CN103613781B - A kind of preparation method based on three-dimensional netted chitosan loaded super-hydrophobic particle oil suction sponge - Google Patents
A kind of preparation method based on three-dimensional netted chitosan loaded super-hydrophobic particle oil suction sponge Download PDFInfo
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- CN103613781B CN103613781B CN201310592718.XA CN201310592718A CN103613781B CN 103613781 B CN103613781 B CN 103613781B CN 201310592718 A CN201310592718 A CN 201310592718A CN 103613781 B CN103613781 B CN 103613781B
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 86
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002245 particle Substances 0.000 title claims abstract description 12
- 244000205754 Colocasia esculenta Species 0.000 claims abstract description 42
- 235000006481 Colocasia esculenta Nutrition 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 39
- 238000010521 absorption reaction Methods 0.000 claims abstract description 9
- 238000004108 freeze drying Methods 0.000 claims abstract description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 19
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 15
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000007710 freezing Methods 0.000 claims description 12
- 230000008014 freezing Effects 0.000 claims description 12
- -1 polydimethylsiloxane Polymers 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- 230000006870 function Effects 0.000 abstract description 4
- 230000006835 compression Effects 0.000 abstract description 2
- 238000007906 compression Methods 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract description 2
- 230000006386 memory function Effects 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 30
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 150000004676 glycans Chemical group 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- UPLPHRJJTCUQAY-WIRWPRASSA-N 2,3-thioepoxy madol Chemical group C([C@@H]1CC2)[C@@H]3S[C@@H]3C[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@](C)(O)[C@@]2(C)CC1 UPLPHRJJTCUQAY-WIRWPRASSA-N 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
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Abstract
Based on a preparation method for three-dimensional netted chitosan loaded super-hydrophobic particle oil suction sponge, relate to a kind of preparation method of super-hydrophobic three-dimensional netted oil absorption material.Preparation method's step of super-hydrophobic oil suction chitosan sponge of the present invention is as follows: (1) adopts freeze-drying to prepare chitosan three-dimensional network sponge.(2) prepare super-hydrophobic taro leaf powder (3) and the super-hydrophobic taro leaf powder in step 2 is assembled into three-dimensional netted chitosan surface.Obtain super-hydrophobic chitosan three-dimensional network sponge.Chitosan three-dimensional network structure prepared by the present invention a kind of three-dimensional nettedly has shape memory function sponge, can Repeated Compression, release, and then there is the function of absorbing fluid.Make it have super-hydrophobic oleophylic function after the hole wall of three-dimensional netted chitosan is assembled one deck super-hydrophobic particle, the object of selectivity oil suction can be reached.<sub />
Description
Technical field
The present invention relates to a kind of preparation method of super-hydrophobic three-dimensional netted oil absorption material.
Background technology
Along with the frequent generation that increase and the marine oil of industrial oily waste water discharge leak, how effective implemention oily water separation becomes one of focus of current research.According to statistics, the annual oil spilling flowed into the sea because of various accident is up to 3000 ~ 5000kt in the world, and it is havoc marine ecology balance not only, contaminate environment, but also causes great energy dissipation.Recent study finds, the solid surface simultaneously having super-hydrophobicity and super-oleophilic concurrently is the effective ways solving oily water separation.The developing direction of oil absorber is that synthesis speed of oil absorption is fast, is suitable for face width, abundant raw material source, and biodegradable, not easily causes secondary pollution.
At present, remove method that marine oils pollutes mainly contain from, so facture, contain with reclaim, marine burn oil spilling, dispersion method, the precipitator method, biological restoring method and sorbing material method etc.At present, studying more deoiling method is sorbing material method, namely utilizes the oleophylic performance of material, greasy dirt is adsorbed in material internal and as the container of temporary reservoir greasy dirt, then the material after absorption greasy dirt being carried out desorption process can isolate greasy dirt.Natural organic type sorbing material is novel absorption material, is easy to get with low cost and protects oily rate high and receive much concern due to its raw material.
Current taro leaf is applied to and reclaims leakage of oil and have been reported and excellent performance, but itself and chitosan skeleton are combined into super-hydrophobic oil suction sponge have no report.
Summary of the invention
The object of this invention is to provide a kind of preparation method based on three-dimensional netted chitosan loaded super-hydrophobic particle oil suction sponge, adopt lyophilize and absorption method to prepare super-hydrophobic chitosan composite sponge.It is a kind of simple, convenient, method that parameter is controlled that freeze-drying prepares chitosan sponge, and the method is that certain density chitosan solution is carried out lyophilize, its self-assembling formation three-dimensional network shape after dry.Taro leaf comes from green plants, natural biologic material is used for a kind of method that leakage of oil recovery is very economical environment-protective, chitosan is a kind of biological environmental production material, its biodegradability is good, is convenient to secondary recovery, and can not cause secondary pollution, and there is good oil absorptiveness and recycle performance, solve existing oil suction product oil absorbency now low, cause secondary pollution, super-hydrophobic oil absorption material prepared by the method is expected to the new direction becoming the development of following oil absorption material.
