CN103965571A - Polyvinyl alcohol composite foam material and preparation method thereof - Google Patents
Polyvinyl alcohol composite foam material and preparation method thereof Download PDFInfo
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- CN103965571A CN103965571A CN201410229516.3A CN201410229516A CN103965571A CN 103965571 A CN103965571 A CN 103965571A CN 201410229516 A CN201410229516 A CN 201410229516A CN 103965571 A CN103965571 A CN 103965571A
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- polyvinyl alcohol
- nanofiber
- foam material
- composite foam
- alcohol composite
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Abstract
The invention provides a polyvinyl alcohol composite foam material and a preparation method thereof, and relates to the technical field of nano materials. The polyvinyl alcohol composite foam material is composed of polyvinyl alcohol and nanofiber. The preparation method of the polyvinyl alcohol composite material comprises the following steps of: adding nanofiber suspension liquid in polyvinyl alcohol liquor, evaporating a solvent under a stirring state, freezing and forming, and freezing and drying to obtain the polyvinyl alcohol composite foam material. The polyvinyl alcohol composite foam material disclosed by the invention is added with nanofiber, so that water resistance of the foam material is strengthened, and therefore, dimension stability of foams is improved; on the other hand, compression strength resistance and modulus of the foam are increased. The preparation method disclosed by the invention is carried out in a water-phase solvent without adding organic substances, and a freeze-drying method is adopted, so that process is green and pollution-free; and moreover, nanofiber in the materials is renewable resources such as cellulose, chitin, chitosan, and the like; and the composite foam is green and degradable environment-friendly material.
Description
Technical field
The present invention relates to field of nanometer material technology, be specifically related to a kind of polyvinyl alcohol porous composite foam material and preparation method thereof.
Background technology
Polyvinyl alcohol is a kind of water-soluble polyhydroxyl polymer, it has a lot of excellent specific properties as wetting ability, biological activity, film-forming properties and good mechanical property, and nontoxic, cost is low, biodegradable, therefore be widely used in biomedicine and wrapping material field, polyvinyl alcohol foam is also subject to extensive concern.But in prior art, polyvinyl alcohol porous foam, in moister environment, easily absorbs moisture, thereby makes volume-diminished, fades away in hole, not the frothy speciality of tool.
Summary of the invention
The object of this invention is to provide that a kind of good waterproof performance, ultimate compression strength are high, the polyvinyl alcohol composite foam material of dimensional stabilizing.
Another object of the present invention is to provide a kind of preparation method of polyvinyl alcohol composite foam material.
Object of the present invention adopts following technical scheme to realize.
A kind of polyvinyl alcohol composite foam material, is made up of polyvinyl alcohol and nanofiber.
In the present invention, the weight percentage of the each composition of polyvinyl alcohol composite foam material is: nanofiber 20%-60%, polyvinyl alcohol 80%-40%.
In the present invention, described nanofiber derives from Mierocrystalline cellulose, chitosan, chitin.
In the present invention, described Mierocrystalline cellulose source is bamboo fibers, xylon, Microcrystalline Cellulose, and described chitin, chitosan derive from shrimp crab crust, mycelium, insect, silkworm chrysalis.
In the present invention, the diameter of described nanofiber is 20-80nm, and length is 2-50 μ m.
The present invention also provides the preparation method of described polyvinyl alcohol composite foam material, comprise the steps: nanofiber suspension to add in polyvinyl alcohol solution, under whipped state, evaporating solvent to the weight percentage of polyvinyl alcohol and nanofiber is 1%-10%, freezing shaping, then lyophilize, obtains described polyvinyl alcohol composite foam material.
In the present invention, the method for described freezing shaping is: freezing 1-3 days under-20 DEG C～-80 DEG C conditions, or be placed in liquid nitrogen quick freezing.
In the present invention, in described nanofiber suspension, the mass percent of nanofiber is 0.5%-5%; In described nanofiber suspension, the diameter of nanofiber is 20-80nm, and length is 2-50 μ m.
In the present invention, the preparation method of described nanofiber suspension is as follows: by nanofiber raw material pulverizing, boil, mill, immersion, ultrasonic dispersion, obtain described nanofiber suspension after high-pressure homogeneous.
