CN104558677B - A kind of preparation method of nano-cellulose/chitosan composite foam - Google Patents
A kind of preparation method of nano-cellulose/chitosan composite foam Download PDFInfo
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Abstract
一种纳米纤维素/壳聚糖复合泡沫的制备方法，本发明涉及纤维素复合材料领域，它为了解决传统泡沫、气凝胶等材料生物相容性差以及壳聚糖复合材料热稳定性低的问题。复合泡沫的制备方法：一、对含有纤维素的生物质原料进行化学处理和机械解纤处理，制备纳米纤维素水悬浊液；二、向冰醋酸溶液加入壳聚糖配制壳聚糖混合溶液；三、将纳米纤维素水悬浊液与壳聚糖混合溶液混合，得到纳米纤维素/壳聚糖复合溶液；四、对复合溶液进行低温冷冻处理；五、对冻结的混合溶液进行干燥处理，得到纳米纤维素/壳聚糖复合泡沫。本发明所用原料均为天然高分子材料，生物相容性好，热体积收缩率低，热稳定性良好。
A preparation method of nanocellulose/chitosan composite foam, the invention relates to the field of cellulose composite materials, it aims to solve the problem of poor biocompatibility of materials such as traditional foams and aerogels and low thermal stability of chitosan composite materials question. The preparation method of the composite foam: 1. Carry out chemical treatment and mechanical defibrillation treatment on the biomass raw material containing cellulose to prepare the nano-cellulose aqueous suspension; 2. Add chitosan to the glacial acetic acid solution to prepare a chitosan mixed solution 3. Mix the nanocellulose aqueous suspension with the chitosan mixed solution to obtain a nanocellulose/chitosan composite solution; 4. Carry out low-temperature freezing treatment to the composite solution; 5. Dry the frozen mixed solution , to obtain nanocellulose/chitosan composite foam. The raw materials used in the invention are all natural polymer materials, have good biocompatibility, low thermal volume shrinkage rate and good thermal stability.
Description
Technical field
The present invention relates to cellulose composite material field, and in particular to a kind of nano-cellulose/chitosan composite foam
Preparation method.
Background technology
At present, conventional foamed material mainly has benzene plate (EPS), polyurethane foam, pearl cotton etc., and foamed material is due to tool
There is light, insulation, absorb sound, be shockproof, so as to be widely used in insulation material, acoustic material, packaging material, car and boat housing
Deng field.Although these foamed materials have many advantages, such as, because non-renewable raw material, poor biocompatibility and not be present in it
The problems such as degradable so that existing foamed material it is more or less manufacture with application process or it is discarded after to natural environment
Affect, and then application of the material in some fields is restricted.Cellulose and chitosan are the world respectively
Upper first and second big natural reproducible resource, has the advantages that environment-friendly, nontoxic, degradable, and its product can be extensive
Applied to fields such as medicine, packaging for foodstuff, biological supports.Nano-cellulose is that the one kind isolated from cellulose resource has
Wire, needle-like or the club-shaped material of nanoscale, there is high Young's modulus, high intensity, high-specific surface area and low-thermal-expansion system
The advantages that number, can be carried out with some polymer it is compound be prepared into foam or aerogel material, and applied to packing heat-insulated, mistake
The fields such as filter.Chitosan has positively charged amino group as a kind of environmental type polymer, can be with nano-cellulose
Generation electrostatic adsorption forms Hydrogenbond.
The content of the invention
The Biocompatibilities such as conventional foam, aeroge are poor, quality is more crisp the invention aims to solving and
The problem of Chitosan Composites heat endurance is low, and a kind of preparation method of nano-cellulose/chitosan composite foam is provided.
