CN113150336B - Method for preparing high-crystallization high-orientation regenerated cellulose material by high-voltage electrostatic field assisted self-assembly and product - Google Patents
Method for preparing high-crystallization high-orientation regenerated cellulose material by high-voltage electrostatic field assisted self-assembly and product Download PDFInfo
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- 239000004627 regenerated cellulose Substances 0.000 title claims abstract description 54
- 239000000463 material Substances 0.000 title claims abstract description 47
- 230000005686 electrostatic field Effects 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000002425 crystallisation Methods 0.000 title claims abstract description 18
- 238000001338 self-assembly Methods 0.000 title claims abstract description 18
- 229920002678 cellulose Polymers 0.000 claims abstract description 50
- 239000001913 cellulose Substances 0.000 claims abstract description 50
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 230000005684 electric field Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229920000742 Cotton Polymers 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229920001131 Pulp (paper) Polymers 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 25
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 15
- 239000011521 glass Substances 0.000 description 13
- 239000004202 carbamide Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000003513 alkali Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
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- 230000003068 static effect Effects 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000000707 layer-by-layer assembly Methods 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 description 1
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
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- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 1
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
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Abstract
The invention discloses a method for preparing a high-crystalline high-orientation regenerated cellulose material by self-assembly assisted by a high-voltage electrostatic field and a product thereof, wherein the method comprises the following steps: (1) dissolving a cellulose raw material in a dissolving solution to obtain a cellulose solution; (2) coating the cellulose solution on a substrate, and drying the substrate in a high-voltage electrostatic field to form a film; (3) and after film formation, post-treatment is carried out to obtain the high-crystallization high-orientation regenerated cellulose material. The invention adopts a method of high-voltage electrostatic field assisted self-assembly, can accurately and controllably prepare the regenerated cellulose material with high crystallization and high orientation, and the regenerated cellulose material has obvious high orderliness on structure.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a method for preparing a high-crystallization high-orientation regenerated cellulose material by high-voltage electrostatic field assisted self-assembly and a product.
Background
Natural crystalline polysaccharides, such as cellulose, are a material having excellent properties of biocompatibility, biodegradability and non-toxicity, and have been the focus of research. However, the microstructure of the regenerated cellulose material prepared by the prior art is mostly disordered or short-range ordered, and the crystallinity and the orientation degree are low, so the application of the regenerated cellulose material is greatly limited.
The chinese patent application No. 201510255365.3 discloses a method for preparing a highly oriented polysaccharide cellulose material, which utilizes a directional temperature field freezing technique to control the growth direction of ice crystals, thereby forming a highly oriented cellulose material. However, the preparation process is relatively complex, the cost consumption is high, and the orientation degree cannot be accurately controlled.
The chinese patent application No. 201611062361.4 discloses a method for preparing a highly oriented cellulose film, which mainly uses an oriented stretching method to stretch and fix a cellulose film plasticized by an ionic liquid, and removes the plasticizer in a stretched state, thereby preparing a cellulose film with high strength and high orientation.
Although the prior art orients cellulose films to improve their properties, the search for new methods for regulating the microstructure of regenerated cellulose materials is still of great significance in the field of the preparation of new cellulose materials. Self-assembly is a controllable preparation process, and how to regulate and control the microstructure of the regenerated cellulose material through self-assembly of regenerated cellulose macromolecules needs to be deeply developed.
Disclosure of Invention
In order to prepare the regenerated cellulose material with high crystallization and high orientation, improve the comprehensive performance of the regenerated cellulose material and expand the application range of the regenerated cellulose material, the invention provides a method for preparing the regenerated cellulose material with high crystallization and high orientation by high-voltage electrostatic field assisted self-assembly.
The technical scheme of the invention is as follows:
a method for preparing a high-crystalline high-orientation regenerated cellulose material by high-voltage electrostatic field assisted self-assembly comprises the following steps:
(1) dissolving a cellulose raw material in a dissolving solution to obtain a cellulose solution;
(2) coating the cellulose solution on a substrate, and drying the substrate in a high-voltage electrostatic field to form a film;
(3) and after film formation, post-treatment is carried out to obtain the high-crystallization high-orientation regenerated cellulose material.
