CN104558677A - Preparation method of nano cellulose/chitosan composite foam - Google Patents
Preparation method of nano cellulose/chitosan composite foam Download PDFInfo
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- CN104558677A CN104558677A CN201510060910.3A CN201510060910A CN104558677A CN 104558677 A CN104558677 A CN 104558677A CN 201510060910 A CN201510060910 A CN 201510060910A CN 104558677 A CN104558677 A CN 104558677A
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Abstract
The invention discloses a preparation method of nano cellulose/chitosan composite foam, relates to the field of cellulose composite materials, and aims at solving the problems of poor biocompatibility of traditional materials such as foam and aerogel and low thermostability of a chitosan composite material. The preparation method of the composite foam comprises the following steps: 1 carrying out chemical treatment and mechanical fiber degradation treatment on a biomass material containing cellulose to prepare a nano cellulose turbid liquid; 2 adding chitosan to an acetic acid glacial solution to prepare a chitosan mixed liquid; 3 mixing the nano cellulose turbid liquid with the chitosan mixed liquid to obtain a nano cellulose/chitosan composite liquid; 4 carrying out low-temperature freezing treatment on the composite liquid; and 5 carrying out drying treatment on the frozen mixed liquid to obtain the nano cellulose/chitosan composite foam. The used raw materials are natural high polymer materials, so that the nano cellulose/chitosan composite foam is good in biocompatibility, low in thermal volume shrinkage rate and good in heat stability.
Description
Technical field
The present invention relates to cellulose composite material field, be specifically related to the preparation method of a kind of nano-cellulose/chitosan composite foam.
Background technology
At present, conventional foam materials mainly contains benzene plate (EPS), polyurethane foam, PE Foam etc., foam materials owing to having light weight, insulation, sound absorption, the advantage such as shockproof, thus is widely used in the fields such as lagging material, sound-proof material, wrapping material, car and boat housing.Although these foam materialss have plurality of advantages, but because it exists, raw material is non-renewable, the problem such as poor biocompatibility and non-degradable, make existing foam materials more or less in Manufacture and application process or discarded after physical environment is affected, and then material is restricted in the application in some field.Mierocrystalline cellulose and chitosan are the first and second large natural reproducible resources in the world respectively, and have the advantages such as environmental friendliness, nontoxic, degradable, its goods can be widely used in the fields such as medicine, food product pack, biological support.Nano-cellulose is isolated a kind of wire, needle-like or club-shaped material with nanoscale from cellulose resource, there is the advantages such as high Young's modulus, high strength, high-ratio surface sum low thermal coefficient of expansion, compound can be carried out with some polymkeric substance and be prepared into foam or aerogel material, and be applied to the fields such as packaging is heat insulation, filtration.Chitosan, as a kind of environmental type polymkeric substance, has positively charged amino group, with nano-cellulose generation electrostatic adsorption or can form hydrogen bonded.
Summary of the invention
The object of the invention is to solve the problem that the Biocompatibility such as conventional foam, aerogel is poor, quality is more crisp and Chitosan Composites thermostability is low, and the preparation method of a kind of nano-cellulose/chitosan composite foam is provided.
The preparation method of nano-cellulose of the present invention/chitosan composite foam realizes according to the following steps:
One, carry out chemical treatment to containing cellulosic biomass material, obtain purifying cellulose, then machinery is carried out to purifying cellulose and separate fine process, prepare nano-cellulose aqueous suspension;
Two, by Glacial acetic acid and distilled water mixing, obtain glacial acetic acid solution, then add chitosan, magnetic agitation is even, obtains chitosan mixing solutions;
Three, the chitosan mixing solutions that the nano-cellulose aqueous suspension and the step 2 that step one are obtained obtain mixes, and obtains nano-cellulose/chitosan composite solution after stirring;
Four, at-20 DEG C, cryogenic freezing process is carried out to nano-cellulose/chitosan composite solution, obtain the mixing solutions freezed;
Five, drying treatment is carried out to the mixing solutions freezed, obtain nano-cellulose/chitosan composite foam;
The concentration of the glacial acetic acid solution wherein described in step 2 is 0.1wt% ~ 4.0wt%, and in chitosan mixing solutions, the concentration of chitosan is 0.1wt% ~ 5.0wt%.