Preparation method based on three-dimensional netted chitosan loaded super-hydrophobic particle oil suction sponge of the present invention, step is as follows:
1st step, employing freeze-drying prepare chitosan sponge
Be transferred to by chitosan solution in furnace pot, cover filter paper on vessel top, and seal with scotch tape, be then placed in the cold steel pole at freeze drier top, by liquid nitrogen cooling with completely freezing, freezing temp scope is-5 ~-60 DEG C; Three-dimensional network shape chitosan is frozen into ice crystal by water-cooled and is formed after dry removing;
2nd step, prepare super-hydrophobic taro leaf powder:
Clayed into power by dried taro leaf, powder uses fine mesh filter further; Then, after drying 2 ~ 48h in 25 ~ 90 DEG C of vacuum, super-hydrophobic taro leaf powder is obtained;
3rd step, synthesize super-hydrophobic chitosan three-dimensional network sponge:
Super-hydrophobic taro leaf powder in step 2 is dissolved in the chloroform soln of polydimethylsiloxane (PDMS), fully stirs; Join in above-mentioned solution after chitosan three-dimensional network sponge is compressed, and repeatedly carry out compressing, expanding; Take out after 0.2 ~ 5h, at 25 ~ 100 DEG C, solidify 0.5 ~ 24h, obtain super-hydrophobic chitosan three-dimensional network sponge.
The present invention utilizes the chitosan that aboundresources, biodegradability are excellent to be raw material, preparation three-dimensional network shape chitosan sponge, and carries out modification to it, makes it have good ultra-hydrophobicity and oleophylic performance, good circulation use properties.Chitosan structure prepared by the present invention a kind of three-dimensional nettedly has shape memory function sponge, can Repeated Compression, release, and then there is the function of absorbing fluid.Make it have super-hydrophobic oleophylic function after the hole wall of three-dimensional netted chitosan is assembled one deck super-hydrophobic particle, the object of selectivity oil suction can be reached.
The preparation method of chitosan of the present invention super-hydrophobic oil suction sponge is simple to operate, experiment parameter is controlled, cost is low, can be used for manufacturing a kind of super-hydrophobic oil suction sponge, this super-hydrophobic oil suction sponge is that three-dimensional net structure has very strong hydrophobicity and oil absorbency, and there is biological degradability, secondary recovery is convenient.
The super-hydrophobic oil suction sponge of chitosan that the present invention adopts lyophilize to prepare in conjunction with chemiadsorption, the area of its sponge is 1cm
2~ 80dm
3, three-dimensional porous size is at 0.5 μm ~ 1cm, and the diameter of hydrophobicity powder particles is at 0.1 ~ 50 μm.
Accompanying drawing explanation
Fig. 1 is the preparation process schematic diagram of the super-hydrophobic oil suction sponge of chitosan;
Fig. 2 is chitosan super-hydrophobic oil suction sponge structure schematic diagram.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment one: as shown in Figure 1, present embodiment prepares the super-hydrophobic oil suction sponge of chitosan in accordance with the following steps:
1st step, employing freeze-drying prepare chitosan sponge
Chitosan powder is dissolved in aqueous acetic acid (2wt%), the chitosan solution of preparation 0.1 ~ 10wt%; Be transferred to by chitosan solution in furnace pot, cover filter paper on vessel top, and seal with scotch tape, be then placed in the cold steel pole at freeze drier top, by liquid nitrogen cooling with completely freezing, freezing temp scope is-5 ~-60 DEG C; Three-dimensional network shape chitosan is frozen into ice crystal by water-cooled and is formed after dry removing.
2nd step, prepare super-hydrophobic taro leaf powder:
Preparation taro leaf powder: fresh taro leaf is cut into small pieces, repeatedly washes away screw tap with deionized water, at room temperature dry 1 ~ 3 week; Clayed into power by dried taro leaf, powder uses the fine mesh filter of < 50 μm further; Then, after drying 2 ~ 48h in 25 ~ 90 DEG C of vacuum, super-hydrophobic taro leaf powder is obtained.
3rd step, synthesize super-hydrophobic chitosan three-dimensional network sponge:
Super-hydrophobic taro leaf powder in step 2 is dissolved in 100mL and contains 0.01 ~ 10%(w/w) in the chloroform soln of polydimethylsiloxane (PDMS), fully stir; Join in the chloroform soln (100mL) of the polydimethylsiloxane (PDMS) being dissolved with taro leaf powder after chitosan three-dimensional network sponge is compressed, and repeatedly carry out compressing, expanding; Take out after 0.2 ~ 5h, at 25 ~ 100 DEG C, solidify 0.5 ~ 24h, obtain super-hydrophobic chitosan three-dimensional network sponge.
