CN103172886A - Method for quickly preparing colorful nanocrystalline cellulose film - Google Patents
Method for quickly preparing colorful nanocrystalline cellulose film Download PDFInfo
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- CN103172886A CN103172886A CN2013100803890A CN201310080389A CN103172886A CN 103172886 A CN103172886 A CN 103172886A CN 2013100803890 A CN2013100803890 A CN 2013100803890A CN 201310080389 A CN201310080389 A CN 201310080389A CN 103172886 A CN103172886 A CN 103172886A
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Abstract
The invention relates to a novel method for quickly preparing a colorful nanocrystalline cellulose film and belongs to the functional high-additional value utilization field of cellulose resources. The vacuum degree is changed to realize accelerating volatilizing process of moisture in cellulose nanocrystalline suspension liquid, so that a purpose of quickly preparing the colorful nanocrystalline cellulose film is realized. According to the method for quickly preparing the colorful nanocrystalline cellulose film disclosed by the invention, the cellulose materials are easily available and the nanocrystalline cellulose suspension liquid is simple to prepare; the prepared nanocrystalline cellulose film has the reflected light selecting characteristic of the cholesteric liquid crystal; moreover, the cellulose has good biocompatibility; and the cellulose film material can further be applied to the biomedical field.
Description
Technical field
The invention belongs to the functionalization high value added utilization field of cellulose resource, relate to a kind of fast preparation method of the color nano crystal fiber element film based on the filter paper fibre element.
Background technology
Mierocrystalline cellulose is a kind of renewable organic polymer that extensively is present in occurring in nature, and plant cell wall, marine alga, tunicate, cotton, bacterium etc. are all cellulosic abundant sources.Nanocrystalline Mierocrystalline cellulose is the product that is obtained through hydrolysis by Mierocrystalline cellulose, and this material receives much concern because of the enhancement in high polymer composite material and unique self-assembly optical property in the past twenty years.Mierocrystalline cellulose is through forming the rod-like nano crystal fiber element of surface band electric charge (sulfate group) after sulphuric acid hydrolysis, the anisotropy pattern that it is special and surface band electrically can form the lyotropic cholesteric liquid crystal in water.
By moisture evaporation, the hand of rod-like nano crystal fiber element in water levied in the translucent cellulose solids film that nematic phase self-assembly ordered structure can well be kept at final formation.This translucent fibre element solid film with ordered arrangement structure is understood the visible light of the certain wavelength of selective reflection usually, thereby demonstrates distinct colors.
In the document of having reported, the color of cellulose membrane mainly is subject to three large factor impacts.The one, cellulosic material and nanocrystalline preparation condition; The 2nd, add electrolyte concentration; The 3rd, intensity of sonification.And the moisture evaporation process is generally to carry out under field conditions (factors), and volatilization process is very slow.
Summary of the invention
The present invention adopts the method that changes vacuum tightness, realizes accelerating the moisture evaporation process, reaches the purpose of the colorful nanocrystalline cellulosefilm of quick preparation.In order to achieve the above object, preparation method of the present invention is:
1) preparation of rod-like nano crystal fiber element suspension
Adopt filter paper as cellulosic material, obtain nanocrystalline rod-like fibre element suspension by certain density sulphuric acid hydrolysis.
Step:
Take a certain amount of filter paper fibre element, add a certain amount of sulphuric acid soln, heat up, water bath with thermostatic control magnetic agitation certain hour, thin up stops hydrolysis reaction, the centrifugal part acid solution of going out, distilled water wash, centrifugal several repeatedly, cellulose suspension is transferred in dialysis tubing and dialyses, and to remove remaining acid solution, measures pH value and the concentration of final cellulose suspension.
2) preparation of nanocrystalline cellulosefilm
Get above-mentioned cellulose suspension after sonic oscillation under certain power, be put in drying and forming-film in vacuum drying oven.And under different vacuum tightnesss, the maximum reflection optical wavelength of film formation time and film.
The invention has the advantages that:
1) cellulosic material in the present invention is easy to get.
2) in the present invention, nanocrystalline cellulose suspension preparation is simple.
3) the nanocrystalline cellulosefilm in the present invention has the catoptrical characteristic of selection of cholesteric liquid crystal.
4) the nanocrystalline cellulosefilm in the present invention can be used for biomedical sector.
Description of drawings
The maximum reflection optical wavelength of cellulosefilm under the different vacuum tightnesss of Fig. 1
Illustrate: use uv-vis spectra (UV-2450, Shimadzu Corporation Analysis ﹠amp; Measuring Instrument Division, Tokyo, Japan) to measure, 90 ° of input angles, test wavelength scope are 200-800nm.