The present invention adopts the methods such as lyophilize to prepare nano-cellulose/chitosan composite foam, this nano-cellulose/chitosan composite foam is a kind of matrix material with sheet and tridimensional network, there is biocompatibility and larger porosity, can be used in Medical rack, sound-absorbing material, this nano-cellulose/chitosan composite foam also has less thermal conductivity and thermal expansivity simultaneously, 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 prepares comprises following advantage:
1, the present invention prepares the biopolymer that Mierocrystalline cellulose that composite foam uses and chitosan are pure natural, no cytotoxicity and possess biocompatibility;
2, nano-cellulose/chitosan composite foam has low density (0.006 ~ 0.014g/cm
-3), the feature such as high-specific surface area;
3, the thermal conductivity of nano-cellulose of the present invention/chitosan composite foam is 0.03 ~ 0.032w/ (mk), and hot volumetric shrinkage is low, and volumetric shrinkage is 3% ~ 10%, can as a kind of novel heat-insulating heat-preserving material;
4, nano-cellulose/chitosan composite foam that the present invention obtains be a kind of no cytotoxicity, cell growth without the green compounds of negative interaction, can be used as packaging material for food and Biodegradable scaffold;
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of nano-cellulose/chitosan composite foam that embodiment one obtains;
Fig. 2 is the thermal conductivity histogram of the nano-cellulose/chitosan composite foam of different mass ratio.
Embodiment
Embodiment one: the preparation method of present embodiment nano-cellulose/chitosan composite foam implements according to the following steps:
One, carry out chemical treatment to containing cellulosic biomass material, obtain purifying cellulose, then machinery is carried out to purifying cellulose and separate fine process, prepare nano-cellulose aqueous suspension;
Two, by Glacial acetic acid and distilled water mixing, obtain glacial acetic acid solution, then add chitosan, magnetic agitation is even, obtains chitosan mixing solutions;
Three, the chitosan mixing solutions that the nano-cellulose aqueous suspension and the step 2 that step one are obtained obtain mixes, and obtains nano-cellulose/chitosan composite solution after stirring;
Four, at-20 DEG C, cryogenic freezing process is carried out to nano-cellulose/chitosan composite solution, obtain the mixing solutions freezed;
Five, drying treatment is carried out to the mixing solutions freezed, obtain nano-cellulose/chitosan composite foam;
The concentration of the glacial acetic acid solution wherein described in step 2 is 0.1wt% ~ 4.0wt%, and in chitosan mixing solutions, the concentration of chitosan is 0.1wt% ~ 5.0wt%.
The nano-cellulose obtained after the process of present embodiment drying/chitosan composite foam has tridimensional network, and unique fine structure can improve the nano-cellulose/mechanics of chitosan composite foam, thermal property further.Simultaneously due to features such as had green non-poisonous, lightweight, heat insulation, sound absorption, good biocompatibilities, be applied in fields such as biological support, heat preserving and insulating material, sound-absorbing material, degradable package materials.
Embodiment two: present embodiment and embodiment one are unlike described in step one being timber, bamboo wood, cotton, fiber crops, bacteria cellulose or Ascidian Mierocrystalline cellulose containing cellulosic biomass material.Other step and parameter identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two are adopt sodium chlorite solution to process successively and alkaline solution treatment unlike step one chemical treatment.Other step and parameter identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are treated to supersound process, high-speed stirring process, speed lapping process or high pressure homogenization process unlike the machinery solution fibre described in step one.Other step and parameter identical with one of embodiment one to three.
Embodiment five: present embodiment and embodiment four are the Power Processing 30 ~ 40min with 400 ~ 2000W unlike described supersound process.Other step and parameter identical with embodiment four.
Embodiment six: one of present embodiment and embodiment one to five are 0.1% ~ 10.0% unlike the total mass concentration of nano-cellulose and chitosan in step 3 nano-cellulose/chitosan mixing solutions.Other step and parameter identical with one of embodiment one to five.
Embodiment seven: present embodiment and embodiment six are 4% ~ 8% unlike the total mass concentration of nano-cellulose and chitosan in step 3 nano-cellulose/chitosan mixing solutions.Other step and parameter identical with embodiment six.