In the present invention, the mass percentage concentration of described polyvinyl alcohol solution is 1%-15%.
beneficial effect
The present invention compared to existing technology tool has the following advantages:
1. polyvinyl alcohol has very strong water-absorbent, and the foam materials of preparing with it is easily water suction distortion, poor stability in wet environment.Polyvinyl alcohol composite foam material of the present invention has added nanofiber, has reduced the water-intake rate of polyvinyl alcohol, has strengthened the dimensional stability under wet condition, and mechanical property raising, and resistance to compression is strong.
2. preparation method of the present invention carries out in aqueous phase solvent, does not need to add organism, adopts freeze-drying, and synthesis technique is simple, building-up process green non-pollution, products obtained therefrom environmental protection; Use renewable resources, with low cost.
3. nanofiber has that source is wide, price is low, the advantage of easy preparation, it add intensity, the water-repellancy that can obviously promote foam and the degradation speed that accelerates foam materials.
4. this degradable stephanoporate composite foam material is with a wide range of applications in fields such as energy storage, biological skeleton, organic waste or heavy metal ion adsorbed and food product pack.
Brief description of the drawings
Fig. 1 is the cellulose nano-fibrous transmission electron microscope photo (TEM) that embodiment 1 obtains, and the diameter of nanofiber is 20-80nm, and length is 2-50 μ m.
Fig. 2 is an embodiment 7(left side) polyvinyl alcohol foam and the embodiment 4(right side) the stereoscan photograph (SEM) of cellulose nano-fibrous enhancing composite foam.Wherein (A) is the stereoscan photograph of foam materials 7, the stereoscan photograph that (B) is foam materials 4.
Fig. 3 is that the length of side is the pattern picture after the cubic foam materials 7, foam materials 6, foam materials 4, foam materials 3 water absorption tests of 25mm, is followed successively by from left to right foam materials 7, foam materials 6, foam materials 4, foam materials 3, contrast (the cubic foam materials 7 that the length of side is 25mm do not absorb water state).
Embodiment
Taking cellulose nano-fibrous as example, the present invention is further illustrated with concrete embodiment by reference to the accompanying drawings below.
the preparation of embodiment 1 nanofiber suspension
Method one
(1) shear and boil: get 5g paper (composition is Mierocrystalline cellulose) and with medical scissors, raw material is shredded to (diameter is less than 1mm) and put into there-necked flask, add deionized water 95mL, boil 1 hour, obtain slurry.
(2) mill: after slurry is cooling, pour into and in wet wheeling machine, mill 1 time (gear spacing 0.5 μ m), each 2 minutes.
(3) immersion and ultrasonic dispersion: adding deionized water to make the massfraction of nanofiber in the slurry after milling is 5%, soaks after 1 hour ultrasonic 2 (ultrasonic frequency 2000H
z), each 2 minutes.
(4) high pressure homogenizing: the slurry that step (3) obtains after processing speed with 50ml/min under 150MPa is passed through high pressure homogenizing device 20 times, obtain nanofiber suspension, wherein the length of nanofiber is 12-20 μ m, and diameter is 30-35nm, and transmission electron microscope is illustrated in Fig. 1.
Method two
(1) shear and boil: get 5g paper (composition is Mierocrystalline cellulose) and with medical scissors, raw material is shredded to (diameter is less than 1mm) and put into there-necked flask, add deionized water 950mL, boil 10 hours, obtain slurry.
(2) mill: after slurry is cooling, pour into and in wet wheeling machine, mill 10 times (gear spacing 5 μ m), each 15 minutes.
(3) immersion and ultrasonic dispersion: adding deionized water to make the massfraction of nanofiber in the slurry after milling is 0.5%, soaks after 24 hours ultrasonic 10 (ultrasonic frequency 50H
z), each 30 minutes.
(4) high pressure homogenizing: the slurry that step (3) obtains after processing speed with 200ml/min under 300MPa is passed through high pressure homogenizing device 1 time, obtain nanofiber suspension, wherein the length of nanofiber is 35-40 μ m, and diameter is 50-55nm.
Method three
(1) shear and boil: get 5g paper (composition is Mierocrystalline cellulose) and with medical scissors, raw material is shredded to (diameter is less than 1mm) and put into there-necked flask, add deionized water 500mL, boil 5 hours, obtain slurry.
(2) mill: after slurry is cooling, pour into and in wet wheeling machine, mill 5 times (gear spacing 2.5 μ m), each 8 minutes.