The polymerization degree of cellulose molecules of the cellulose raw material is 100-2000; the viscosity average molecular weight of the cellulose raw material is 1.62 multiplied by 104~3.24×105。
Further preferably, the cellulose raw material is at least one of cotton linter pulp, absorbent cotton pulp and wood pulp.
The dissolving solution is at least one of an NMMO aqueous solution, a lithium chloride (LiCl)/N, N-Dimethylformamide (DMAC) system, an alkali/urea system and an alkali/thiourea system.
Preferably, the concentration of the cellulose in the cellulose solution is 1-8 wt%; it is further preferred that the concentration of cellulose is 2-6 wt%.
The polymerization degree and concentration of the cellulose raw material directly influence the solubility of the cellulose raw material in the dissolving solution, and the cellulose raw material cannot be completely dissolved in the dissolving solution due to the excessive polymerization degree or concentration, so that a uniform and stable regenerated cellulose solution cannot be obtained.
In the step (1), the cellulose is dissolved in the dissolving solution by stirring at a stirring speed of 300-2000 rpm.
In step (2), the cellulose solution may be coated onto the substrate by dipping, knife coating, brush coating, or the like.
The substrate is a flat substrate and can be one of a glass sheet, a polyethylene terephthalate (PET) plate, a polypropylene (PP) plate and a Polytetrafluoroethylene (PTFE) plate.
Preferably, in step (2), the coating thickness of the cellulose solution is 100-.
When the coating thickness is small, the regenerated cellulose content in the solution is small, so that the crystallinity is low. When the concentration of the cellulose solution is further increased, the effective crystallinity of the cellulose solution is increased. However, when the coating thickness is too high, the regenerated cellulose content in the solution is too high, so that the movement of the regenerated cellulose is limited in the high-voltage electrostatic self-assembly process, and the orientation degree of the regenerated cellulose is influenced.
It is further preferred that the coating thickness is 100-.
Preferably, in the step (2), drying the film in a high-voltage electrostatic field for 12 to 48 hours; more preferably, the mixture is placed in a high-voltage electrostatic field to be dried into a film for 12 to 24 hours.
Preferably, the electric field intensity of the high-voltage electrostatic field is 600-2000V-cm-1。
The electric field intensity of the high-voltage electrostatic field is changed by adjusting the voltage of the high-voltage electrostatic field and the distance between the electric fields (the distance between the positive electrode plate and the negative electrode plate). When the voltage is larger and the electric field distance is smaller, the electric field intensity of the obtained high-voltage electrostatic field is stronger. When the electric field intensity is too weak, a highly crystalline, highly oriented regenerated cellulose material cannot be obtained.
Further preferably, the voltage of the high-voltage electrostatic field is 10-24 kV; the electric field distance is 10-25 cm; preferably, the voltage of the high-voltage electrostatic field is 12-20 kV; the electric field distance is 10-20 cm.
In the step (3), the post-treatment comprises the following steps: and (3) placing the film-formed cellulose material into deionized water, cleaning and drying.
The drying is natural drying or vacuum heating drying.
Preferably, the drying is vacuum heating drying; the heating temperature is 40-80 ℃; the relative vacuum degree is 0 to-60 KPa.
The invention also provides a high-crystallization high-orientation regenerated cellulose material prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts a method of high-voltage electrostatic field assisted self-assembly, can accurately and controllably prepare the regenerated cellulose material with high crystallization and high orientation, and the regenerated cellulose material has obvious high orderliness on structure, thereby greatly widening the practical application range of the regenerated cellulose material.
The preparation process is simple, can realize large-area production, does not use toxic organic reagents, is green and renewable in raw materials, and has great significance in the field of environmental protection.
Drawings
FIGS. 1 (a) and (b) are SEM electron micrographs of the regenerated cellulose material of example 3 and comparative example 1, respectively;
fig. 2 is XRD patterns of the regenerated cellulose materials of example 3 and comparative example 1.