Embodiment eight: one of present embodiment and embodiment one to seven are lyophilize, supercritical drying or critical point drying unlike the drying treatment described in step 5.Other step and parameter identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight are 0.1% ~ 5% unlike cellulosic mass percentage in step one nano-cellulose aqueous suspension.Other step and parameter identical with one of embodiment one to eight.
Embodiment one: the preparation method of the present embodiment nano-cellulose/chitosan composite foam implements according to the following steps:
One, by sodium chlorite solution and potassium hydroxide solution, chemical treatment is carried out to 15g China fir wood powder, obtain purifying cellulose, carry out supersound process 30min with the power of 1200W after purifying cellulose being mixed with the aqueous solution, preparation quality concentration is the nano-cellulose aqueous suspension of 1.0wt%;
Two, by Glacial acetic acid and distilled water mixing, obtain the glacial acetic acid solution that concentration is 1.0wt%, then add chitosan, magnetic agitation is even, obtains chitosan mixing solutions;
Three, the chitosan mixing solutions that the nano-cellulose aqueous suspension and the step 2 that step one are obtained obtain mixes, and obtains nano-cellulose/chitosan composite solution that mass concentration is 1.0wt% after stirring;
Four, at-20 DEG C, cryogenic freezing process is carried out to nano-cellulose/chitosan composite solution, obtain the mixing solutions freezed;
Five, carry out lyophilize process to the mixing solutions freezed, condenser temperature is-40 DEG C, and vacuum tightness is 1pa, and time of drying is 50h, obtains nano-cellulose/chitosan composite foam.
The chemical treating process of the present embodiment step a pair China fir wood powder is as follows:
A, the China fir wood powder of 15g to be joined in 1500g distilled water, add 15g Textone and 2mL Glacial acetic acid, use preservative film cover upper container, 1h is heated in 75 DEG C of waters bath with thermostatic control, then continue to add 15g Textone and 2ml Glacial acetic acid, repeat to add Textone and Glacial acetic acid 5 times, cleaning sample; B, to step a cleaning after sample in add 800g, 5wt% potassium hydroxide solution, left at room temperature 10h, then heated sample 2h at 90 DEG C; C, cleaning material after draining step b process, adopt weighting method after dried to survey the mass concentration of purifying cellulose.
In this implementation step two chitosan mixing solutions, the concentration of chitosan is 1.0wt%, and in step 3 nano-cellulose/chitosan composite solution, the solid masses of nano-cellulose and chitosan is than being 10:90.
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), and hot volumetric shrinkage is 10%, and biocompatibility test cell cultivates photo showed cell well-grown, nano-cellulose/chitosan composite foam no cytotoxicity.
Embodiment two: carry out high pressure homogenization process again after the present embodiment and embodiment one carry out supersound process 30min unlike step one purifying cellulose with the power of 1200W, first class pressure is 80bar and secondary pressure is 400bar, process 30min.
Embodiment three: the present embodiment compares for 45:55 with the solid masses of embodiment one unlike nano-cellulose in step 3 and chitosan.
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), and hot volumetric shrinkage is 8.2%, and biocompatibility test cell cultivates photo showed cell well-grown, nano-cellulose/chitosan composite foam no cytotoxicity.
Embodiment four: the present embodiment compares for 30:70 with the solid masses of embodiment one unlike nano-cellulose in step 3 and chitosan.
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), and hot volumetric shrinkage is 3.7%, and biocompatibility test cell cultivates photo showed cell well-grown, nano-cellulose/chitosan composite foam no cytotoxicity.
Embodiment five: the present embodiment and embodiment one carry out supercritical drying process unlike step 5 to the mixing solutions freezed, and the mixing solutions freezed is placed in autoclave, pass into CO at 40 DEG C
2, reach 12MPa to pressure, and keep 1h, afterwards under the condition keeping temperature and pressure, with low discharge Sc CO
2continue to purge sample 4h, to remove solvent remaining in gel, finally by pressure slow releasing to normal pressure, obtain nano-cellulose/chitosan composite foam.