The preparation method of nano-cellulose of the present invention/chitosan composite foam is realized according to the following steps：
First, the biomass material containing cellulose is chemically treated, purifying cellulose is obtained, then to cleaning cellulose
Element carries out the fine processing of machinery solution, prepares nano-cellulose aqueous suspension；
2nd, glacial acetic acid and distilled water are mixed, obtains glacial acetic acid solution, then add chitosan, magnetic agitation is uniform, obtains
To chitosan mixed solution；
3rd, the nano-cellulose aqueous suspension that step 1 obtains is mixed with the chitosan mixed solution that step 2 obtains,
Nano-cellulose/chitosan composite solution is obtained after stirring；
4th, cryogenic freezing processing is carried out at -20 DEG C to nano-cellulose/chitosan composite solution, that is freezed is mixed
Close solution；
5th, processing is dried to the mixed solution freezed, obtains nano-cellulose/chitosan composite foam；
The concentration of glacial acetic acid solution wherein described in step 2 is 0.1wt%~4.0wt%, shell in chitosan mixed solution
The concentration of glycan is 0.1wt%~5.0wt%.
The present invention prepares nano-cellulose/chitosan composite foam using the methods of freeze-drying, and the nano-cellulose/
Chitosan composite foam is a kind of composite with sheet and tridimensional network, has biocompatibility and larger
Porosity, it can be used in Medical rack, sound-absorbing material, while this nano-cellulose/chitosan composite foam is also with less
Thermal conductivity and thermal coefficient of expansion, it can be used as heat preserving and insulating material and packaging material for food.
To sum up, nano-cellulose/chitosan composite foam that the present invention is prepared includes advantages below：
1st, it is pure natural boiomacromolecule that the present invention, which prepares cellulose used in composite foam and chitosan, without thin
Cellular toxicity and possesses biocompatibility；
2nd, nano-cellulose/chitosan composite foam has low-density (0.006~0.014g/cm-3), high-specific surface area etc.
Feature；
3rd, the thermal conductivity of nano-cellulose of the present invention/chitosan composite foam is 0.03~0.032w/ (mk), heat
Cubical contraction is low, and cubical contraction is 3%~10%, can be as a kind of new heat-insulating heat-preserving material；
4th, the obtained nano-cellulose/chitosan composite foam of the present invention be a kind of no cytotoxicity, cell growth without
The green compounds of negative interaction, packaging material for food and Biodegradable scaffold can be used as；
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph for nano-cellulose/chitosan composite foam that embodiment one obtains；
Fig. 2 be different quality than nano-cellulose/chitosan composite foam thermal conductivity block diagram.
Embodiment
Embodiment one：The preparation method of present embodiment nano-cellulose/chitosan composite foam presses following step
It is rapid to implement：
First, the biomass material containing cellulose is chemically treated, purifying cellulose is obtained, then to cleaning cellulose
Element carries out the fine processing of machinery solution, prepares nano-cellulose aqueous suspension；
2nd, glacial acetic acid and distilled water are mixed, obtains glacial acetic acid solution, then add chitosan, magnetic agitation is uniform, obtains
To chitosan mixed solution；
3rd, the nano-cellulose aqueous suspension that step 1 obtains is mixed with the chitosan mixed solution that step 2 obtains,
Nano-cellulose/chitosan composite solution is obtained after stirring；
4th, cryogenic freezing processing is carried out at -20 DEG C to nano-cellulose/chitosan composite solution, that is freezed is mixed
Close solution；
5th, processing is dried to the mixed solution freezed, obtains nano-cellulose/chitosan composite foam；
The concentration of glacial acetic acid solution wherein described in step 2 is 0.1wt%~4.0wt%, shell in chitosan mixed solution
The concentration of glycan is 0.1wt%~5.0wt%.
The nano-cellulose that present embodiment obtains after drying process/chitosan composite foam has three-dimensional netted knot
Structure, unique fine structure can further improve mechanics, the thermal property of nano-cellulose/chitosan composite foam.Simultaneously
The features such as due to possessed green non-poisonous, lightweight, heat-insulated, sound absorption, good biocompatibility, in biological support, insulation material
The fields such as material, sound-absorbing material, degradable package material are applied.
