrogel or the bacterial cellulose composite hydrogel is stretched in a wet state along the plane direction, so that the nanocellulose forming the hydrogel is oriented in the stretching direction, the bacterial cellulose hydrogel or the bacterial cellulose composite hydrogel is stacked layer by layer after the hydrogel is stretched in the wet state, a certain angle is formed between adjacent layers along the stretching direction, and the bacterial cellulose block material with the oriented spiral structure is obtained by compression at a certain temperature and under pressure. The bacterial cellulose material has the properties of a nano cellulose block, the micro orientation structure enables the obtained block to have better mechanical strength, and the spiral structure enables the obtained block to have better impact strength; meanwhile, the raw material adopted by the method is natural nano-cellulose which is safe, non-toxic and harmless and can be naturally degraded.
For further understanding of the present invention, the following examples are given to illustrate the preparation method of the bacterial cellulose material with oriented helical structure provided by the present invention, and the scope of the present invention is not limited by the following examples.
Example 1
A) Carrying out wet stretching on a bacterial cellulose hydrogel film with the thickness of 5mm, the length of 10cm and the width of 6cm along the length direction, wherein the stretching degree is 30 percent of the original length of the bacterial cellulose, namely stretching to 13 cm;
B) and B), stacking the wet stretched bacterial cellulose hydrogel obtained in the step A) layer by layer, wherein the angle between adjacent layers is 30 degrees, the number of stacked layers is 200, the temperature is 80 ℃, and the pressure is 100MPa, and compressing the stacked layers by using a flat metal plate mold to obtain the bacterial cellulose block material with the oriented spiral structure.
Fig. 1 is a photograph of the oriented helical structured bacterial cellulose bulk prepared in this example, and fig. 2 and 3 are micrographs of the oriented helical structured bacterial cellulose bulk prepared in this example on different scales, and it can be found through calculation that the density of the oriented helical structured bacterial cellulose bulk prepared in this example is 1.33g · cm-3The coefficient of thermal expansion was about 4 ppm/K.
The mechanical properties of the bacterial cellulose block with the oriented helical structure prepared in this embodiment are tested, as shown in fig. 4, fig. 4 is a bending stress curve diagram of the bacterial cellulose block with the oriented helical structure prepared in this embodiment under different strains, and it can be known from the diagram that the bending strength of the bacterial cellulose block with the oriented helical structure prepared in this embodiment can reach 162MPa, and the bending modulus can reach 9 GPa. FIG. 6 is a graph showing the drop weight impact of the oriented helical structured bacterial cellulose material prepared in the present example; as can be seen from FIG. 6, the maximum impact force which can be borne is 2.2kN, and the impact toughness can reach 70kJ/m2The impact energy absorption of the drop hammer can reach 3 kJ.
Example 2
A) The bacterial cellulose/nano-clay sheet hydrogel film with the thickness of 0.5cm, the length of 6cm and the width of 4cm and the content of 45 percent of the nano-clay sheet is stretched in a wet state along the length direction, and the stretching degree is 25 percent of the original length of the bacterial cellulose, namely the stretching degree is 7.5 cm;
B) stacking the wet stretched bacterial cellulose hydrogel obtained in the step A) layer by layer, wherein the angle between adjacent layers is 10 degrees, the number of stacked layers is 90 layers, the temperature is 100 ℃, and the pressure is 150MPa, and compressing the stacked layers by using a flat metal plate mold to obtain the bacterial cellulose block material with the oriented spiral structure.
Fig. 7 is a photograph of a block of bacterial cellulose having an oriented helical structure prepared in this example.