Film formation time under the different vacuum tightnesss of Fig. 2
Embodiment
Example 1: rod-like nano crystal fiber element suspension can obtain according to following method:
The 1g filter paper fibre is plain, adds 64% sulphuric acid soln 8.75ml, magnetic agitation 2.5h in 60 ℃ of waters bath with thermostatic control.Add 10 times of deionized waters to dilute to stop hydrolysis reaction.4000 leave heart 10min, remove supernatant liquor.The cleaning of remaining suspension liquid water and centrifugal several are until pH ≈ 2.Dialysed in deionized water 2-3 days with rear suspension liquid until suspension becomes transparent and pH ≈ 5.At last, with the fine micro-pore-film filtration suspension of the vinegar of 0.45 μ m, remove macrobead.The final concentration of solution is about 1% left and right.
Example 2: rod-like nano crystal fiber element film can prepare according to following method:
1. get the rod-like nano crystal fiber element suspension 2.5g of aforesaid method preparation, 300W sonic oscillation 30min is transferred in the plastics casing of polystyrene 2cm * 2cm, is put in subsequently and carries out drying in vacuum drying oven, and vacuum tightness is adjusted to 0MPa.
2. get the rod-like nano crystal fiber element suspension 2.5g of aforesaid method preparation, 300W sonic oscillation 30min is transferred in the plastics casing of polystyrene 2cm * 2cm, is put in subsequently and carries out drying in vacuum drying oven, and vacuum tightness is adjusted to-0.01MPa.
3. get the rod-like nano crystal fiber element suspension 2.5g of aforesaid method preparation, 300W sonic oscillation 30min is transferred in the plastics casing of polystyrene 2cm * 2cm, is put in subsequently and carries out drying in vacuum drying oven, and vacuum tightness is adjusted to-0.03MPa.
4. get the rod-like nano crystal fiber element suspension 2.5g of aforesaid method preparation, 300W sonic oscillation 30min is transferred in the plastics casing of polystyrene 2cm * 2cm, is put in subsequently and carries out drying in vacuum drying oven, and vacuum tightness is adjusted to-0.05MPa.
5. get the rod-like nano crystal fiber element suspension 2.5g of aforesaid method preparation, 300W sonic oscillation 30min is transferred in the plastics casing of polystyrene 2cm * 2cm, is put in subsequently and carries out drying in vacuum drying oven, and vacuum tightness is adjusted to-0.07MPa.
6. get the rod-like nano crystal fiber element suspension 2.5g of aforesaid method preparation, 300W sonic oscillation 30min is transferred in the plastics casing of polystyrene 2cm * 2cm, is put in subsequently and carries out drying in vacuum drying oven, and vacuum tightness is adjusted to-0.095MPa.
Claims (5)
1. quick method of the colorful nanocrystalline cellulosefilm of preparation, it is characterized in that: colorful nanocrystalline cellulosefilm can obtain according to the following step:
1. take a certain amount of filter paper fibre element, add a certain amount of sulphuric acid soln, heat up, water bath with thermostatic control magnetic agitation certain hour, thin up stops hydrolysis reaction, the centrifugal part acid solution of going out, distilled water wash, centrifugal several repeatedly, cellulose suspension is transferred in dialysis tubing and dialyses, and to remove remaining acid solution, measures pH value and the concentration of final cellulose suspension.
2. get above-mentioned cellulose suspension after sonic oscillation under certain power, be put in vacuum drying oven drying and forming-film under different vacuum tightnesss.
2. colorful nanocrystalline cellulosefilm according to claim 1, it is characterized in that: the mass percentage concentration of sulphuric acid soln used is 64%.
3. colorful nanocrystalline cellulosefilm according to claim 1 is characterized in that: the pH value of final cellulose suspension is 5, and concentration is 1% left and right.
4. colorful nanocrystalline cellulosefilm according to claim 1, it is characterized in that: the supersound process condition is 300W sonic oscillation 30min.