Embodiment two：Present embodiment contains fiber from described in step 1 unlike embodiment one
The biomass material of element is timber, bamboo wood, cotton, fiber crops, bacteria cellulose or ascidian cellulose.Other steps and parameter with it is specific
Embodiment one is identical.
Embodiment three：Present embodiment step 1 unlike embodiment one or two is chemically treated
Successively using sodium chlorite solution's processing and alkaline solution treatment.Other steps and parameter are identical with embodiment one or two.
Embodiment four：Described in step 1 unlike one of present embodiment and embodiment one to three
The mechanical fine processing of solution is supersound process, high-speed stirred processing, speed lapping processing or high pressure homogenization processing.Other steps and parameter
It is identical with one of embodiment one to three.
Embodiment five：Present embodiment supersound process described unlike embodiment four be with
400~2000W 30~40min of Power Processing.Other steps and parameter are identical with embodiment four.
Embodiment six：Step 3 Nanowire unlike one of present embodiment and embodiment one to five
It is 0.1%~10.0% to tie up the total mass concentration of nano-cellulose and chitosan in element/chitosan mixed solution.Other steps and
Parameter is identical with one of embodiment one to five.
Embodiment seven：Present embodiment and step 3 nano-cellulose/shell unlike embodiment six
The total mass concentration of nano-cellulose and chitosan is 4%~8% in glycan mixed solution.Other steps and parameter and specific reality
It is identical to apply mode six.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven described in step 5
Drying process be freeze-drying, supercritical drying or critical point drying.Other steps and parameter and embodiment one to
One of seven is identical.
Embodiment nine：Step 1 Nanowire unlike one of present embodiment and embodiment one to eight
The weight/mass percentage composition for tieing up cellulose in plain aqueous suspension is 0.1%~5%.Other steps and parameter and embodiment one
It is identical to one of eight.
Embodiment one：The preparation method of the present embodiment nano-cellulose/chitosan composite foam is implemented according to the following steps：
First, 15g China fir wood powders are chemically treated by sodium chlorite solution and potassium hydroxide solution, obtain pure chemical fiber
Dimension element, purifying cellulose is configured to after the aqueous solution to carry out supersound process 30min with 1200W power, preparing mass concentration is
1.0wt% nano-cellulose aqueous suspension；
2nd, glacial acetic acid and distilled water are mixed, obtain the glacial acetic acid solution that concentration is 1.0wt%, then add chitosan,
Magnetic agitation is uniform, obtains chitosan mixed solution；
3rd, the nano-cellulose aqueous suspension that step 1 obtains is mixed with the chitosan mixed solution that step 2 obtains,
Nano-cellulose/chitosan composite solution that mass concentration is 1.0wt% is obtained after stirring；
4th, cryogenic freezing processing is carried out at -20 DEG C to nano-cellulose/chitosan composite solution, that is freezed is mixed
Close solution；
5th, freeze-drying process is carried out to the mixed solution freezed, condenser temperature is -40 DEG C, vacuum 1pa, is dried
Time is 50h, obtains nano-cellulose/chitosan composite foam.
The present embodiment step 1 is as follows to the chemical treating process of China fir wood powder：
A, 15g China fir wood powder is added in 1500g distilled water, 15g sodium chlorites and 2mL glacial acetic acid is added, with guarantor
Fresh membrane cover upper container, 1h is heated in 75 DEG C of waters bath with thermostatic control, then proceedes to add 15g sodium chlorites and 2ml glacial acetic acid, repeats to add
Enter sodium chlorite and glacial acetic acid 5 times, cleaning sample；B, 800g, 5wt% potassium hydroxide are added in the sample after being cleaned to step a
Solution, 10h is stood at room temperature, sample 2h is then heated at 90 DEG C；C, clean and drain the material after step b processing, use
Weighting method after dried surveys the mass concentration of purifying cellulose.