(3) immersion and ultrasonic dispersion: adding deionized water to make the massfraction of nanofiber in the slurry after milling is 3%, soaks after 10 hours ultrasonic 5 (ultrasonic frequency 1000H
z), each 15 minutes.
(4) high pressure homogenizing: the slurry that step (3) obtains after processing speed with 120ml/min under 200MPa is passed through high pressure homogenizing device 15 times, obtain nanofiber suspension, wherein the length of nanofiber is 15-20 μ m, and diameter is 35-40nm.
the preparation of embodiment 2 polyvinyl alcohol solutions
Take 5g polyvinyl alcohol (PVA) powder and be positioned in there-necked flask, add 45-495mL deionized water, at 80-100 DEG C, under stirring velocity 60-500r/min, stir 0.5-3 hour, to dissolving completely, obtaining massfraction is the PVA solution of 1%-10%, and cooling, low temperature (1-4 DEG C) is preserved.
embodiment 3
Take PVA solution in example 2 (containing 0.8g polyvinyl alcohol), be positioned in there-necked flask, under churned mechanically condition, in there-necked flask, add nanofiber suspension in embodiment 1 (containing 1.2g nanofiber), under whipped state, be warming up to 80 DEG C, transpiring moisture to remainder quality is 40g.Then remainder is poured in culture dish coolingly, at 1-4 DEG C, placed 2 days, be then placed in freezing 1 day of the cryogenic refrigerator of-78 DEG C, take out lyophilize 24h in Freeze Drying Equipment and obtain foam materials 3.In foam materials 3, the quality percentage composition of nanofiber is 60%.
embodiment 4
Take PVA solution in example 2 (containing 1.2g polyvinyl alcohol), be positioned in there-necked flask, under churned mechanically condition, in there-necked flask, add nanofiber suspension in embodiment 1 (containing 0.8g nanofiber), under whipped state, being warming up to 100 DEG C of transpiring moistures to remainder quality is 100g, then remainder is poured in culture dish cooling, at 1-4 DEG C, place 5 days, then be placed in freezing 3 days of the cryogenic refrigerator of-78 DEG C, take out lyophilize 72h in Freeze Drying Equipment and obtain foam materials 4.In foam materials 4, the quality percentage composition of nanofiber is 40%.
embodiment 5
Taking PVA solution in example 2 (containing 1.4g polyvinyl alcohol) is positioned in there-necked flask, under churned mechanically condition, in there-necked flask, add nanofiber suspension in embodiment 1 (containing 0.6g nanofiber), under whipped state, being warming up to 90 DEG C of transpiring moistures to remainder quality is 80g, then pour in culture dish first cooling, at 1-4 DEG C, place 3 days, then be placed in freezing 2 days of the cryogenic refrigerator of-78 DEG C, take out lyophilize 48h in Freeze Drying Equipment and obtain foam materials 5.In foam materials 5, the quality percentage composition of nanofiber is 30%.
embodiment 6
Taking PVA solution in example 2 (containing 1.6g polyvinyl alcohol) is positioned in there-necked flask, under churned mechanically condition, in there-necked flask, add nanofiber suspension in embodiment 1 (containing 0.4g nanofiber), under whipped state, being warming up to 90 DEG C of transpiring moistures to remainder quality is 70g, then remainder is poured in culture dish first cooling, at 1-4 DEG C, place 3 days, then be placed in freezing 2 days of the cryogenic refrigerator of-78 DEG C, take out lyophilize 40h in Freeze Drying Equipment and obtain foam materials 6.In foam materials 6, the quality percentage composition of nanofiber is 20%.
embodiment 7
In there-necked flask, add the deionized water of 2g polyvinyl alcohol and 70ml, individual hour of mechanical stirring 1-3 under 90 DEG C of conditions, and continue at normal temperatures to stir 1-3 hour to dissolving completely, obtain polyvinyl alcohol solution.Polyvinyl alcohol solution is poured in culture dish first cooling, at 1-4 DEG C, placed 3 days, be then placed in freezing 2 days of the cryogenic refrigerator of-78 DEG C, take out lyophilize 48h in Freeze Drying Equipment and obtain foam materials 7.The scanning electron microscope (SEM) photograph of foam materials 4 prepared by foam materials 7 and embodiment 4, as Fig. 2, can find out that foam materials 7 is laminated structures, be easy to absorb moisture and form lamella pile up, cause volume to reduce, be out of shape.Foam materials 4 is the netted structures of obvious Mierocrystalline cellulose, and the dimensional stability to composite foam and mechanical property all play promoter action.