Embodiment two: present embodiment prepares the super-hydrophobic oil suction sponge of chitosan in accordance with the following steps:
1st step, employing freeze-drying prepare chitosan sponge
Chitosan powder (2g) is dissolved in the aqueous acetic acid (2wt%) of 100 milliliters, preparation chitosan solution (2wt%); Be transferred to by chitosan solution in furnace pot, cover filter paper on vessel top, and seal with scotch tape, be then placed in the cold steel pole at top, by liquid nitrogen cooling with completely freezing, freezing temp is-5 DEG C; Three-dimensional network shape chitosan is frozen into ice crystal by water-cooled and forms three-dimensional netted chitosan skeleton after dry removing.
2nd step, prepare super-hydrophobic taro leaf powder
Preparation taro leaf powder: fresh taro leaf is cut into small pieces, repeatedly washes away screw tap with deionized water, at room temperature dry 2 weeks; Clayed into power by dried taro leaf, powder uses the fine mesh filter of 50 μm further; Taro leaf powder (yy) is obtained after drying in vacuum.
3rd step, synthesize super-hydrophobic chitosan three-dimensional network sponge
Super-hydrophobic taro leaf powder in step 2 is dissolved in 1%(w/w) in the chloroform soln (100mL) of polydimethylsiloxane (PDMS), fully stir; Join in above-mentioned solution after chitosan three-dimensional network sponge is compressed, and repeatedly carry out compressing, expanding; Take out after 2h, at 80 DEG C, solidify 1h, obtain super-hydrophobic chitosan three-dimensional network sponge.
The area of super-hydrophobic chitosan three-dimensional network sponge prepared by present embodiment is 4cm
2, its structure is glycan three-dimensional network sponge load super-hydrophobic taro leaf powder, and three-dimensional network hole dimension is 50 ~ 600 μm (Fig. 2), and the thickness of skeleton wall is 500 ~ 1000nm.
Embodiment three: present embodiment prepares the super-hydrophobic oil suction sponge of chitosan in accordance with the following steps:
1st step, employing freeze-drying prepare chitosan sponge
Chitosan powder (4g) is dissolved in the aqueous acetic acid (2wt%) of 200 milliliters, preparation chitosan solution (2wt%); Be transferred to by chitosan solution in furnace pot, cover filter paper on vessel top, and seal with scotch tape, be then placed in the cold steel pole at top, by liquid nitrogen cooling with completely freezing, freezing temp is-20 DEG C; Three-dimensional network shape chitosan is frozen into ice crystal by water-cooled and forms three-dimensional netted chitosan skeleton after dry removing.
2nd step, prepare super-hydrophobic taro leaf powder
Preparation taro leaf powder: fresh taro leaf is cut into small pieces, repeatedly washes away screw tap with deionized water, at room temperature dry 2 weeks; Dried taro leaf is clayed into power.Powder uses the fine mesh filter of 30 μm further; Taro leaf powder (yy) is obtained after drying in vacuum.
3rd step, synthesize super-hydrophobic chitosan three-dimensional network sponge
Super-hydrophobic taro leaf powder in step 2 is dissolved in 1%(w/w) in the chloroform soln (200mL) of polydimethylsiloxane (PDMS), fully stir; Join in above-mentioned solution after chitosan three-dimensional network sponge is compressed, and repeatedly carry out compressing, expanding; Take out after 2h, at 80 DEG C, solidify 1h, obtain super-hydrophobic chitosan three-dimensional network sponge.
The area of super-hydrophobic chitosan three-dimensional network sponge prepared by present embodiment is 8cm
2, its structure is glycan three-dimensional network sponge load super-hydrophobic taro leaf powder, and three-dimensional network hole dimension is 20 ~ 200 μm (Fig. 2), and the thickness of skeleton wall is 500 ~ 1000nm.
Embodiment four: present embodiment prepares the super-hydrophobic oil suction sponge of chitosan in accordance with the following steps:
1st step, employing freeze-drying prepare chitosan sponge
Chitosan powder (4g) will be dissolved in the aqueous acetic acid (2wt%) of 200 milliliters, preparation chitosan solution (2wt%); Be transferred to by chitosan solution in furnace pot, cover filter paper on vessel top, and seal with scotch tape, be then placed in the cold steel pole at top, by liquid nitrogen cooling with completely freezing, freezing temp is-60 DEG C; Three-dimensional network shape chitosan is frozen into ice crystal by water-cooled and forms three-dimensional netted chitosan skeleton after dry removing.