5. colorful nanocrystalline cellulosefilm according to claim 1, it is characterized in that: cellulose suspension is put in and carries out drying and forming-film in vacuum drying oven, and the vacuum tightness regulation range is-0.01～-0.095MPa.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131129A (en) * | 2015-10-12 | 2015-12-09 | 长春工业大学 | Preparation method for nanocellulose |
| CN105199123A (en) * | 2015-11-13 | 2015-12-30 | 南京林业大学 | Preparation method of cellulose nanocrystal iridescent anti-counterfeiting mark |
| CN105670044A (en) * | 2016-01-19 | 2016-06-15 | 青岛科技大学 | High-strength high-toughness cellulose nano-crystalline color film and preparation method thereof |
| CN106084135A (en) * | 2016-06-01 | 2016-11-09 | 上海交通大学 | Humidity based on Cellulose nanocrystal response photon crystal material and preparation method thereof |
| CN106800605A (en) * | 2017-01-20 | 2017-06-06 | 华南理工大学 | A kind of preparation method of nano-cellulose |
| CN107345143A (en) * | 2017-05-15 | 2017-11-14 | 华南理工大学 | A kind of bacteria cellulose liquid crystalline phase iridescent film and preparation method and application |
| CN111205499A (en) * | 2020-03-11 | 2020-05-29 | 刘珂贝 | Nano microcrystalline cellulose piezoelectric material and preparation method thereof |
| CN112280072A (en) * | 2020-10-29 | 2021-01-29 | 华南理工大学 | Wavelength-controllable cellulose iridescent film and preparation method thereof |
| CN112321859A (en) * | 2020-10-29 | 2021-02-05 | 华南理工大学 | Full-color display film based on structural color and preparation method thereof |
| CN113480756A (en) * | 2021-06-11 | 2021-10-08 | 北京航空航天大学 | Preparation method and application of cellulose nanocrystalline spiral self-assembly body and glycerol composite film |
Citations (1)
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| CN102440979A (en) * | 2010-09-30 | 2012-05-09 | 迪特克(济源)绿色生物科技有限公司 | Cellulose derivative composite film and preparation method thereof |
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Patent Citations (1)
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| CN102440979A (en) * | 2010-09-30 | 2012-05-09 | 迪特克(济源)绿色生物科技有限公司 | Cellulose derivative composite film and preparation method thereof |
Non-Patent Citations (1)
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| 薛岚: "纳米晶纤维素胆甾相液晶、膜的制备及氧化性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, no. 11, 15 November 2012 (2012-11-15), pages 014 - 93 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131129B (en) * | 2015-10-12 | 2017-12-15 | 长春工业大学 | A kind of preparation method of nano-cellulose |
| CN105131129A (en) * | 2015-10-12 | 2015-12-09 | 长春工业大学 | Preparation method for nanocellulose |
| CN105199123A (en) * | 2015-11-13 | 2015-12-30 | 南京林业大学 | Preparation method of cellulose nanocrystal iridescent anti-counterfeiting mark |
| CN105670044A (en) * | 2016-01-19 | 2016-06-15 | 青岛科技大学 | High-strength high-toughness cellulose nano-crystalline color film and preparation method thereof |
| CN106084135A (en) * | 2016-06-01 | 2016-11-09 | 上海交通大学 | Humidity based on Cellulose nanocrystal response photon crystal material and preparation method thereof |
| CN106800605A (en) * | 2017-01-20 | 2017-06-06 | 华南理工大学 | A kind of preparation method of nano-cellulose |
| CN107345143A (en) * | 2017-05-15 | 2017-11-14 | 华南理工大学 | A kind of bacteria cellulose liquid crystalline phase iridescent film and preparation method and application |
| CN111205499A (en) * | 2020-03-11 | 2020-05-29 | 刘珂贝 | Nano microcrystalline cellulose piezoelectric material and preparation method thereof |
| CN112280072A (en) * | 2020-10-29 | 2021-01-29 | 华南理工大学 | Wavelength-controllable cellulose iridescent film and preparation method thereof |
| CN112321859A (en) * | 2020-10-29 | 2021-02-05 | 华南理工大学 | Full-color display film based on structural color and preparation method thereof |
| CN112321859B (en) * | 2020-10-29 | 2022-03-25 | 华南理工大学 | Full-color display film based on structural color and preparation method thereof |
| CN112280072B (en) * | 2020-10-29 | 2022-03-29 | 华南理工大学 | Wavelength-controllable cellulose iridescent film and preparation method thereof |
| CN113480756A (en) * | 2021-06-11 | 2021-10-08 | 北京航空航天大学 | Preparation method and application of cellulose nanocrystalline spiral self-assembly body and glycerol composite film |
| CN113480756B (en) * | 2021-06-11 | 2022-12-27 | 北京航空航天大学 | Preparation method and application of cellulose nanocrystalline spiral self-assembly body and glycerol composite film |
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Application publication date: 20130626 |