Detailed Description
Example 1
Taking cellulose (viscosity average molecular weight M)η=9.72×104)4 g, 100 g of mixed aqueous solution of 7 wt% sodium hydroxide and 12 wt% urea (namely 7 wt% sodium hydroxide and 12 wt% urea) is added, stirred in an ice-water bath for 10 minutes, then placed in a refrigerator for freezing for 3 hours, taken out and fully stirred to obtain colorless transparent solution. After a small amount of undissolved cellulose is removed by filtration, a film is scraped on glass, the glass is placed in a high-voltage electrostatic field,at the moment, the electrostatic field voltage is 14kV, the distance between the positive electrode plate and the negative electrode plate is 15cm, and after the film is formed, the film is cleaned and dried at the temperature of 40 ℃ in vacuum, so that the regenerated cellulose material with high crystallization and high orientation is obtained.
Example 2
Taking cellulose (viscosity average molecular weight M)η=9.72×104)4 g, 100 g of 7 wt%/12 wt% aqueous alkali urea solution is added, stirred in an ice-water bath for 10 minutes, then placed in a refrigerator for freezing for 3 hours, taken out and fully stirred to obtain a colorless transparent solution. After a small amount of undissolved cellulose is removed by filtration, a film is scraped on glass, the glass is placed in a high-voltage electrostatic field, the voltage of the electrostatic field is 16kV, the distance between a positive electrode plate and a negative electrode plate is 15cm, and after the film is formed, the glass is cleaned and dried at 40 ℃ in vacuum, so that the regenerated cellulose material with high crystallization and high orientation is obtained.
Example 3
Taking cellulose (viscosity average molecular weight M)η=9.72×104)4 g, 100 g of 7 wt%/12 wt% aqueous alkali urea solution is added, stirred in an ice-water bath for 10 minutes, then placed in a refrigerator for freezing for 3 hours, taken out and fully stirred to obtain a colorless transparent solution. After a small amount of undissolved cellulose is removed by filtration, a film is scraped on glass, the glass is placed in a high-voltage electrostatic field, the voltage of the electrostatic field is 18kV, the distance between a positive electrode plate and a negative electrode plate is 15cm, and after the film is formed, the glass is cleaned and dried at 40 ℃ in vacuum, so that the regenerated cellulose material with high crystallization and high orientation is obtained.
Example 4
Taking cellulose (viscosity average molecular weight M)η=9.72×104)4 g, 100 g of 7 wt%/12 wt% aqueous alkali urea solution is added, stirred in an ice-water bath for 10 minutes, then placed in a refrigerator for freezing for 3 hours, taken out and fully stirred to obtain a colorless transparent solution. After a small amount of undissolved cellulose is removed by filtration, a film is scraped on glass, the glass is placed in a high-voltage electrostatic field, the voltage of the electrostatic field is 20kV, the distance between a positive electrode plate and a negative electrode plate is 15cm, and after the film is formed, the glass is cleaned and dried at 40 ℃ in vacuum, so that the regenerated cellulose material with high crystallization and high orientation is obtained.
Comparative example 1
Taking cellulose (viscosity average molecular weight M)η=9.72×104)4 g, 100 g of 7 wt%/12 wt% aqueous alkali urea solution is added, stirred in an ice-water bath for 10 minutes, then placed in a refrigerator for freezing for 3 hours, taken out and fully stirred to obtain a colorless transparent solution. After a small amount of undissolved cellulose was removed by filtration, the film was scraped off from the glass, and the film was naturally formed at room temperature in the same manner as in example 3, and then washed and dried at 40 ℃.
Method for calculating crystallinity and orientation degree of regenerated cellulose material:
XRD analysis was performed using X-ray diffractometer model D8 Advance, brueck, germany: cu (Kalpha) ray, voltage 40kV, current 40mA, scanning range 2 theta of 5-50 DEG, and scanning speed of 2 DEG cm-1The crystallinity calculation was performed according to the two-phase structure theory method using the following formula:
Xc=(Sc/(Sc+Sa)
in the formula: scAnd SaThe areas of diffraction of the crystalline and amorphous regions of regenerated cellulose in the sample, respectively.