2nd step, prepare super-hydrophobic taro leaf powder
Preparation taro leaf powder: fresh taro leaf is cut into small pieces, repeatedly washes away screw tap with deionized water, at room temperature dry 2 weeks; Clayed into power by dried taro leaf, powder uses the fine mesh filter of 30 μm further; Taro leaf powder (yy) is obtained after drying in vacuum.
3rd step, synthesize super-hydrophobic chitosan three-dimensional network sponge
Super-hydrophobic taro leaf powder in step 2 is dissolved in 1%(w/w) in the chloroform soln (200mL) of polydimethylsiloxane (PDMS), fully stir; Join in above-mentioned solution after chitosan three-dimensional network sponge is compressed, and repeatedly carry out compressing, expanding; Take out after 2h, at 80 DEG C, solidify 1h, obtain super-hydrophobic chitosan three-dimensional network sponge.
The area of super-hydrophobic chitosan three-dimensional network sponge prepared by present embodiment is 8cm
2, its structure is glycan three-dimensional network sponge load super-hydrophobic taro leaf powder, and three-dimensional network hole dimension is 5 ~ 50 μm (Fig. 2), and the thickness of skeleton wall is 500 ~ 1000nm.
Embodiment five: present embodiment and embodiment one ~ tetra-unlike, the concentration 5wt% of described chitosan solution, the concentration of polydimethylsiloxane (PDMS) is 5%.
Embodiment six: present embodiment and embodiment one ~ tetra-unlike, the concentration 8wt% of described chitosan solution, the concentration of polydimethylsiloxane (PDMS) is 8%.
Claims (4)
1., based on a preparation method for three-dimensional netted chitosan loaded super-hydrophobic particle oil suction sponge, it is characterized in that described method adopts lyophilize and absorption method to prepare super-hydrophobic chitosan composite sponge, concrete steps are as follows:
1st step, employing freeze-drying prepare chitosan sponge
Be transferred to by chitosan solution in furnace pot, cover filter paper on vessel top, and seal with scotch tape, be then placed in the cold steel pole at freeze drier top, by liquid nitrogen cooling with completely freezing, freezing temp scope is-5 ~-60 DEG C; Three-dimensional network shape chitosan is frozen into ice crystal by water-cooled and is formed after dry removing;
2nd step, prepare super-hydrophobic taro leaf powder:
Clayed into power by dried taro leaf, powder uses fine mesh filter further; Then, after drying 2 ~ 48h in 25 ~ 90 DEG C of vacuum, super-hydrophobic taro leaf powder is obtained;
3rd step, synthesize super-hydrophobic chitosan three-dimensional network sponge:
Super-hydrophobic taro leaf powder in step 2 is dissolved in the chloroform soln of polydimethylsiloxane (PDMS), fully stirs; Join in above-mentioned solution after chitosan three-dimensional network sponge is compressed, and repeatedly carry out compressing, expanding; Take out after 0.2 ~ 5h, at 25 ~ 100 DEG C, solidify 0.5 ~ 24h, obtain super-hydrophobic chitosan three-dimensional network sponge.
2. a kind of preparation method based on three-dimensional netted chitosan loaded super-hydrophobic particle oil suction sponge according to claim 1, is characterized in that the concentration 0.1 ~ 10wt% of described chitosan solution.
3. a kind of preparation method based on three-dimensional netted chitosan loaded super-hydrophobic particle oil suction sponge according to claim 1, is characterized in that the concentration of described polydimethylsiloxane is 0.01 ~ 10%(w/w).
4. a kind of preparation method based on three-dimensional netted chitosan loaded super-hydrophobic particle oil suction sponge according to claim 1, is characterized in that fresh taro leaf to be cut into small pieces, washes away screw tap with deionized water, at room temperature dry 1 ~ 3 week, obtains dry taro leaf.
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| CN104448317B (en) * | 2014-11-28 | 2017-03-01 | 华东理工大学 | A kind of preparation method of porous oil-absorbing material |
| CN104674384B (en) * | 2015-02-12 | 2017-10-03 | 中国科学院城市环境研究所 | Three-dimensional water-oil separating material based on electrostatic spinning technique and preparation method thereof |
| CN106564997B (en) * | 2016-11-14 | 2020-04-03 | 西南交通大学 | Water purification element, preparation method of water purification element and water purifier |
| CN106977764B (en) * | 2017-04-26 | 2018-11-16 | 杭州鼎好新材料有限公司 | A kind of superhydrophobic/supspongephilic spongephilic and preparation method thereof |
| CN112513154B (en) * | 2018-09-14 | 2023-01-10 | 港大科桥有限公司 | Gravity-driven chitosan-reinforced melamine sponge for stable ultrafast filtration |
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| CN103289016B (en) * | 2013-05-09 | 2016-01-20 | 燕山大学 | The preparation method of modified chitosan compound acrylic ester system oil-absorbing resin |
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