The concentration of chitosan is 1.0wt% in the chitosan mixed solution of this implementation steps two, step 3 nano-cellulose/shell
The solid masses of nano-cellulose and chitosan ratio is 10 in glycan composite solution:90.
The density of the nano-cellulose that the present embodiment obtains/chitosan composite foam is 0.0135g/cm-3, thermal conductivity is
0.032w/ (mk), hot cubical contraction are 10%, and biocompatibility test cell culture photo shows that cell growth is good, receives
Rice Cellulose/Chitosan composite foam no cytotoxicity.
Embodiment two：The present embodiment is carried out from step 1 purifying cellulose unlike embodiment one with 1200W power
High pressure homogenization processing is carried out again after being ultrasonically treated 30min, and first class pressure is 80bar and secondary pressure is 400bar, processing
30min。
Embodiment three：The solid matter of the present embodiment and nano-cellulose in step 3 unlike embodiment one and chitosan
Amount is than being 45:55.
The density of the nano-cellulose that the present embodiment obtains/chitosan composite foam is 0.0130g/cm-3, thermal conductivity is
0.031w/ (mk), hot cubical contraction are 8.2%, and biocompatibility test cell culture photo shows that cell growth is good, receives
Rice Cellulose/Chitosan composite foam no cytotoxicity.
Example IV：The solid matter of the present embodiment and nano-cellulose in step 3 unlike embodiment one and chitosan
Amount is than being 30:70.
The density of the nano-cellulose that the present embodiment obtains/chitosan composite foam is 0.0128g/cm-3, thermal conductivity is
0.030w/ (mk), hot cubical contraction are 3.7%, and biocompatibility test cell culture photo shows that cell growth is good, receives
Rice Cellulose/Chitosan composite foam no cytotoxicity.
Embodiment five：The present embodiment carries out supercritical drying from step 5 unlike embodiment one to the mixed solution freezed
Dry processing, the mixed solution freezed is placed in autoclave, CO is passed through at 40 DEG C2, reach 12MPa to pressure, and 1h is kept,
Afterwards under conditions of keeping temperature and pressure, with low discharge Sc CO2Sample 4h is persistently purged, it is remaining in gel to remove
Solvent, pressure is finally released slowly to normal pressure, obtains nano-cellulose/chitosan composite foam.
Embodiment six：The preparation method of the present embodiment nano-cellulose/chitosan composite foam is implemented according to the following steps：
First, China fir wood powder is chemically treated by sodium chlorite solution and potassium hydroxide solution, obtains cleaning cellulose
Element, it is configured to carry out supersound process 30min to purifying cellulose with 1200W power after the aqueous solution, preparing mass concentration is
0.5wt% nano-cellulose aqueous suspension；
2nd, glacial acetic acid and distilled water are mixed, obtain the glacial acetic acid solution that concentration is 0.5wt%, then add chitosan,
Magnetic agitation is uniform, obtains the chitosan mixed solution that chitosan concentration is 0.5wt%；
3rd, the nano-cellulose aqueous suspension that step 1 obtains is mixed with the chitosan mixed solution that step 2 obtains,
Nano-cellulose/chitosan composite solution that mass concentration is 0.5wt% is obtained after stirring；
4th, cryogenic freezing processing is carried out at -20 DEG C to nano-cellulose/chitosan composite solution, that is freezed is mixed
Close solution；
5th, freeze-drying process is carried out to the mixed solution freezed, condenser temperature is -40 DEG C, vacuum 1pa, is dried
Time is 50h, obtains nano-cellulose/chitosan composite foam.
The solid masses of nano-cellulose and chitosan ratio is 10 in the present embodiment step 3:90.
The density of the nano-cellulose that the present embodiment obtains/chitosan composite foam is 0.0078g/cm-3, hot volume contraction
Rate is 6.5%, and biocompatibility test cell culture photo shows that cell growth is good, nano-cellulose/chitosan compound vacuole
Foam no cytotoxicity.