The degree of orientation analysis was carried out using a two-dimensional X-ray diffractometer model D8 Discover from Bruker, Germany: the test voltage was 40kV, the current was 40mA, and the incident X-ray wavelength was 1.5418X 10-10And m is selected. According to the measured two-dimensional diffraction pattern, integrating each crystal face (shown as bright spots on the two-dimensional pattern) to obtain a one-dimensional diffraction peak pattern, performing fitting peak separation processing by a computer, and calculating the orientation degree according to the following formula:
fc=(180°-H°)/180°
in the formula: f. ofcIs the degree of orientation; h is the peak width at half height.
In FIG. 1, (a) and (b) are SEM images of the regenerated cellulose film of example 3 self-assembled by high-voltage static electricity and comparative example 1 under natural drying, respectively. It can be found from the figure that compared with the regenerated cellulose membrane which is naturally dried, the regenerated cellulose membrane which is self-assembled by high-voltage static electricity has an obvious orientation structure, the direction of the orientation structure is consistent with the direction of a high-voltage static field, and the high-voltage static electricity method is used for self-assembling the regenerated cellulose membrane in the drying process, so that the ordered structure is obtained, and the orientation degree of the ordered structure is greatly improved.
Meanwhile, the XRD patterns of the regenerated cellulose films obtained in example 3 and comparative example 1 are shown in fig. 2, and a comparative analysis can find that diffraction peaks of the regenerated cellulose appear at 12.4 °, 20.2 ° and 21.9 ° to confirm the formation of the regenerated cellulose.
The calculation of the crystallinity and the orientation degree shows that compared with the comparative example 1, the crystallinity and the orientation degree of the regenerated cellulose membrane obtained by high-voltage electrostatic self-assembly in the example 3 are greatly improved, which shows that the high-voltage electrostatic self-assembly method can effectively improve the crystallinity and the orientation degree of the material.
The above-mentioned embodiments are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions, equivalents, etc. made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (9)
1. A method for preparing a high-crystallization high-orientation regenerated cellulose material by high-voltage electrostatic field assisted self-assembly is characterized by comprising the following steps:
(1) dissolving a cellulose raw material in a dissolving solution to obtain a cellulose solution;
(2) coating the cellulose solution on a substrate, and drying the substrate in a high-voltage electrostatic field to form a film; the electric field intensity is 600-2000V ∙ cm-1;
(3) And after film formation, post-treatment is carried out to obtain the high-crystallization high-orientation regenerated cellulose material.
2. The method for preparing the high-crystallization high-orientation regenerated cellulose material by self-assembly assisted by the high-voltage electrostatic field according to claim 1, wherein the polymerization degree of cellulose molecules of the cellulose raw material is 100-2000.
3. The method for preparing the high-crystallization high-orientation regenerated cellulose material by self-assembly assisted by the high-voltage electrostatic field according to claim 2, wherein the cellulose raw material is at least one of cotton linter pulp, absorbent cotton pulp and wood pulp.
4. The method for preparing the high-crystalline high-orientation regenerated cellulose material by self-assembly assisted by the high-voltage electrostatic field according to claim 1, wherein the concentration of the cellulose in the cellulose solution is 1-8 wt%.
5. The method for preparing high-crystalline high-orientation regenerated cellulose material by self-assembly assisted by high-voltage electrostatic field as claimed in claim 1, wherein the coating thickness of the cellulose solution in step (2) is 100-2000 μm.
6. The method for preparing the high-crystalline high-orientation regenerated cellulose material by self-assembly assisted by the high-voltage electrostatic field according to claim 1, characterized in that in the step (2), the film is dried in the high-voltage electrostatic field for 12-48 h.
7. The method for preparing the high-crystalline high-orientation regenerated cellulose material by the self-assembly assisted by the high-voltage electrostatic field according to claim 1, wherein in the step (3), the post-treatment is as follows: and (3) placing the film-formed cellulose material into deionized water, cleaning and drying.
8. The method for preparing the high-crystalline high-orientation regenerated cellulose material by the self-assembly assisted by the high-voltage electrostatic field according to claim 7, wherein the drying is vacuum heating drying; the heating temperature is 40-80 ℃; the relative vacuum degree is 0 to-60 KPa.
9. A highly crystalline, highly oriented regenerated cellulose material prepared by the process of any one of claims 1 to 8.
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