embodiment 8
Prepare foam materials according to method in embodiment 4, only change preliminary freezing method and be freezing 2 days of the cryogenic refrigerator that is placed in-61 DEG C, obtain foam materials 8.
embodiment 9
Prepare foam materials according to method in embodiment 4, only change preliminary freezing method and be freezing 3 days of the cryogenic refrigerator that is placed in-20 DEG C, obtain foam materials 9.
embodiment 10
Prepare foam materials according to method in embodiment 4, only changing preliminary freezing method is quick freezing in liquid nitrogen, obtains foam materials 10.
Table 1. embodiment sample mechanical property, porosity and water-absorbent parameters.
| Embodiment sample | Stress under compression (kPa) | Young's modulus (MPa) | Porosity (%) | Water-intake rate (%) | Foam size (mm) after water suction | Volume washing shrinkage (%) |
| Foam materials 3 | 85.9 | 0.23 | 91.88 | 11.38 | 24.8 | 2.4% |
| Foam materials 4 | 141.7 | 0.29 | 91.85 | 11.87 | 23.6 | 15.8% |
| Foam materials 5 | 328.5 | 0.56 | 91.78 | 11.94 | 23.5 | 16.9% |
| Foam materials 6 | 263.3 | 0.34 | 89.71 | 13.38 | 20.9 | 41.6% |
| Foam materials 7 | 202.7 | 0.32 | 77.32 | 15.70 | 16.6 | 70.7% |
| Foam materials 8 | 134.2 | 0.27 | 92.03 | 11.85 | 23.5 | 16.9% |
| Foam materials 9 | 119.7 | 0.26 | 92.36 | 11.88 | 23.6 | 15.8% |
| Foam materials 10 | 164.1 | 0.30 | 88.72 | 11.84 | 23.9 | 12.6% |
The mechanical property of above-mentioned table 1 is the value that each foam materials is measured under 50% draught.In addition, getting respectively the length of side is the cubic foam materials 3-10 of 25mm, detects its water absorbing properties, comprises water-intake rate, the rear foam size (length of side) of water suction and volume washing shrinkage, and concrete data are as table 1 and Fig. 3.Can see that foam materials prepared by the inventive method has lower water-intake rate, reduce the water-absorbent in wet environment, on-deformable, and also resistance to compression is strong; The foam materials 7 that only adopts polyvinyl alcohol to prepare, water-intake rate is higher, and volume washing shrinkage is also very large.As can be seen from Figure 3 the rear volume change of foam materials 7 water suction that only adopts polyvinyl alcohol to prepare is very large, and adds the composite foam of nanofiber to greatly reduce the variation of lather volume.
Claims (10)
1. a polyvinyl alcohol composite foam material, is characterized in that: described polyvinyl alcohol composite foam material is made up of polyvinyl alcohol and nanofiber.
2. polyvinyl alcohol composite foam material according to claim 1, is characterized in that the weight percentage of the each composition of described polyvinyl alcohol composite foam material is: nanofiber 20%-60%, polyvinyl alcohol 40%-80%.
3. according to polyvinyl alcohol composite foam material described in claim 1 or 2, it is characterized in that described nanofiber derives from Mierocrystalline cellulose, chitosan, chitin.
4. polyvinyl alcohol composite foam material according to claim 3, is characterized in that described Mierocrystalline cellulose source is bamboo fibers, xylon, Microcrystalline Cellulose, and described chitin and chitosan derives from shrimp crab crust, mycelium, insect, silkworm chrysalis.
5. polyvinyl alcohol composite foam material according to claim 4, the diameter that it is characterized in that described nanofiber is 20-80 nm, length is 2-50 μ m.
6. the preparation method of the described polyvinyl alcohol composite foam material of one of claim 1-5, it is characterized in that comprising the steps: nanofiber suspension is added in polyvinyl alcohol solution, under whipped state, evaporating solvent to the weight percentage of polyvinyl alcohol and nanofiber is 1%-10%, freezing shaping, then lyophilize, obtains described polyvinyl alcohol composite foam material.