Embodiment six: the preparation method of the present embodiment nano-cellulose/chitosan composite foam implements according to the following steps:
One, by sodium chlorite solution and potassium hydroxide solution, chemical treatment is carried out to China fir wood powder, obtain purifying cellulose, carry out supersound process 30min to purifying cellulose with the power of 1200W after being mixed with the aqueous solution, preparation quality concentration is the nano-cellulose aqueous suspension of 0.5wt%;
Two, by Glacial acetic acid and distilled water mixing, obtain the glacial acetic acid solution that concentration is 0.5wt%, then add chitosan, magnetic agitation is even, obtains the chitosan mixing solutions that chitosan concentration is 0.5wt%;
Three, the chitosan mixing solutions that the nano-cellulose aqueous suspension and the step 2 that step one are obtained obtain mixes, and obtains nano-cellulose/chitosan composite solution that mass concentration is 0.5wt% after stirring;
Four, at-20 DEG C, cryogenic freezing process is carried out to nano-cellulose/chitosan composite solution, obtain the mixing solutions freezed;
Five, carry out lyophilize process to the mixing solutions freezed, condenser temperature is-40 DEG C, and vacuum tightness is 1pa, and time of drying is 50h, obtains nano-cellulose/chitosan composite foam.
In the present embodiment step 3, the solid masses of nano-cellulose and chitosan is than being 10:90.
The density of the nano-cellulose that the present embodiment obtains/chitosan composite foam is 0.0078g/cm
-3, hot volumetric shrinkage is 6.5%, and biocompatibility test cell cultivates photo showed cell well-grown, nano-cellulose/chitosan composite foam no cytotoxicity.
Claims (9)
1. a preparation method for nano-cellulose/chitosan composite foam, it is characterized in that following these steps to realize:
One, carry out chemical treatment to containing cellulosic biomass material, obtain purifying cellulose, then machinery is carried out to purifying cellulose and separate fine process, prepare nano-cellulose aqueous suspension;
Two, by Glacial acetic acid and distilled water mixing, obtain glacial acetic acid solution, then add chitosan, magnetic agitation is even, obtains chitosan mixing solutions;
Three, the chitosan mixing solutions that the nano-cellulose aqueous suspension and the step 2 that step one are obtained obtain mixes, and obtains nano-cellulose/chitosan composite solution after stirring;
Four, at-20 DEG C, cryogenic freezing process is carried out to nano-cellulose/chitosan composite solution, obtain the mixing solutions freezed;
Five, drying treatment is carried out to the mixing solutions freezed, obtain nano-cellulose/chitosan composite foam;
The concentration of the glacial acetic acid solution wherein described in step 2 is 0.1wt% ~ 4.0wt%, and in chitosan mixing solutions, the concentration of chitosan is 0.1wt% ~ 5.0wt%.
2. the preparation method of a kind of nano-cellulose/chitosan composite foam according to claim 1, it is characterized in that described in step one containing cellulosic biomass material be timber, bamboo wood, cotton, fiber crops, bacteria cellulose or Ascidian Mierocrystalline cellulose.
3. the preparation method of a kind of nano-cellulose/chitosan composite foam according to claim 1, is characterized in that step one chemical treatment adopts sodium chlorite solution to process successively and alkaline solution treatment.
4. the preparation method of a kind of nano-cellulose/chitosan composite foam according to claim 1, is characterized in that the machinery solution fibre described in step one is treated to supersound process, high-speed stirring process, speed lapping process or high pressure homogenization process.
5. the preparation method of a kind of nano-cellulose/chitosan composite foam according to claim 4, is characterized in that described supersound process is the Power Processing 30 ~ 40min with 400 ~ 2000W.
6. the preparation method of a kind of nano-cellulose/chitosan composite foam according to claim 1, is characterized in that the total mass concentration of nano-cellulose and chitosan in step 3 nano-cellulose/chitosan mixing solutions is 0.1% ~ 10.0%.
7. the preparation method of a kind of nano-cellulose/chitosan composite foam according to claim 6, is characterized in that the total mass concentration of nano-cellulose and chitosan in step 3 nano-cellulose/chitosan mixing solutions is 4% ~ 8%.
8. the preparation method of a kind of nano-cellulose/chitosan composite foam according to claim 1, is characterized in that the drying treatment described in step 5 is lyophilize, supercritical drying or critical point drying.
9. the preparation method of a kind of nano-cellulose/chitosan composite foam according to claim 1, is characterized in that in step one nano-cellulose aqueous suspension, cellulosic mass percentage is 0.1% ~ 5%.