Claims (9)
1. the preparation method of a kind of nano-cellulose/chitosan composite foam, it is characterised in that be to follow these steps to realize：
First, the biomass material containing cellulose is chemically treated, obtains purifying cellulose, then purifying cellulose is entered
The fine processing of row machinery solution, prepares nano-cellulose aqueous suspension；
2nd, glacial acetic acid and distilled water are mixed, obtains glacial acetic acid solution, then add chitosan, magnetic agitation is uniform, obtains shell
Glycan mixed solution；
3rd, the nano-cellulose aqueous suspension that step 1 obtains is mixed with the chitosan mixed solution that step 2 obtains, stirred
Nano-cellulose/chitosan composite solution is obtained after uniformly；
4th, cryogenic freezing processing is carried out at -20 DEG C to nano-cellulose/chitosan composite solution, the mixing freezed is molten
Liquid；
5th, processing is dried to the mixed solution freezed, obtains nano-cellulose/chitosan composite foam；
The concentration of glacial acetic acid solution wherein described in step 2 is 0.1wt%~4.0wt%, chitosan in chitosan mixed solution
Concentration be 0.1wt%~5.0wt%.
A kind of 2. preparation method of nano-cellulose/chitosan composite foam according to claim 1, it is characterised in that step
The biomass material containing cellulose described in rapid one is timber, bamboo wood, cotton, fiber crops, bacteria cellulose or ascidian cellulose.
A kind of 3. preparation method of nano-cellulose/chitosan composite foam according to claim 1, it is characterised in that step
A rapid chemical treatment is successively using sodium chlorite solution's processing and alkaline solution treatment.
A kind of 4. preparation method of nano-cellulose/chitosan composite foam according to claim 1, it is characterised in that step
The fine processing of mechanical solution described in rapid one is supersound process, high-speed stirred processing, speed lapping processing or high pressure homogenization processing.
A kind of 5. preparation method of nano-cellulose/chitosan composite foam according to claim 4, it is characterised in that institute
The supersound process stated is 30~40min of Power Processing with 400~2000W.
A kind of 6. preparation method of nano-cellulose/chitosan composite foam according to claim 1, it is characterised in that step
The total mass concentration of nano-cellulose and chitosan is 0.1%~10.0% in rapid three nano-celluloses/chitosan mixed solution.
A kind of 7. preparation method of nano-cellulose/chitosan composite foam according to claim 6, it is characterised in that step
The total mass concentration of nano-cellulose and chitosan is 4%~8% in rapid three nano-celluloses/chitosan mixed solution.
A kind of 8. preparation method of nano-cellulose/chitosan composite foam according to claim 1, it is characterised in that step
Drying process described in rapid five is freeze-drying, supercritical drying or critical point drying.
A kind of 9. preparation method of nano-cellulose/chitosan composite foam according to claim 1, it is characterised in that step
The weight/mass percentage composition of cellulose is 0.1%~5% in rapid nano-cellulose aqueous suspension.
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| WO2020237205A1 (en) | 2019-05-22 | 2020-11-26 | Cruz Foam, Inc. | Biodegradable foam with laminate layers |
| CN110591141B (en) * | 2019-09-02 | 2022-06-14 | 广西大学 | Holocellulose composite aerogel and preparation method thereof |
| CN111171384A (en) * | 2020-02-10 | 2020-05-19 | 东华大学 | Lightweight thermal insulation flexible chitosan/nanocellulose aerogel and preparation method thereof |
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| CN114377188B (en) * | 2022-01-14 | 2023-01-10 | 宋金华 | Super-absorbent bio-based foam material and preparation method and application thereof |
| CN116510062B (en) * | 2023-04-25 | 2025-08-22 | 山东大学 | A rapid hemostatic sponge reinforced with sea squirt nanocellulose and having photothermal antibacterial effect and its preparation method |
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