7. the preparation method of polyvinyl alcohol composite foam material according to claim 6, is characterized in that the method for described freezing shaping is: freezing 1-3 days under-20 DEG C～-80 DEG C conditions, or be placed in liquid nitrogen quick freezing.
8. the preparation method of polyvinyl alcohol composite foam material according to claim 7, the mass percent that it is characterized in that nanofiber in described nanofiber suspension is 0.5%-5%; In described nanofiber suspension, the diameter of nanofiber is 20-80nm, and length is 2-50 μ m.
9. the preparation method of polyvinyl alcohol composite foam material according to claim 8, is characterized in that the preparation method of described nanofiber suspension is as follows: by nanofiber raw material pulverizing, boil, mill, immersion, ultrasonic dispersion, obtain described nanofiber suspension after high-pressure homogeneous.
10. the preparation method of polyvinyl alcohol composite foam material according to claim 8, the mass percentage concentration that it is characterized in that described polyvinyl alcohol solution is 1%-15%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371141A (en) * | 2014-11-21 | 2015-02-25 | 南京林业大学 | Method for preparing nano-crystalline cellulose enhanced polyvinyl alcohol foam material with oriented porous structure |
| CN105951189A (en) * | 2016-05-31 | 2016-09-21 | 苏州大学 | Nanofiber solution and preparation method thereof |
| WO2017088038A1 (en) * | 2015-11-23 | 2017-06-01 | Universidade Federal Do Paraná | Use and production of chitosan and/or nanochitosan dry foam and powder by foam layer drying method |
| CN109364894A (en) * | 2018-11-22 | 2019-02-22 | 中国科学院新疆理化技术研究所 | A kind of Preparation method and use of the composite sponge adsorbent of quick adsorption mercury ion |
| CN109897315A (en) * | 2019-03-05 | 2019-06-18 | 中原工学院 | A kind of preparation method of maleated polypropylene micro nanometer fiber/polyvinyl alcohol foam material |
| CN109912911A (en) * | 2019-03-05 | 2019-06-21 | 中原工学院 | A kind of preparation method of polymer micro-nanometer fiber enhancing polyvinyl alcohol foam material |
| CN112280091A (en) * | 2020-10-29 | 2021-01-29 | 南京信息工程大学 | Biomass-based antiviral filter material and synthesis method thereof |
| 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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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371141A (en) * | 2014-11-21 | 2015-02-25 | 南京林业大学 | Method for preparing nano-crystalline cellulose enhanced polyvinyl alcohol foam material with oriented porous structure |
| WO2017088038A1 (en) * | 2015-11-23 | 2017-06-01 | Universidade Federal Do Paraná | Use and production of chitosan and/or nanochitosan dry foam and powder by foam layer drying method |
| CN105951189A (en) * | 2016-05-31 | 2016-09-21 | 苏州大学 | Nanofiber solution and preparation method thereof |
| CN109364894A (en) * | 2018-11-22 | 2019-02-22 | 中国科学院新疆理化技术研究所 | A kind of Preparation method and use of the composite sponge adsorbent of quick adsorption mercury ion |
| CN109364894B (en) * | 2018-11-22 | 2021-08-17 | 中国科学院新疆理化技术研究所 | Preparation method and application of composite sponge adsorbent for rapidly adsorbing mercury ions |
| CN109897315A (en) * | 2019-03-05 | 2019-06-18 | 中原工学院 | A kind of preparation method of maleated polypropylene micro nanometer fiber/polyvinyl alcohol foam material |
| CN109912911A (en) * | 2019-03-05 | 2019-06-21 | 中原工学院 | A kind of preparation method of polymer micro-nanometer fiber enhancing polyvinyl alcohol foam material |
| CN109912911B (en) * | 2019-03-05 | 2021-10-29 | 中原工学院 | Preparation method of polymer micro-nanofiber reinforced polyvinyl alcohol foam material |
| CN109897315B (en) * | 2019-03-05 | 2021-10-29 | 中原工学院 | Preparation method of maleic anhydride polypropylene micro-nanofiber/polyvinyl alcohol foam material |
| CN112280091A (en) * | 2020-10-29 | 2021-01-29 | 南京信息工程大学 | Biomass-based antiviral filter material and synthesis method thereof |
| CN112280091B (en) * | 2020-10-29 | 2022-11-29 | 南京信息工程大学 | Biomass-based antiviral filter material and synthesis method thereof |
| 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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