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| CN105396561A (en) * | 2015-12-12 | 2016-03-16 | 常州大学 | Preparation method for holocellulose/chitosan microsphere adsorbent |
| CN105949514A (en) * | 2016-05-03 | 2016-09-21 | 广西大学 | Method for preparing nano-crystalline cellulose of flexible screen matrix material |
| CN105949778A (en) * | 2016-06-06 | 2016-09-21 | 凤阳加松新型材料科技有限公司 | High-toughness antimicrobial silica gel baking mat |
| CN106009691A (en) * | 2016-06-06 | 2016-10-12 | 凤阳加松新型材料科技有限公司 | High-toughness antibacterial baking cushion and preparation method thereof |
| CN106065183A (en) * | 2016-06-06 | 2016-11-02 | 凤阳加松新型材料科技有限公司 | A kind of ageing-resistant antibacterial roasting pad |
| CN108079966A (en) * | 2017-12-26 | 2018-05-29 | 肇庆市华师大光电产业研究院 | A kind of carbonitride/cellulose aerogels composite photo-catalyst and its preparation method and application |
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| CN110791829A (en) * | 2018-08-02 | 2020-02-14 | 华南理工大学 | Preparation method and application of nano antibacterial fiber |
| CN111171384A (en) * | 2020-02-10 | 2020-05-19 | 东华大学 | Light warm-keeping flexible chitosan/nano-cellulose aerogel and preparation method thereof |
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| CN105169477A (en) * | 2015-08-15 | 2015-12-23 | 罗卫华 | Preparation method of nano cellulose/chitosan/polycaprolactone porous scaffold |
| CN105396561A (en) * | 2015-12-12 | 2016-03-16 | 常州大学 | Preparation method for holocellulose/chitosan microsphere adsorbent |
| CN105949514A (en) * | 2016-05-03 | 2016-09-21 | 广西大学 | Method for preparing nano-crystalline cellulose of flexible screen matrix material |
| CN105949778A (en) * | 2016-06-06 | 2016-09-21 | 凤阳加松新型材料科技有限公司 | High-toughness antimicrobial silica gel baking mat |
| CN106009691A (en) * | 2016-06-06 | 2016-10-12 | 凤阳加松新型材料科技有限公司 | High-toughness antibacterial baking cushion and preparation method thereof |
| CN106065183A (en) * | 2016-06-06 | 2016-11-02 | 凤阳加松新型材料科技有限公司 | A kind of ageing-resistant antibacterial roasting pad |
| CN108079966A (en) * | 2017-12-26 | 2018-05-29 | 肇庆市华师大光电产业研究院 | A kind of carbonitride/cellulose aerogels composite photo-catalyst and its preparation method and application |
| EP3794068A4 (en) * | 2018-05-07 | 2022-03-16 | Cruz Foam, Inc. | Biodegradable foams |
| CN110791829B (en) * | 2018-08-02 | 2020-09-22 | 华南理工大学 | Preparation method and application of nano antibacterial fiber |
| CN110791829A (en) * | 2018-08-02 | 2020-02-14 | 华南理工大学 | Preparation method and application of nano antibacterial fiber |
| CN111777790A (en) * | 2019-04-04 | 2020-10-16 | 西南林业大学 | Simple, efficient, green and environment-friendly preparation method of nano lignocellulose-chitin nanofiber aerogel |
| CN109942897A (en) * | 2019-04-04 | 2019-06-28 | 西南林业大学 | A kind of preparation of environment-protection low-consumption type nano-chitosan-chitosan-fibrillation cellulose composite material |
| CN110591141A (en) * | 2019-09-02 | 2019-12-20 | 广西大学 | Holocellulose composite aerogel and preparation method thereof |
| 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 | Light warm-keeping flexible chitosan/nano-cellulose aerogel and preparation method thereof |
| CN111420619A (en) * | 2020-03-19 | 2020-07-17 | 南京航空航天大学 | Preparation method of cellulose-chitosan/PANI composite aerogel |
| CN111420619B (en) * | 2020-03-19 | 2022-04-05 | 南京航空航天大学 | Preparation method of cellulose-chitosan/PANI composite aerogel |
| CN114377188A (en) * | 2022-01-14 | 2022-04-22 | 宋金华 | Super-absorbent bio-based foam material and preparation method and application thereof |
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