The mechanical properties of the bacterial cellulose bulk material with the oriented helical structure prepared in this embodiment were tested, as shown in fig. 8, fig. 8 is the bacterial cellulose bulk material with the oriented helical structure prepared in this embodimentAs can be seen from the bending stress-strain curve diagrams under different strains, the bending strength of the bacterial cellulose block material with the oriented helical structure prepared in the embodiment can reach 177MPa, and the bending modulus can reach 10 GPa. FIG. 9 is a drop weight impact curve diagram of the bacterial cellulose bulk material with the oriented helical structure prepared in the embodiment, and it can be seen from FIG. 9 that the maximum impact force-3 kN can be endured, and the impact toughness can reach 76kJ/m2The impact energy absorption of the drop hammer can reach 5 kJ.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method of preparing an oriented helical structured bacterial cellulosic material comprising the steps of:
stretching the hydrogel in a wet state in any one direction of a plane formed along the x direction and the y direction to obtain a primary treated hydrogel; the hydrogel is one or two of bacterial cellulose hydrogel and bacterial cellulose composite material hydrogel;
stacking the primary treatment hydrogel layer by layer in sequence, wherein the stretching direction of the adjacent primary treatment hydrogel forms a certain angle, and compressing to obtain the bacterial cellulose material with the oriented spiral structure.
2. The method of claim 1, wherein the wet state stretching is 1 to 50% of the initial length of the hydrogel.
3. The method according to claim 1 or 2, wherein the wet state stretching is performed to a degree of 10% to 30% of the initial length of the hydrogel.
4. The method of claim 1, wherein the angle between adjacent primary treated hydrogels is between 0 ° and 180 °.
5. The method of claim 1, wherein the angle between adjacent primary treated hydrogels is from 10 ° to 80 °.
6. The method of claim 1, wherein the number of layers in the stack is 20 to 3000.
7. The method according to claim 1, wherein the compression temperature is 10 to 200 ℃ and the compression time is 1 to 800 MPa.
8. The preparation method according to claim 1, wherein the bacterial cellulose composite hydrogel is a hydrogel formed by one or more of a polymer and a nanomaterial and bacterial cellulose.
9. The bacterial cellulose material with the oriented spiral structure comprises a plurality of hydrogel layers which are overlapped, wherein the hydrogel layers are obtained by stretching and compressing one or two of bacterial cellulose hydrogel and bacterial cellulose composite hydrogel, the stretching direction is any direction of a plane formed by the x direction and the y direction of the hydrogel, and the stretching directions of the adjacent hydrogel layers form a certain angle.
10. The bacterial cellulose material of claim 9, wherein the number of layers of hydrogel layers is 20 to 3000.
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Citations (5)
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|---|---|---|---|---|
| CN101570616A (en) * | 2009-06-08 | 2009-11-04 | 天津科技大学 | Bacteria cellulose/ polyvinyl alcohol plural gel material and preparation method thereof |
| CN105237925A (en) * | 2015-11-05 | 2016-01-13 | 南京理工大学 | Nanometer bacterial cellulose\polyvinyl alcohol\polyethylene glycol porous composite hydrogel |
| CN105926050A (en) * | 2016-05-23 | 2016-09-07 | 东华大学 | Macroscopic fibers based on directional arrangement of bacterial cellulose nanofibers and preparation method of macroscopic fibers |
| CN108744017A (en) * | 2018-06-25 | 2018-11-06 | 中国科学技术大学 | A kind of operation suture thread |
| CN108754658A (en) * | 2018-06-25 | 2018-11-06 | 中国科学技术大学 | A kind of preparation method of bacteria cellulose composite material yarn |
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|---|---|---|---|---|
| CN101570616A (en) * | 2009-06-08 | 2009-11-04 | 天津科技大学 | Bacteria cellulose/ polyvinyl alcohol plural gel material and preparation method thereof |
| CN105237925A (en) * | 2015-11-05 | 2016-01-13 | 南京理工大学 | Nanometer bacterial cellulose\polyvinyl alcohol\polyethylene glycol porous composite hydrogel |
| CN105926050A (en) * | 2016-05-23 | 2016-09-07 | 东华大学 | Macroscopic fibers based on directional arrangement of bacterial cellulose nanofibers and preparation method of macroscopic fibers |
| CN108744017A (en) * | 2018-06-25 | 2018-11-06 | 中国科学技术大学 | A kind of operation suture thread |
| CN108754658A (en) * | 2018-06-25 | 2018-11-06 | 中国科学技术大学 | A kind of preparation method of bacteria cellulose composite material yarn |
Non-Patent Citations (1)
| Title |
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| ZHI JIAN WANG等: ""Programmed planar-to-helical shape transformations of composite hydrogels with bioinspired layered fibrous structures "", 《JOURNAL OF MATERIALS CHEMISTRY B》 * |
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